CN102373507A - Method for hydrothermally synthesizing Bi2WO6 material under assistance of imidazole ionic liquids - Google Patents
Method for hydrothermally synthesizing Bi2WO6 material under assistance of imidazole ionic liquids Download PDFInfo
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- CN102373507A CN102373507A CN2010102645582A CN201010264558A CN102373507A CN 102373507 A CN102373507 A CN 102373507A CN 2010102645582 A CN2010102645582 A CN 2010102645582A CN 201010264558 A CN201010264558 A CN 201010264558A CN 102373507 A CN102373507 A CN 102373507A
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- ion liquid
- glyoxaline ion
- mimbf
- solution
- ionic liquids
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Abstract
The invention relates to a method for hydrothermally synthesizing a Bi2WO6 material in an aqueous solution system containing imidazole ionic liquids. In the invention, the used ionic liquids are an imidazole ionic liquids of different side chain lengths (C4mimBF4, C8mimBF4, C10mimBF4, C12mimBF4, C14mimBF4 and C16mimBF4) and carboxyl-functionalized imidazole ionic liquid (AcmimBF4). The method comprises the following step of: performing hydrothermal crystallization on bismuth nitrate and sodium tungstate serving as raw materials to obtain a Bi2WO6 material with divergent photocatalytic degradation RhB performance. The Bi2WO6 material synthesized with a hydrothermal crystallization method based on the application of imidazole ionic liquids to the synthesis of photocatalytic materials has high dispersibility.
Description
Invention field
The present invention relates to synthetic and a kind of glyoxaline ion liquid auxiliary water of the photocatalysis field thermal synthesis Bi of inorganic materials
2WO
6The method of material.
Background of invention
Bi
2WO
6Energy gap is about 2.8eV, can absorb visible light, and it is at the photocatalytic degradation pollutent, and photochemical catalyzing is put O
2All there is application the aspect.Its compound method relates to solid sintering technology, hydrothermal crystallization method etc. at present.
Hydro-thermal is synthesized Bi at present
2WO
6The tensio-active agent that material relates to mainly contains: polyoxyethylene-poly-oxypropylene polyoxyethylene (EO
20PO
70EO
20) triblock copolymer, cetyl trimethylammonium bromide (CTAB), PVP K120 (PVP), polyoxyethylene glycol series (PEG-400 etc.), YD 30 etc.They are usually as synthetic Bi
2WO
6The structure directing agent of material can be controlled the generation of specific morphology.
The application of ionic liquid in inorganic materials is synthetic progressively causes people's attention, utilized its synthetic multiple inorganic molecule sieve with unique texture and performance, oxide compound, sulfide, inorganic materials such as metal.Ionic liquid is usually as the tensio-active agent (effect of rapping plate or structure directing) or the reaction solvent of synthetic inorganic material.Because the zwitterion adjustability of structure of ionic liquid itself in the preparation process of inorganic materials, can be regulated and control the size of product, pattern and dispersiveness, thus prepare the inorganic materials of different performance.The present invention has prepared with the glyoxaline ion liquid assisting alcohol-hydrothermal method and has had polymolecularity Bi
2WO
6Material, and study its influence to product photocatalysis performance.
Summary of the invention
It is a kind of in containing the water solution system of glyoxaline ion liquid that the object of the invention is to provide, and hydro-thermal is synthesized Bi
2WO
6The method of material.Expectation obtains having the Bi of polymolecularity
2WO
6Material, and study its photocatalytic degradation of dye RhB performance.
Concrete grammar of the present invention may further comprise the steps:
(1) pre-reaction material preparation:
A certain amount of Bismuth trinitrate is dissolved in the aqueous solution, and adds a certain amount of ionic liquid, stir fully dissolving; The sodium wolframate aqueous solution is dropwise joined above-mentioned solution, generate white precipitate;
(2) hydrothermal crystallizing reaction:
Above-mentioned precursor solution is transferred in the polytetrafluoroethylkettle kettle hydrothermal crystallizing 10～40h; Product is washed through filtering, and ethanol is washed, and oven dry obtains product.
The raw material Bismuth trinitrate of said reaction system is that metering was than 2: 1 with sodium wolframate.
Said reaction system ionic liquid consumption is that IL: Bi is 0.5～5.
