CN105481009A - Preparation method of bismuth subcarbonate nanoribbon - Google Patents

Preparation method of bismuth subcarbonate nanoribbon Download PDF

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CN105481009A
CN105481009A CN201510922593.1A CN201510922593A CN105481009A CN 105481009 A CN105481009 A CN 105481009A CN 201510922593 A CN201510922593 A CN 201510922593A CN 105481009 A CN105481009 A CN 105481009A
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preparation
nano belt
reaction kettle
bismuthyl carbonate
carbonate nano
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CN105481009B (en
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李海斌
黄国游
付圣豪
陈曙光
李富进
刘鹏
张健
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Changsha University of Science and Technology
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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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • 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
    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/17—Nanostrips, nanoribbons or nanobelts, i.e. solid nanofibres with two significantly differing dimensions between 1-100 nanometer

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Compounds Of Iron (AREA)

Abstract

The invention provides a preparation method of a bismuth subcarbonate nanoribbon. The method comprises the steps that Bi(NO3)3.5H2O serves as the raw material and is added to a mixed solution of ethanolamine and water, and magnetic stirring and ultrasonic treatment are conducted; obtained white suspension is transferred to a hydrothermal reaction kettle for a reaction, after the reaction is completed, cooling is conducted, white precipitate in the reaction kettle is taken out, washed and dried, and the bismuth subcarbonate nanoribbon is obtained. The method has the advantages that devices are simple, the temperature ranging from 120 DEG C to 140 DEG C is low, and environmental protection is achieved due to the fact that the synthesis reaction is conducted in a sealed system; a chemical reagent capable of being decomposed to generate CO2 does not need to be introduced to serve as the raw material, powder is synthesized in one time through a solvent-thermal method, high-temperature calcination is not needed, synthesized powder is high in purity, high in crystallinity and regular in morphology, and the preparation method is simple in technology, high in efficiency, low in energy consumption, low in cost and environmentally friendly.

