CN105251474B - One kind is used for light-catalysed bismuth nanospheres and preparation method - Google Patents
One kind is used for light-catalysed bismuth nanospheres and preparation method Download PDFInfo
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- CN105251474B CN105251474B CN201510646002.2A CN201510646002A CN105251474B CN 105251474 B CN105251474 B CN 105251474B CN 201510646002 A CN201510646002 A CN 201510646002A CN 105251474 B CN105251474 B CN 105251474B
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Abstract
It is used for light-catalysed bismuth nanospheres and preparation method the present invention relates to one kind, belongs to field of inorganic nano material.Bismuth nanoparticle is prepared as：First, a certain amount of bismuth nitrate is weighed, is dissolved in certain volume ethylene glycol solution, round-bottomed flask is moved into after stirring a period of time.The above-mentioned flask equipped with solution is put into microwave reaction device, and magnetic stir bar is added in the solution, adjust rotating speed, connect condensed water, power, time, temperature are set, and opening program is reacted, and question response terminates rear natural cooling, obtained product is centrifuged, washed, is dried, bismuth nanoparticle is obtained.It is characterized in that the material microstructure is the um of diameter about 10 20 microballoon, microballoon is made up of the nm of thickness about 150 ~ 300 laminated structure, and composition is the bismuth simple substance of the hexagonal crystal phase structure of JCPDS numberings 44 1246.
Description
Technical field
The invention belongs to inorganic nano material and technical field of environment pollution control, and in particular to one kind can be used for degraded dirty
Contaminate thing（Dyestuff）The bismuth nanospheres and preparation method with high efficiency photocatalysis activity.
Background technology
With population drastically expansion and industry fast development, problem of environmental pollution have become influence human being's production,
The matter of utmost importance of life.National governments all by environmental pollution improvement be classified as at this stage and the coming years cardinal task.Especially
It is a large amount of discharges of a large amount of soluble azo dyes such as methyl orange in dyeing, water quality for the survival of mankind is increasingly disliked
Change.The many difficult for biological degradation of these polluters, once into water body, due to it, natural degradation process is slow in water body, and it is endangered
Evil property retardation is longer.Light-catalyzed reaction can permineralization be various inorganic ions under illumination condition by pollutant, therefore
Got the attention in terms of environmental improvement, on the research and development of photochemical catalyst, as current study hotspot both domestic and external.
Nanometer bismuth microballoon due to size is small, specific surface area big and the features such as having noble metal and semimetal simultaneously, from
And cause the active sites on its surface more, scraggly atomic stepses are formd, can be increased when being used as catalyst
With the contact area of reactant, therefore, compared with traditional catalyst, with higher catalytic activity.In photocatalysis field, nanometer
Bismuth is finally decomposed as can make the harmful organic substances in water during catalyst, it is to avoid its pollution to environment.Research shows, nanometer
The reaction speed of bismuth is 100 ~ 1000 times of bulk bismuth material, and compared with ordinary particle, nanometer bismuth hardly causes light
Scattering, therefore one of be the photochemical catalyst of great application prospect.
Up to the present, people use chemical vapour deposition technique, and coprecipitation, anodizing, hydro-thermal method etc. is a variety of
Method has prepared the nanometer bismuth of different-shape.Although preparation method is a lot, but still all comes with some shortcomings, prepare at present
Nanometer bismuth the degradation efficiency of pollutant is still waited to improve.Seek photocatalysis inexpensive, environment-friendly and with high catalytic activity
Material is the key of photocatalysis technology development.
The content of the invention
It can be used for degradation of contaminant it is an object of the invention to overcome the deficiencies of the prior art and provide one kind（Dyestuff）Tool
There are the bismuth micro-sphere material and preparation method of high efficiency photocatalysis activity.
The method that the present invention is provided is to use the cheap bismuth nitrate and ethylene glycol industrially commonly used as reagent, in microwave
Reaction obtains the bismuth microballoon of layer structure in reaction unit, and experimentation is simple to operation, easily realizes the large-scale production of product,
Gained bismuth microballoon has good application prospect in terms of pollutant control.Specifically include following steps：
1）First, a certain amount of bismuth nitrate is weighed, is dissolved in certain volume ethylene glycol solution, is moved into after stirring a period of time
Round-bottomed flask.
2) the above-mentioned flask equipped with solution is put into microwave reaction device, and adds magnetic stir bar in the solution, adjusted
Rotating speed, connects condensed water, sets power, time, temperature, and opening program is reacted, and question response terminates rear natural cooling, will
Obtained product is centrifuged, washed, being dried, and obtains bismuth nanoparticle.
In the present invention, step（1）Concentration of the middle bismuth nitrate in ethylene glycol is controlled in 0.05-0.4 mol/L, liquor capacity
Control steps between the 1/8 to 2/3 of reaction vessel cumulative volume（2）Middle power setting is 500 ~ 1000W, and the time is set as 0.5
~ 2h, temperature is set as 200 ~ 250 DEG C.
Compared with prior art, the present invention has the advantages that：
The inventive method uses industrial conventional use of bismuth nitrate and ethylene glycol as raw material, and simple and easy to get, cost is low
Honest and clean, synthetic method is Microwave-assisted synthesis method, and whole experiment process is simple, easy to operate, it is easy to realize the extensive of product
Production, degraded of the gained bismuth nanoparticle to methyl orange has good catalytic effect.
