CN104689838A - Preparation method for BiOCl photocatalyst with controllable morphology and crystal face - Google Patents
Preparation method for BiOCl photocatalyst with controllable morphology and crystal face Download PDFInfo
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- CN104689838A CN104689838A CN201510077454.3A CN201510077454A CN104689838A CN 104689838 A CN104689838 A CN 104689838A CN 201510077454 A CN201510077454 A CN 201510077454A CN 104689838 A CN104689838 A CN 104689838A
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Abstract
The invention provides a preparation method for a BiOCl photocatalyst with a controllable morphology and a crystal face, and belongs to the technical field of environmental chemical engineering photocatalysis water treatment. The preparation method is characterized by comprising the following steps: adding Bi(NO3)3.5H2O into a certain amount of water, ethyl alcohol or a dimethyl formamide solvent, uniformly stirring, then adding a certain amount of chlorination-1-butyl-3-methylimidazole, stirring for 20min for uniform mixing, performing ultrasonic treatment under room temperature for 10-60min, and reacting to generate white precipitate; washing the precipitate by water and ethyl alcohol, and drying the precipitate under the temperature of 60 DEG C to obtain BiOCl photocatalyst powder with different morphologies. According to the preparation method provided by the invention, the BiOCl preparation period is short, and the use of a surfactant is avoided; by control on the solvent, the preparation method for implementing BiOCl crystal surface control (101 and 102) and morphology control (a nano sheet shape, a flower-like structure and an irregular disk shape) can be conveniently realized. The preparation method is completed in the next step under the room temperature, has the advantages of simple process, extremely short preparation period, environment friendliness and the like and is favorable for engineering large-scale preparation. The catalyst has outstanding degrading effects on rhodamine B, methyl orange, quinoline blue and the like by visible light and sunshine and has an actual application prospect.
Description
Technical field
The present invention relates to the preparation method of a kind of pattern and the controlled BiOCl photochemical catalyst of crystal face, belong to environmental chemical engineering photocatalysis water-treatment technology field.
Background technology
Environment in recent years is polluted day by day serious, and mostly organic pollution can not get effective improvement.Photocatalysis oxidation technique directly converts solar energy into chemical energy and electric energy by conductor photocatalysis material, and organic pollution permineralization poisonous in environment is degraded, be considered to solve one of the human society energy and the potential technical scheme of environmental problem most at present.
Bismoclite (BiOCl) is that a kind of ternary is partly led, because it has the electrical properties of uniqueness and high-quality, and magnetic property, optical property, catalytic property and be considered to a kind of semi-conducting material with potential using value.BiOCl is not only cheaply easy to get as a kind of novel photochemical catalyst, stable performance, active good, and than traditional photochemical catalyst TiO
2, it has and better closes catalytic activity.Because the photocatalysis property height of BiOCl depends on its crystal structure and pattern, the BiOCl therefore preparing Morphological Diversity plays most important effect to its application in photocatalysis of development.At present, existing a large amount of report synthesizes nanometer wire, sheet, granular, and flower-shaped BiOCl.Its synthetic method is also varied, comprises hydro-thermal method, template auxiliary law, method for hydrolysis, electrochemical method, phonochemistry synthetic method, microwave method etc.But the usual severe reaction conditions of these preparation methods, as high temperature, high pressure, the reaction time is long, higher acid-base value etc.Therefore, a kind of method developing simple condition gentleness has certain necessity to the BiOCl preparing morphology controllable.
Summary of the invention
The object of this invention is to provide the preparation method of a kind of pattern and the controlled BiOCl photochemical catalyst of crystal face.
The object of the invention is to realize in the following way: the preparation method of a kind of pattern and the controlled BiOCl photochemical catalyst of crystal face:
The first step, accurately takes the Bi (NO that three parts of amount of substances are 10mmol
3)
35H
2o joins the deionized water of 20 ~ 30mL respectively, in ethanol or solvent dimethylformamide, stirs 10min and causes evenly, obtain the mixed liquor of three parts of bismuth-containings, be numbered A respectively, B, C;
Second step, adds the chlorination-1-butyl-3-methylimidazole of 10 ~ 20mmol respectively to A, B, C, stir 10min and mix, obtain white mixed liquor;
3rd step, three portions of white mixed liquors that second step is obtained ultrasonic 10 ~ 60 min at 25 ~ 35 DEG C.
