CN102989507B - Preparation and performance detection method of spherical bismuth-base Bi-DMF (dimethylformamide) photocatalyst - Google Patents
Preparation and performance detection method of spherical bismuth-base Bi-DMF (dimethylformamide) photocatalyst Download PDFInfo
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- CN102989507B CN102989507B CN201210553216.1A CN201210553216A CN102989507B CN 102989507 B CN102989507 B CN 102989507B CN 201210553216 A CN201210553216 A CN 201210553216A CN 102989507 B CN102989507 B CN 102989507B
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Abstract
The invention relates to a preparation and performance detection method of a bismuth-base photocatalyst, belonging to the field of an organic material. The method is characterized by preparing a spherical bismuth-base photocatalyst with regular and uniform appearance with a heating reflux method. A synthesis method comprises the following steps of: dissolving Bi(NO3)3.5H2O in acetic acid, wherein ethylene glycol is used as a reaction medium; stirring uniformly; adding a certain volume of dimethylformamide (DMF); and performing heating reflux on the obtained solution and stirring to obtain Bi-DMF flower spheres. The prepared Bi-DMF flower spheres are subjected to a photocatalytic performance test in visible light, the purple rhodamine becomes colorless in 2 hours, and the degradation is complete. According to the invention, the material preparation method is simple, the synthesis temperature is low, the reaction time is short, the price of raw materials is low, and industrial production is easy to implement. Research shows that the spherical bismuth-base catalyst has good photocatalytic performance in the range of visible light, is easy to recover and reuse and has broad development and application value in terms of environment purification.
Description
Technical field
The invention belongs to organic material field, relate to a kind of three-dimensional manometer/preparation of micron multi-stage bismuth-based catalysts material and the research in visible light catalytic performance thereof, be characterized in adopting a kind of hot reflux synthetic method that adds easily to synthesize regular appearance, homogeneous spherical bismuth-based catalysts, according to raw material preparation condition called after Bi-DMF bouquet.Take rhodamine liquor as the target compound of light-catalyzed reaction, research shows that this Bi-DMF bouquet has good degradation to rhodamine liquor in visible-range, illustrates that it has vast potential for future development in the depollution of environment.
Background technology
Environmental pollution now has become an acid test of facing mankind, material also one of focus becoming Recent study of catalytic degradation, low-density solar energy can be converted into highdensity chemical energy and electric energy by photocatalysis technology, directly utilize sunshine to degrade and each pollutant in mineralized water and air, receive the very big concern of people.TiO
2because photocatalytic is good, good stability uses more photochemical catalyst at present.But TiO
2with gap wider (3.2ev), can only the ultraviolet light of absorbing wavelength λ≤387nm.In recent years, some researchers explore the exploitation of novel photocatalyst, and achieve some impressive progresses.Bismuth series photocatalyst has good catalytic performance, particularly in visible-range, has obvious absorption, and this is their common outstanding feature and advantages.At present, the synthetic method of bismuth-based catalysts nano material mainly contains vapor phase method, solid phase method, liquid phase method.In prepared product, although some novel photochemical catalyst its at ultraviolet region and visible region, all there is good photocatalysis performance, but its preparation method generally needs the harsh conditions such as higher temperature, complicated technical process and Preparation equipment, improving the preparation method of photochemical catalyst, is an important research direction of photochemical catalyst.Along with deepening continuously of the research to bismuth series photocatalyst, three-dimensional manometer/micron multi-stage has revealed its superiority relative to 2 dimensions, 1 dimension and 0 dimension nano material, causes the great interest of people.Although made a lot of effort, the synthesis of the multistage material structure of the Nano/micron of controllable appearance and size has been had to be still a challenge.Therefore, the simple and easy method adopting a kind of preparation method improving photochemical catalyst accurately can control product morphology has very important significance concerning tool the material preparing special appearance.
Summary of the invention
The chemical method that the object of this invention is to provide a kind of simple and easy, low cost to obtain exterior appearance homogeneous, strong spherical bismuthino visible light catalyst Bi-DMF bouquet can be manipulated.