Brief description of the drawings
Fig. 1 is the SEM figures of the bismuth nanoparticle prepared.
Fig. 2 is the SEM figures of the bismuth nanoparticle prepared.
Fig. 3 is the SEM figures of the bismuth nanoparticle prepared.
Fig. 4 is the bismuth nanoparticle degradation of methylene blue design sketch prepared.
Embodiment
The present invention is further described with reference to embodiment.For the production technology of the invention people professional to this
Easily implement.The present embodiment is implemented lower premised on technical solution of the present invention, gives detailed embodiment
And process, but protection scope of the present invention is not limited to following embodiments.The experiment of unreceipted actual conditions in the following example
Method, generally according to normal condition, or according to the condition proposed by manufacturer.
Embodiment
2g bismuth nitrates are weighed, is dissolved in 50ml ethylene glycol, stirs.
Above-mentioned solution is moved into microwave reaction instrument, stirring is opened, condensed water is connected.
Microwave reaction parameter, time are set：1 h, power：900W, temperature：200 °, rear operation program is provided with, is started
Reaction.
After reaction terminates, sediment is centrifuged, is washed respectively three times with water and ethanol, is finally putting into vacuum drying chamber
In 60 ° be dried overnight.
The photocatalysis performance test of material
The g of precise 0.1 bismuth nano material adds 100 ml methylene blues（MB）Solution（20 mg/L）In, ultrasound
It is scattered；Gained suspension lucifuge, which stirs 1 h, makes material reach adsorption equilibrium；3 ml suspension are taken out after balance, residue is outstanding
Supernatant liquid is poured into 500 ml quartz ampoules, is then placed in light-catalyzed reaction instrument；500 W high voltage mercury lamp radiations are opened, every 5
Min takes 3 ml suspension in centrifuge tube, the h of total reaction time 1；Reaction terminates, and each sample of taking-up is centrifuged
Afterwards, supernatant is taken to survey its absorbance in 664 nm or so with ultraviolet-visible spectrophotometer, so that when reflecting each degraded
Between after section remaining methylene blue concentration, reflect that bismuth nanoparticle photocatalyst for degrading methylene blue is made in this method with this
Effect.
Claims (1)
1. a kind of preparation method for light-catalysed bismuth nanospheres, it is characterised in that specific synthesis step is as follows：
First, a certain amount of bismuth nitrate is weighed, is dissolved in certain volume ethylene glycol solution, round bottom is moved into after stirring a period of time and is burnt
Bottle；Concentration control of the bismuth nitrate in ethylene glycol is in 0.05-0.4 mol/L, and liquor capacity control is overall in reaction vessel
Between long-pending 1/8 to 2/3；
The above-mentioned flask equipped with solution is put into microwave reaction device, and adds magnetic stir bar in the solution, rotating speed is adjusted, even
Connect condensed water, it 500 ~ 1000W, time is that 0.5 ~ 2h, temperature are 200 ~ 250 DEG C that setting power, which is, and opening program is reacted,
Question response terminates rear natural cooling, and obtained product is centrifuged, washed, is dried, bismuth nanoparticle is obtained；The bismuth nanometer
Microballoon microstructure is diameter 10-20 um, and microballoon is made up of the nm of thickness 150 ~ 300 laminated structure, and composition is compiled for JCPDS
The bismuth simple substance of number 44-1246 hexagonal crystal phase structures.
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| CN105903474A (en) * | 2016-05-12 | 2016-08-31 | 江苏华夏制漆科技有限公司 | Preparation method of magnetic Fe3O4@ elemental bismuth sphere photocatalyst |
| CN106179372B (en) * | 2016-07-29 | 2018-12-14 | 江苏大学 | A kind of C@Fe based on biomass porous carbon3O4The Preparation method and use of@Bi composite photo-catalyst |
| CN108421987A (en) * | 2018-03-16 | 2018-08-21 | 南京工业大学 | A kind of preparation method of sheet bismuth with elementary |
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| CN102212880B (en) * | 2010-04-08 | 2013-03-13 | 中国检验检疫科学研究院 | Elementary substance Bi nano-structured material and preparation method and application thereof |
| CN103774217B (en) * | 2012-10-26 | 2016-08-24 | 北京师范大学 | A kind of preparation method of micron order bismuth single crystal flower |
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Inventor after: Liu Bitao Inventor after: Yan Hengqing Inventor after: Li Lu Inventor before: Liu Bitao Inventor before: Chen Yuan Inventor before: Mo Qionghua Inventor before: Yan Xuelian Inventor before: Li Lu |
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Effective date of registration: 20190628 Address after: 213000 Nandu Town Industrial Concentration Zone, Liyang City, Changzhou City, Jiangsu Province Patentee after: Liyang Dadi New Materials Co.,Ltd. Address before: 402168 Chongqing Yongchuan District double bamboo town Patentee before: Chongqing University of Arts and Sciences |
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Denomination of invention: Bismuth nanospheres material and preparation method for photocatalysis Effective date of registration: 20230629 Granted publication date: 20170725 Pledgee: China Zheshang Bank Co.,Ltd. Changzhou Branch Pledgor: Liyang Dadi New Materials Co.,Ltd. Registration number: Y2023980046759 |
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