4th step, by three parts of mixed liquor centrifugations after ultrasonic, the precipitation obtained after deionized water and ethanol alternately each washing three times at 60 DEG C vacuum drying 24h obtain the BiOCl photochemical catalyst powder of different-shape.
Compared with prior art, advantage of the present invention:
(1) method is simple, is easy to operation, and reaction condition is gentle;
(2) manufacturing cycle is extremely short, only needs 10 ~ 60min both can prepare sample;
(3) pattern and crystal face controlled.
(4) bismuthyl chloride prepared by is to rhodamine B under visible ray and sunshine, and quinoline blue, methyl orange all has efficient photocatalytic degradation effect.
Accompanying drawing explanation
Fig. 1 is the XRD figure of the BiOCl prepared by the embodiment of the present invention one.
Fig. 2 is the BiOCl(prepared by the embodiment of the present invention one take water as reaction dissolvent) SEM figure, multiplication factor 25000 times.
Fig. 3 is the BiOCl(prepared by the embodiment of the present invention one take ethanol as reaction dissolvent) SEM figure, multiplication factor 10000 times.
Fig. 4 be BiOCl(prepared by the embodiment of the present invention one with dimethyl formamide for answering solvent) SEM figure, multiplication factor 15000 times.
Fig. 5 is the C/C of BiOCl prepared by the embodiment of the present invention one catalytic degradation rhodamine B under visible light
0with the graph of a relation of time.
Fig. 6 is the C/C of the BiOCl catalytic degradation methyl orange under sunshine prepared by the embodiment of the present invention one
0with the graph of a relation of time.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further described, but the present invention is not limited to this.
Embodiment 1
The first step, accurately takes the Bi (NO that three parts of amount of substances are 10mmol
3)
35H
2o joins the deionized water of 30mL respectively, in ethanol or solvent dimethylformamide, stirs 10min and causes evenly, obtain
The mixed liquor of three parts of bismuth-containings, is numbered A respectively, B, C;
Second step, respectively to the chlorination-1-butyl-3-methylimidazole adding 11.5mmol in A, B, C, stirs 10min and mixes, obtain white mixed liquor;
3rd step, the three portions of white mixed liquors obtained by second step are put into KQ-100 type ultrasonic cleaner and are carried out ultrasonic 10 min, regulate reaction temperature to be 30 DEG C;
4th step, by three parts of mixed liquor centrifugations after ultrasonic, the precipitation obtained after deionized water and ethanol alternately each washing three times at 60 DEG C vacuum drying 24h obtain the BiOCl photochemical catalyst powder of different-shape.
Embodiment 2
The first step, accurately takes the Bi (NO that three parts of amount of substances are 10mmol
3)
35H
2o joins the deionized water of 20mL respectively, in ethanol or solvent dimethylformamide, stirs 10min and causes evenly, obtain the mixed liquor of three parts of bismuth-containings, be numbered A respectively, B, C;
Second step, respectively to the chlorination-1-butyl-3-methylimidazole adding 10mmol in A, B, C, stirs 10min and mixes, obtain white mixed liquor;
3rd step, the three portions of white mixed liquors obtained by second step are put into KQ-100 type ultrasonic cleaner and are carried out ultrasonic 20 min, regulate reaction temperature to be 25 DEG C;
4th step, by three parts of mixed liquor centrifugations after ultrasonic, the precipitation obtained after deionized water and ethanol alternately each washing three times at 60 DEG C vacuum drying 24h obtain the BiOCl photochemical catalyst powder of different-shape.
Embodiment three
The first step, accurately takes the Bi (NO that three parts of amount of substances are 10mmol
3)
35H
2o joins the deionized water of 25mL respectively, in ethanol or solvent dimethylformamide, stirs 10min and causes evenly, obtain the mixed liquor of three parts of bismuth-containings, be numbered A respectively, B, C;
Second step, respectively to the chlorination-1-butyl-3-methylimidazole adding 15mmol in A, B, C, stirs 10min and mixes, obtain white mixed liquor;
3rd step, the three portions of white mixed liquors obtained by second step are put into KQ-100 type ultrasonic cleaner and are carried out ultrasonic 30 min, regulate reaction temperature to be 25 DEG C;
4th step, by three parts of mixed liquor centrifugations after ultrasonic, the precipitation obtained after deionized water and ethanol alternately each washing three times at 60 DEG C vacuum drying 24h obtain the BiOCl photochemical catalyst powder of different-shape.