The pH value scope of said reaction system precursor is 1～7.The pH value is passed through 1.2molL
-1Dilute nitric acid solution and 0.6molL
-1NaOH solution regulate.
The filling ratio of said reaction system hydro-thermal reaction is 80%.
The TR of said reaction system hydrothermal crystallizing is 120 ℃～160 ℃.
Auxiliary water thermal synthesis Bi according to the invention
2WO
6Glyoxaline ion liquid be:
(1) the long glyoxaline ion liquid (C of different side chains
4MimBF
4, C
8MimBF
4, C
10MimBF
4, C
12MimBF
4, C
14MimBF
4, C
16MimBF
4).
(2) the glyoxaline ion liquid AcmimBF of carboxyl-functional
4
Wherein, three kinds of representational ion liquid structural formulas are following:
Ionic liquid is as a kind of structure directing agent; Its side chain lengths has very big influence to the state of aggregation of reaction process intermediate ion liquid; Thereby possibly cause the inorganic species of synthetic that certain difference is arranged on size, state of aggregation and pattern, so the present invention has selected the long glyoxaline ion liquid of above-mentioned a series of side chain for use; The present invention has also attempted the ionic liquid AcmimBF behind the glyoxaline cation carboxyl-functional in addition
4Auxiliary synthetic Bi
2WO
6The present invention is through the auxiliary hydrothermal crystallization method synthetic Bi of glyoxaline ion liquid
2WO
6Material has higher dispersiveness.
Description of drawings
Fig. 1 is different sorts ionic liquid auxiliary water thermal synthesis Bi
2WO
6The XRD figure of material, hydrothermal crystallizing 20h
Fig. 2 is different sorts ionic liquid auxiliary water thermal synthesis Bi
2WO
6The SEM figure of material, hydrothermal crystallizing 20h
Fig. 3 ionic liquid BmimBF
4Auxiliary water thermal synthesis Bi
2WO
6The photocatalytic degradation RhB performance of material.
Embodiment
Embodiment 1.BmimBF
4Ionic liquid auxiliary water thermal synthesis Bi
2WO
6
The Bismuth trinitrate of 4mmol is dissolved in 1.2molL
-1In the dilute nitric acid solution, and the BmimBF of adding 4mmol
4Ionic liquid stirs fully dissolving, is made into water white solution; With 0.05molL
-1The sodium wolframate aqueous solution dropwise join above-mentioned solution, generate white precipitate; Use 0.6molL
-1The NaOH solution pH value of regulating above-mentioned solution be 1, and stir 20h in 40 ℃;
Afterwards, above-mentioned solution is transferred in the 100ml polytetrafluoroethylkettle kettle, filling ratio is 80%, in 160 ℃ of hydrothermal crystallizing 20h; Naturally cool to room temperature then, product is washed through filtering, and ethanol is washed, and 70 ℃ of oven dry obtain the faint yellow solid powder.SEM schemes to show: this Bi
2WO
6Product has very high dispersiveness, and is the flower-shaped structure of organizing certainly.
Embodiment 2.BmimBF
4Ionic liquid auxiliary water thermal synthesis Bi
2WO
6
The Bismuth trinitrate of 4mmol is dissolved in 1.2molL
-1In the dilute nitric acid solution, and the BmimBF of adding 20mmol
4Ionic liquid stirs fully dissolving, is made into water white solution; With 0.05molL
-1The sodium wolframate aqueous solution dropwise join above-mentioned solution, generate white precipitate; Use 0.6molL
-1The NaOH solution pH value of regulating above-mentioned solution be 1, and stir 20h in 40 ℃;
Afterwards, above-mentioned solution is transferred in the 100ml polytetrafluoroethylkettle kettle, filling ratio is 80%, in 160 ℃ of hydrothermal crystallizing 20h; Naturally cool to room temperature then, product is washed through filtering, and ethanol is washed, and 70 ℃ of oven dry obtain the faint yellow solid powder.Embodiment 3.BmimBF
4Ionic liquid auxiliary water thermal synthesis Bi
2WO
6
The Bismuth trinitrate of 4mmol is dissolved in 1.2molL
-1In the dilute nitric acid solution, and the BmimBF of adding 4mmol
4Ionic liquid stirs fully dissolving, is made into water white solution; With 0.05molL
-1The sodium wolframate aqueous solution dropwise join above-mentioned solution, generate white precipitate; Use 0.6molL
-1The NaOH solution pH value of regulating above-mentioned solution be 7, and stir 20h in 40 ℃;
Afterwards, above-mentioned solution is transferred in the 100mi polytetrafluoroethylkettle kettle, filling ratio is 80%, in 120 ℃ of hydrothermal crystallizing 20h; Naturally cool to room temperature then, product is washed through filtering, and ethanol is washed, and 70 ℃ of oven dry obtain the faint yellow solid powder.SEM schemes to show: this Bi
2WO
6Product has very high dispersiveness, and organizes structure certainly for flower-shaped, but the fine granularity material occurs on the sheet of composition flower-like structure.