A preparation method for spherical bismuthino Bi-DMF photochemical catalyst, is characterized in by adding hot reflux and the method for Keep agitation prepares regular appearance, homogeneous spherical bismuth-based catalysts three-dimensional manometer/micron multi-stage material.Synthesis step is: by Bi (NO
3)
35H
2o is dissolved in acetic acid as bismuth source and stirs 15min and make it fully dissolve, form bismuth acetate solution, using organic solvent ethylene glycol as reaction medium, join in bismuth acetate solution, stir 30min, then the dimethyl formamide (being called for short DMF) of certain volume is added, after stirring 15min, the settled solution obtained is placed in 100ml three-necked bottle, add hot reflux and Keep agitation, there is a large amount of white precipitate, Deng reaction terminate and after being cooled to room temperature, obtained white precipitate is transferred in centrifuge tube, totally six times are washed with distilled water and ethanol alternating centrifugal, again products therefrom after the baking oven inner drying 12 ~ 16h of 60 ~ 80 ° of C temperature ranges, namely spherical bismuthino photochemical catalyst is obtained, be called Bi-DMF bouquet.
Concentration range and the relevant reaction condition of various reactant are: in acetic acid-ethylene glycol-dimethyl formamide reaction system, Bi (NO
3)
3concentration in reaction system is 0.05mol/L, in reaction system, the volume ratio of acetic acid and ethylene glycol is 0.5 ~ 1.25, the addition of DMF is 0.500 ~ 0.630 mL/mL, heating reflux temperature is 60 ~ 120 ° of C, the heating reflux reaction time is 10 min ~ 60min, adds in thermal reflow process and needs Keep agitation.
Adding of each reactant have certain order, namely first bismuth source should be dissolved in acetic acid, then add a certain amount of ethylene glycol.
By scanning electron microscopic observation, spherical bismuthino Bi-DMF photochemical catalyst can find that product is spherical in shape, spherical hierarchy, there is good ball shaped nano/micron multi-stage, average diameter is about 2-8um, be interweaved by many nanometer sheet and form, nanometer sheet thickness is between 30 ~ 50nm, forms the loose structure of many openings.
The method of testing of spherical bismuthino Bi-DMF properties of catalyst is: the Bi-DMF photochemical catalyst powder 0.2g of preparation is joined 10 of 200ml
-5in the rhodamine colored dyes of mol/L, within the scope of visible ray λ ﹥ 420nm, carry out photocatalysis test, show that this Bi-DMF photochemical catalyst has good photocatalysis performance under visible light conditions, to the photocatalytic degradation of colored dyes, there is potential using value.
Material preparation method of the present invention is simple and easy, and equipment is simple, and synthesis temperature is lower, and the reaction time is shorter, low in raw material price, without the need to the surfactant of costliness as template; The solvent used and other reactants have free from environmental pollution, save the energy, conversion ratio high, be easy to the features such as suitability for industrialized production.In addition, this synthetic method can control the pattern of product effectively, stable in properties, repeatable strong, be a kind of desirable friendly process.Research shows that this Bi-DMF bouquet is in visible-range, has good photocatalysis performance, and more easily reclaims, reuse, and illustrates that it has wide development and application and is worth in the depollution of environment.Illustrate that it has wide development and application and is worth in the depollution of environment.
Accompanying drawing explanation
Fig. 1 heating reflux reaction temperature 80 DEG C, heating reflux reaction time 20min, the XRD collection of illustrative plates of the Bi-DMF bouquet reclaimed after the XRD collection of illustrative plates of the end product Bi-DMF bouquet synthesized under acetic acid 20ml and ethylene glycol 20ml, dimethyl formamide 40ml condition in reaction system and catalysis.
Fig. 2 heating reflux reaction temperature 80 DEG C, heating reflux reaction time 20min, the scanning electron microscopic picture of the end product Bi-DMF bouquet synthesized under acetic acid 20ml and ethylene glycol 20ml, dimethyl formamide 40ml condition in reaction system.