Embodiment four
The first step, accurately takes the Bi (NO that three parts of amount of substances are 10mmol
3)
35H
2o joins the deionized water of 30mL respectively, in ethanol or solvent dimethylformamide, stirs 10min and causes evenly, obtain the mixed liquor of three parts of bismuth-containings, be numbered A respectively, B, C;
Second step, respectively to the chlorination-1-butyl-3-methylimidazole adding 20mmol in A, B, C, stirs 10min and mixes, obtain white mixed liquor;
3rd step, the three portions of white mixed liquors obtained by second step are put into KQ-100 type ultrasonic cleaner and are carried out ultrasonic 60 min, regulate reaction temperature to be 35 DEG C;
4th step, by A, B, C tri-parts of mixed liquor centrifugations after ultrasonic, the precipitation obtained after deionized water and ethanol alternately each washing three times at 60 DEG C vacuum drying 24h obtain the BiOCl photochemical catalyst powder of different-shape.
Claims (6)
1. a preparation method for pattern and the controlled BiOCl photochemical catalyst of crystal face, comprises the steps:
The first step, accurately takes the Bi (NO that three parts of amount of substances are 10mmol
3)
35H
2o joins the deionized water of 20 ~ 30mL respectively, ethanol, in solvent dimethylformamide, stirs 10min and causes evenly, obtain the mixed liquor of three parts of bismuth-containings, be numbered A respectively, B, C;
Second step, respectively to the chlorination-1-butyl-3-methylimidazole adding 10 ~ 20mmol in A, B, C, stirs 10min and mixes, obtain white mixed liquor;
3rd step, by three portions of white mixed liquors ultrasonic 10 ~ 60 min at 25 ~ 35 DEG C;
4th step, by three parts of mixed liquor centrifugations after ultrasonic, the precipitation obtained after deionized water and ethanol alternately each washing three times at 60 DEG C vacuum drying 24h obtain the BiOCl photochemical catalyst powder of different-shape.
2. the preparation method of a kind of pattern according to claim 1 and the controlled BiOCl photochemical catalyst of crystal face, the deionized water added in described second step, the amount of ethanol or solvent dimethylformamide is equal.
3. the preparation method of a kind of pattern according to claim 1 and the controlled BiOCl photochemical catalyst of crystal face, in described 3rd step, mixed solution is put into KQ-100 type ultrasonic cleaner to carry out ultrasonic 10 ~ 60 min by ultrasonic 10 ~ 60 min.
4. the preparation method of a kind of pattern according to claim 1 and the controlled BiOCl photochemical catalyst of crystal face, it is characterized in that: be that reaction dissolvent obtains irregular nanometer plate-like BiOCl with water, being that reaction dissolvent obtains nano-sheet BiOCl with ethanol, is that reaction dissolvent obtains flower ball-shaped BiOCl with dimethyl formamide.
5. the preparation method of a kind of pattern according to claim 1 and the controlled BiOCl photochemical catalyst of crystal face, it is characterized in that: with water, ethanol, 110 crystal faces of the BiOCl that dimethyl formamide obtains as reaction dissolvent and the long-pending peak area ratio of 102 crystal faces are respectively 0.43,0.35 and 0.99.