Embodiment 4.C
8MimBF
4Ionic liquid auxiliary water thermal synthesis Bi
2WO
6
With 3.2mmol C
8MimBF
4Be dissolved in the 48ml zero(ppm) water, add 3.2mmol Bismuth trinitrate solid down in agitation condition, solution becomes white opacity; 1.6mmol sodium wolframate solid being dissolved in the 32ml aqueous solution, dropwise joining above-mentioned Bismuth trinitrate and ionic liquid mixing solutions again, still is white opacity; Stir 20h in 40 ℃ then;
Afterwards, above-mentioned solution is transferred in the 100ml polytetrafluoroethylkettle kettle, filling ratio is 80%, in 160 ℃ of hydrothermal crystallizing 20h; Naturally cool to room temperature then, product is washed through filtering, and ethanol is washed, and 70 ℃ of oven dry obtain the light yellow solid powder.
Embodiment 5.C
16MimBF
4Ionic liquid auxiliary water thermal synthesis Bi
2WO
6
With 3.2mmol C
16MimBF
4Be dissolved in the 48ml zero(ppm) water, add 3.2mmol Bismuth trinitrate solid down in agitation condition, solution becomes white opacity; 1.6mmol sodium wolframate solid being dissolved in the 32ml aqueous solution, dropwise joining above-mentioned Bismuth trinitrate and ionic liquid mixing solutions again, still is white opacity; Stir 20h in 40 ℃ then;
Afterwards, above-mentioned solution is transferred in the 100ml polytetrafluoroethylkettle kettle, filling ratio is 80%, in 160 ℃ of hydrothermal crystallizing 20h; Naturally cool to room temperature then, product is washed through filtering, and ethanol is washed, and 70 ℃ of oven dry obtain the light yellow solid powder.
Embodiment 6.AcmimBF
4Ionic liquid auxiliary water thermal synthesis Bi
2WO
6
AcmimBF with 3.2mmol
4Be dissolved in 1.2molL
-1In the dilute nitric acid solution, add 3.2mmol Bismuth trinitrate solid down, stir fully dissolving, be made into water white solution in agitation condition; With 0.05molL
-1The sodium wolframate aqueous solution dropwise join above-mentioned solution, generate white precipitate; Use 0.6molL
-1The NaOH solution pH value of regulating above-mentioned solution be 1, and stir 20h in 40 ℃;
Afterwards, above-mentioned solution is transferred in the 100ml polytetrafluoroethylkettle kettle, filling ratio is 80%, in 160 ℃ of hydrothermal crystallizing 20h; Naturally cool to room temperature then, product is washed through filtering, and ethanol is washed, and 70 ℃ of oven dry obtain the faint yellow solid powder.
Claims (6)
1. glyoxaline ion liquid auxiliary water thermal synthesis Bi
2WO
6The method of material is characterized in that glyoxaline ion liquid does organic additive auxiliary water thermal crystallisation reaction, may further comprise the steps:
(1) pre-reaction material preparation:
A certain amount of Bismuth trinitrate is dissolved in the aqueous solution, and adds a certain amount of ionic liquid, stir fully dissolving; The sodium wolframate aqueous solution is dropwise joined above-mentioned solution, generate white precipitate;
(2) hydrothermal crystallizing reaction:
Above-mentioned precursor solution is transferred in the polytetrafluoroethylkettle kettle hydrothermal crystallizing; The product that obtains is washed through filtering, and ethanol is washed, and oven dry obtains product.