Fig. 3 heating reflux reaction temperature 80 DEG C, heating reflux reaction time 20min, the end product Bi-DMF bouquet synthesized under acetic acid 20ml and ethylene glycol 20ml, dimethyl formamide 40ml condition in reaction system under radiation of visible light condition to the photocatalytic degradation curve of RhB solution.
Detailed description of the invention
Embodiment one
Take 2g Bi (NO
3)
35H
2o is dissolved in the acetic acid of 14ml, stirs 15 min, then adds 26ml ethylene glycol, stir 30min, finally add the dimethyl formamide of 40ml, stir 15 min, be positioned over by the settled solution obtained in 100ml three-necked bottle, heating is back to 80 DEG C, and Keep agitation, reaction time is 20min, there is a large amount of white precipitate, the precipitation distilled water obtained and ethanol are respectively washed three times, and at the baking oven inner drying 12h of 80 ° of C, namely obtain end product, the product obtained is white powder.
Embodiment two
Take 2g Bi (NO
3)
35H
2o is dissolved in the acetic acid of 16ml, stirs 15 min, then adds 14ml ethylene glycol, stir 30min, finally add the dimethyl formamide of 50ml, stir 15 min, be positioned over by the settled solution obtained in 100ml three-necked bottle, heating is back to 80 DEG C, and Keep agitation, reaction time is 20min, there is a large amount of white precipitate, the precipitation distilled water obtained and ethanol are respectively washed three times, and at the baking oven inner drying 12h of 80 ° of C, namely obtain end product, the product obtained is white powder.
Embodiment three
Take 2g Bi (NO
3)
35H
2o is dissolved in the acetic acid of 20ml, stir 15 min, then 20ml ethylene glycol is added, stir 30min, finally add the dimethyl formamide (DMF) of 40ml, stir 15 min, be positioned over by the settled solution obtained in 100ml three-necked bottle, heating is back to 60 DEG C, and Keep agitation, reaction time is 20min, there is a large amount of white precipitate, the precipitation distilled water obtained and ethanol are respectively washed three times, and at the baking oven inner drying 12h of 80 ° of C, namely obtain end product, the product obtained is white powder.
Embodiment four
Take 2g Bi (NO
3)
35H
2o is dissolved in the acetic acid of 20ml, stirs 15 min, then adds 20ml ethylene glycol, stir 30min-, finally add the dimethyl formamide of 40ml, stir 15 min, be positioned over by the settled solution obtained in 100ml three-necked bottle, heating is back to 120 DEG C, and Keep agitation, reaction time is 20min, there is a large amount of white precipitate, the precipitation distilled water obtained and ethanol are respectively washed three times, and at the baking oven inner drying 12h of 80 ° of C, namely obtain end product, the product obtained is white powder.
Embodiment five
Take 2g Bi (NO
3)
35H
2o is dissolved in the acetic acid of 20ml respectively, stirs 15 min, then adds 20ml ethylene glycol, stir 30min, finally add the dimethyl formamide of 40ml, stir 15 min, be positioned over by the settled solution obtained in 100ml three-necked bottle, heating is back to 80 DEG C, and Keep agitation, reaction time is 20min, there is a large amount of white precipitate, the precipitation distilled water obtained and ethanol are respectively washed three times, and at the baking oven inner drying 12h of 80 ° of C, namely obtain end product, the product obtained is white powder.Obtained dried white powder bismuth-based catalysts Bi-DMF bouquet 0.2g is joined 200ml rhodamine (RhB, 10
-5mol/L), in, first under dark condition, 30min is placed, to reach the adsorption equilibrium between dyestuff and catalyst, gone to visible ray λ ﹥ 420nm afterwards, under illuminate condition, take out 2ml suspension every 30min, centrifugal rear ultraviolet specrophotometer filtrates tested absorbing wavelength change.