6. the preparation method of a kind of pattern according to claim 1 and the controlled BiOCl photochemical catalyst of crystal face, it is characterized in that: described BiOCl falls rhodamine B at visible ray and sunshine, methyl orange and quinoline blue have outstanding degradation effect, and the BiOCl obtained using dimethyl formamide as reaction dissolvent has better photocatalysis effect than deionized water and ethanol as the BiOCl that solvent obtains.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105344366A (en) * | 2015-12-11 | 2016-02-24 | 湘潭大学 | Preparation method for sunlight responding BiPO4 photocatalyst |
| CN105457660A (en) * | 2015-12-10 | 2016-04-06 | 湘潭大学 | Preparation method and use of flower-like bismuthyl iodide/bismuth oxychloride complex |
| CN105833887A (en) * | 2016-04-01 | 2016-08-10 | 合肥学院 | BiOCl/beta-FeOOH composite nanomaterial and preparation method thereof |
| CN105836799A (en) * | 2016-03-22 | 2016-08-10 | 武汉工程大学 | Method for regulation of bismuth oxybromine exposed crystal planes |
| CN106492849A (en) * | 2016-11-03 | 2017-03-15 | 江苏大学 | A kind of preparation method of BiOCl ultrathin nanometers piece photochemical catalyst |
| CN106984340A (en) * | 2017-04-27 | 2017-07-28 | 武汉纺织大学 | A kind of preparation method of sheet BiOCl photochemical catalysts and obtained photochemical catalyst and application |
| CN107335452A (en) * | 2017-06-15 | 2017-11-10 | 江苏大学 | The method that bismuth oxybromide ultrathin nanometer piece photochemical catalyst is synthesized under room temperature condition |
| CN107497491A (en) * | 2017-08-29 | 2017-12-22 | 电子科技大学 | A kind of preparation method of composite Nano catalysis material |
| CN108479815A (en) * | 2018-03-09 | 2018-09-04 | 绍兴文理学院 | A kind of octahedral shape BiOCl photochemical catalysts and the preparation method and application thereof |
| CN109701562A (en) * | 2019-01-04 | 2019-05-03 | 深圳大学 | A kind of bismuth oxybromide and its preparation method and application of three-dimensional flower-shaped structure |
| CN114669309A (en) * | 2022-05-07 | 2022-06-28 | 桂林电子科技大学 | One-dimensional linear BiOCl photocatalytic material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105457660A (en) * | 2015-12-10 | 2016-04-06 | 湘潭大学 | Preparation method and use of flower-like bismuthyl iodide/bismuth oxychloride complex |
| CN105344366A (en) * | 2015-12-11 | 2016-02-24 | 湘潭大学 | Preparation method for sunlight responding BiPO4 photocatalyst |
| CN105836799A (en) * | 2016-03-22 | 2016-08-10 | 武汉工程大学 | Method for regulation of bismuth oxybromine exposed crystal planes |
| CN105836799B (en) * | 2016-03-22 | 2017-11-21 | 武汉工程大学 | A kind of method of regulation and control bromine oxygen bismuth exposure crystal face |
| CN105833887A (en) * | 2016-04-01 | 2016-08-10 | 合肥学院 | BiOCl/beta-FeOOH composite nanomaterial and preparation method thereof |
| CN106492849B (en) * | 2016-11-03 | 2019-05-31 | 江苏大学 | A kind of preparation method of BiOCl ultrathin nanometer piece photochemical catalyst |
| CN106492849A (en) * | 2016-11-03 | 2017-03-15 | 江苏大学 | A kind of preparation method of BiOCl ultrathin nanometers piece photochemical catalyst |
| CN106984340A (en) * | 2017-04-27 | 2017-07-28 | 武汉纺织大学 | A kind of preparation method of sheet BiOCl photochemical catalysts and obtained photochemical catalyst and application |
| CN107335452A (en) * | 2017-06-15 | 2017-11-10 | 江苏大学 | The method that bismuth oxybromide ultrathin nanometer piece photochemical catalyst is synthesized under room temperature condition |
| CN107497491A (en) * | 2017-08-29 | 2017-12-22 | 电子科技大学 | A kind of preparation method of composite Nano catalysis material |
| CN108479815A (en) * | 2018-03-09 | 2018-09-04 | 绍兴文理学院 | A kind of octahedral shape BiOCl photochemical catalysts and the preparation method and application thereof |
| CN108479815B (en) * | 2018-03-09 | 2019-11-15 | 绍兴文理学院 | A kind of BiOCl photochemical catalyst octahedronlike and the preparation method and application thereof |
| CN109701562A (en) * | 2019-01-04 | 2019-05-03 | 深圳大学 | A kind of bismuth oxybromide and its preparation method and application of three-dimensional flower-shaped structure |
| CN109701562B (en) * | 2019-01-04 | 2021-11-16 | 深圳大学 | Bismuth oxybromide with three-dimensional flower-like structure and preparation method and application thereof |
| CN114669309A (en) * | 2022-05-07 | 2022-06-28 | 桂林电子科技大学 | One-dimensional linear BiOCl photocatalytic material and preparation method and application thereof |
| CN114669309B (en) * | 2022-05-07 | 2023-11-07 | 桂林电子科技大学 | One-dimensional linear BiOCl photocatalytic material and preparation method and application thereof |
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Application publication date: 20150610 |