2. there are following two types according to the said glyoxaline ion liquid of claim 1: the long glyoxaline ion liquid of different side chains; The carboxyl-functional glyoxaline ion liquid; Said reaction system ionic liquid consumption is that IL: Bi is 0.5～5.
3. according to claim 2, different side chains are long to be C
4Glyoxaline ion liquid comprise: C
4MimBF
4, C
8MimBF
4, C
10MimBF
4, C
12MimBF
4, C
14MimBF
4, C
16MimBF
4
4. the glyoxaline ion liquid according to the said carboxyl-functional of claim 2 is: AcmimBF
4
5. according to the said a kind of glyoxaline ion liquid auxiliary water thermal synthesis Bi of claim 1
2WO
6The method of material, the pH value that it is characterized in that precursor solution is between 1 to 7.
6. according to the said a kind of glyoxaline ion liquid auxiliary water thermal synthesis Bi of claim 1
2WO
6The method of material is characterized in that the filling ratio of precursor in water heating kettle is 80%, and the hydrothermal crystallizing temperature is between 120 ℃ to 160 ℃.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104549269A (en) * | 2014-12-31 | 2015-04-29 | 上海师范大学 | Method for preparing Ag/Bi2WO6 photocatalyst with hollow shell structure by depositing Ag particles with ultrasonic-assisted photoreduction method |
| CN105870439A (en) * | 2016-04-22 | 2016-08-17 | 济南大学 | Preparation method and application of porous Co3O4 |
| CN108126756A (en) * | 2017-12-12 | 2018-06-08 | 上海大学 | Bismuth tungstate-MIL-53 (Al) composite material, preparation method and application |
| CN112142111A (en) * | 2020-08-31 | 2020-12-29 | 盐城工学院 | Method for preparing bismuth tungstate with assistance of ionic liquid, product and application thereof |
| CN113387889A (en) * | 2021-06-17 | 2021-09-14 | 湖南文理学院 | Novel porous imidazole metal compound nano powder and preparation method thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101186336A (en) * | 2007-12-05 | 2008-05-28 | 北京航空航天大学 | Method for preparing layer thickness homogenized bismuth oxyhalide |
-
2010
- 2010-08-27 CN CN2010102645582A patent/CN102373507A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101186336A (en) * | 2007-12-05 | 2008-05-28 | 北京航空航天大学 | Method for preparing layer thickness homogenized bismuth oxyhalide |
Non-Patent Citations (1)
| Title |
|---|
| JIEXIANG XIA ET AL.: "Self-assembly and enhanced optical absorption of Bi2WO6 nests via ionic liquid-assisted hydrothermal method", 《MATERIALS CHEMISTRY AND PHYSICS》 * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104549269A (en) * | 2014-12-31 | 2015-04-29 | 上海师范大学 | Method for preparing Ag/Bi2WO6 photocatalyst with hollow shell structure by depositing Ag particles with ultrasonic-assisted photoreduction method |
| CN104549269B (en) * | 2014-12-31 | 2017-03-15 | 上海师范大学 | Ultrasonic wave added photoreduction met hod deposits Ag particles to prepare hollow shell structure Ag/Bi2WO6The method of photocatalyst |
| CN105870439A (en) * | 2016-04-22 | 2016-08-17 | 济南大学 | Preparation method and application of porous Co3O4 |
| CN105870439B (en) * | 2016-04-22 | 2018-03-16 | 济南大学 | A kind of preparation method and applications of porous cobaltosic oxide |
| CN108126756A (en) * | 2017-12-12 | 2018-06-08 | 上海大学 | Bismuth tungstate-MIL-53 (Al) composite material, preparation method and application |
| CN108126756B (en) * | 2017-12-12 | 2020-12-15 | 上海大学 | Bismuth tungstate-MIL-53 (Al) composite material, and preparation method and application thereof |
| CN112142111A (en) * | 2020-08-31 | 2020-12-29 | 盐城工学院 | Method for preparing bismuth tungstate with assistance of ionic liquid, product and application thereof |
| CN113387889A (en) * | 2021-06-17 | 2021-09-14 | 湖南文理学院 | Novel porous imidazole metal compound nano powder and preparation method thereof |
| CN113387889B (en) * | 2021-06-17 | 2023-05-09 | 湖南文理学院 | Preparation method of porous imidazole metal compound nano-powder |
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Application publication date: 20120314 |