Claims (2)
1. the preparation method of a spherical bismuthino Bi-DMF photochemical catalyst, it is characterized in that, by adding hot reflux and the method for Keep agitation prepares regular appearance, homogeneous spherical bismuth-based catalysts three-dimensional manometer/micron multi-stage material, synthesis step is: by Bi (NO
3)
35H
2o is dissolved in acetic acid stirring as bismuth source and makes it fully dissolve to obtain bismuth acetate solution, using organic solvent ethylene glycol as reaction medium, join in bismuth acetate solution, stir and evenly mix, after adding the dimethyl formamide of certain volume again, the settled solution obtained is placed in three-necked bottle, add hot reflux and Keep agitation, there is a large amount of white precipitate, Deng reaction terminate and after being cooled to room temperature, obtained white precipitate is transferred in centrifuge tube, be total to 5-7 time with distilled water and the washing of ethanol alternating centrifugal, again products therefrom after the baking oven inner drying 12 ~ 16h of 60 ~ 80 DEG C of temperature ranges, namely spherical bismuthino Bi-DMF photochemical catalyst is obtained, be called Bi-DMF bouquet,
Concentration range and the relevant reaction condition of various reactant are: in acetic acid-ethylene glycol-dimethyl formamide reaction system, Bi (NO
3)
3concentration in reaction system is 0.05mol/L, in reaction system, the volume ratio of acetic acid and ethylene glycol is 0.5 ~ 1.25, the addition of dimethyl formamide is 0.500 ~ 0.630mL/mL, heating reflux temperature is 60 ~ 120 DEG C, the heating reflux reaction time is 10min ~ 60min, adds in thermal reflow process and needs Keep agitation;
Adding of each reactant has order, namely first bismuth source is dissolved in acetic acid, then adds a certain amount of ethylene glycol.
2. the method for testing of a kind of spherical bismuthino Bi-DMF properties of catalyst prepared by claim 1, it is characterized in that, the Bi-DMF photochemical catalyst powder 0.2g of preparation is joined in the rhodamine colored dyes of the 10-5mol/L of 200ml, within the scope of visible ray λ ﹥ 420nm, carry out photocatalysis test, in 2h, rhodamine takes off for colourless by purple, and completely, catalytic efficiency can reach more than 95% in degraded; Show that this Bi-DMF photochemical catalyst has good photocatalysis performance under visible light conditions, to the photocatalytic degradation of colored dyes, there is potential using value.
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| CN110180529B (en) * | 2019-05-23 | 2020-10-13 | 北京科技大学 | Preparation method for synthesizing photocatalytic material by using MOF as precursor |
Citations (4)
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|---|---|---|---|---|
| WO1990014307A1 (en) * | 1989-05-22 | 1990-11-29 | MERCK Patent Gesellschaft mit beschränkter Haftung | Process for manufacturing powdered ceramic oxides |
| CN101565204A (en) * | 2009-05-27 | 2009-10-28 | 北京科技大学 | Preparation method of porous bismuth oxide powder with high specific surface area |
| CN101791558A (en) * | 2010-03-19 | 2010-08-04 | 上海师范大学 | Bismuth ferrite microsphere photocatalyst with hollow structure and preparation method thereof |
| CN102226084A (en) * | 2011-04-28 | 2011-10-26 | 北京科技大学 | Synthesis method of flower-like Y2O3:Eu<3+> microspheres |
-
2012
- 2012-12-19 CN CN201210553216.1A patent/CN102989507B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1990014307A1 (en) * | 1989-05-22 | 1990-11-29 | MERCK Patent Gesellschaft mit beschränkter Haftung | Process for manufacturing powdered ceramic oxides |
| CN101565204A (en) * | 2009-05-27 | 2009-10-28 | 北京科技大学 | Preparation method of porous bismuth oxide powder with high specific surface area |
| CN101791558A (en) * | 2010-03-19 | 2010-08-04 | 上海师范大学 | Bismuth ferrite microsphere photocatalyst with hollow structure and preparation method thereof |
| CN102226084A (en) * | 2011-04-28 | 2011-10-26 | 北京科技大学 | Synthesis method of flower-like Y2O3:Eu<3+> microspheres |
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