Description

A kind of preparation method of bismuthyl carbonate nano belt
Technical field
The invention belongs to field of functional materials, be specifically related to a kind of preparation method of bismuthyl carbonate nano belt.
Background technology
Photocatalysis technology is utilized to carry out sewage disposal, can effective degradation of organic substances, reducing heavy metal ion.And energy consumption needed for this technology is low, easy and simple to handle, reaction conditions is gentle, do not have secondary pollution.Therefore, photochemical catalysis is the very promising environmental improvement technology of one.Bismuthyl carbonate (Bi 2o 2cO 3) also known as Bismuth Subcarbonate, bismuth subcarbonate.Bi 2o 2cO 3crystalline structure be by (Bi 2o 2) 2+layer and CO 3 2-layer is staggered and forms, and belongs to typical " sillen " structure.(Bi 2o 2) 2+layer and CO 3 2-layer replaces the interior electrostatic field that symbiosis is formed, and is conducive to promoting that light induced electron is separated with hole.Therefore, from configuration aspects analysis, Bi 2o 2cO 3as photocatalyst, there is huge potential value.
Have between the performance of photocatalyst material and its microscopic appearance and contact closely, the nanostructure of different-shape, due to its different specific surface area, has larger impact to photocatalytic activity.Research shows, nano belt had both had the high-ratio surface value of nano material, has again thinner thickness and larger surface tension, in a dimension, also have the micron-scale of macroscopic view simultaneously.The migration that such constructional feature is conducive to electronics and hole be separated, be also conducive to photocatalyst Separation and Recovery from degradation solution.Therefore, Bi is prepared 2o 2cO 3nano belt has very important theory and realistic meaning.
In recent years, Bi 2o 2cO 3as a kind of novel photocatalyst, its morphology control has prepared concern.At present, Bi 2o 2cO 3preparation method mainly contain hydrothermal method, solvent-thermal method, utilize urea or Na 2cO 3as CO 2source, introduces citric acid and coordinates adjust ph or interpolation tensio-active agent or organic polymer to realize morphology control synthesis, obtain sheet, classification superstructure as flower-shaped, spongiform structure.There is not yet Bi 2o 2cO 3the report of nano belt structure, does not see without the need to additionally introducing containing CO yet 2reagent and morphology control additive (tensio-active agent, organic polymer), and directly utilize solvent to realize the hot legal system of simple solvent of thing phase and morphology control for Bi simultaneously 2o 2cO 3the report of nano belt.
Summary of the invention
The object of the present invention is to provide a kind of bismuthyl carbonate (Bi 2o 2cO 3) preparation method of nano belt, solvent thermal single sintering, without the need to high-temperature calcination, have that technique is simple, efficiency is high, energy consumption is low, with low cost, eco-friendly feature, the powder purity of synthesis is high, degree of crystallinity is high, pattern is regular.
For achieving the above object, the present invention adopts following technical scheme:
A preparation method for bismuthyl carbonate nano belt, comprises the following steps:
1) by thanomin and deionized water thanomin by volume: the ratio mixing of deionized water=(0.6-1.7): 1, obtains mixing solutions after magnetic agitation;
2) by Bi (NO 3) 35H 2o joins in described mixing solutions, carries out magnetic agitation and supersound process, obtains white suspension liquid, is hydro-thermal reaction precursor liquid, the Bi (NO in described precursor liquid 3) 3concentration be 0.05-0.15mol/L;
3) described hydro-thermal reaction precursor liquid is proceeded in hydrothermal reaction kettle, stopped reaction be incubated 15-20 hour at 120-140 DEG C after;
4), after question response temperature is down to room temperature, hydrothermal reaction kettle is taken out, the white depositions that centrifugation goes out to be obtained by reacting, throw out is washed, dry, namely obtain bismuthyl carbonate nano belt.
Preferred version: described step 1) in thanomin and the volume ratio of deionized water be (0.8-1.5): 1, the magnetic agitation time is 5-10min.
Preferred version: described step 2) in the magnetic agitation time be 20-30min, sonication treatment time is 10-15min.
Preferred version, described step 2) in Bi (NO in precursor liquid 3) 3concentration be 0.1mol/L.
Preferred version, described step 3) in hydrothermal reaction kettle liner be tetrafluoroethylene material, hydrothermal reaction kettle packing ratio is 60%-80%.
Preferred version, described step 4) in washing deionized water and dehydrated alcohol by white depositions washing to neutral, described drying is dry 10-20h at 70 DEG C-80 DEG C.
Bi obtained by the present invention 2o 2cO 3the crystal formation of nano belt conforms to card JCPDSNo.84-1752, and the width of described bismuthyl carbonate nano belt is 100-400nm, and length is 10-20 μm, and thickness is 20-30nm.
The present invention will be further explained below:
By method of the present invention, the hot method of contriver's first passage simple solvent has prepared Bi 2o 2cO 3nano belt.Can realize the present invention, reaction conditions of the present invention be most important.
Thanomin generates Bi 2o 2cO 3the key factor of thing phase.Thanomin is a kind of organic bases, the CO simultaneously in energy absorbed air 2, therefore by its by a certain percentage with H 2o mixing is made into weakly alkaline solution and after stir for some time under atmospheric environment, just both containing OH in solution -, again containing CO 3 2-.Bi (NO 3) 3after being dissolved in this solution, Bi 3+with OH -and CO 3 2-effect, generates Bi under High Temperature High Pressure 2o 2cO 3crystal.If thanomin to be replaced to other organic solvent, Bi can not be generated 2o 2cO 3or be difficult to obtain pure Bi 2o 2cO 3thing phase.Such as replace to ethylene glycol, because ethylene glycol is to CO 2do not have adsorption, the product generated after solvent thermal is Bi 2o 3but not Bi 2o 2cO 3; And for example replace to quadrol, although quadrol is to the CO in air 2also have adsorption, but due to quadrol alkalescence too strong, that final solvent thermal obtains is Bi 2o 3and Bi 2o 2cO 3mixture phase.
Thanomin both had crucial effect to the thing of product mutually with the proportioning of water, had crucial effect again to the pattern of product.If the proportioning of thanomin and water is greater than 1.7, in product, there will be dephasign.If the proportioning of thanomin and water is less than 0.6, though product is pure Bi 2o 2cO 3, but its pattern is lath-shaped but not nano belt.Only have the proportioning controlling thanomin and water in the interval of 0.6-1.7, preferably in the interval of 0.8-1.5, just may obtain pure Bi 2o 2cO 3nano belt.
Compared with prior art, the present invention has following beneficial outcomes:
Bi provided by the invention 2o 2cO 3the preparation method of nano belt, with Bi (NO 3) 35H 2o is raw material, by Bi (NO 3) 35H 2o joins in the mixing solutions of thanomin and water, carries out magnetic agitation and supersound process.Proceeded in hydrothermal reaction kettle by gained white suspension liquid and react, after question response completes, cooling, takes out the white depositions in reactor, and washing, drying, namely obtain Bi 2o 2cO 3nano belt.
The method is without the need to additionally introducing containing CO 2reagent and morphology control additive (tensio-active agent, organic polymer), but directly utilize solvent to realize thing phase and morphology control simultaneously.There is the features such as device is simple, low temperature (120-140 DEG C), environmental protection (building-up reactions is carried out in enclosed system).Solvent thermal single sintering powder, without the need to high-temperature calcination, and the powder purity of synthesis is high, degree of crystallinity is high, pattern is regular, is the environmentally friendly preparation method that a kind of technique is simple, efficiency is high, energy consumption is low, with low cost.
Accompanying drawing explanation
Fig. 1 is Bi prepared by the embodiment of the present invention 1 2o 2cO 3the XRD figure of nano belt
Fig. 2 is Bi prepared by the embodiment of the present invention 1 2o 2cO 3the SEM figure of nano belt
Embodiment
Method of the present invention is described by specific embodiment below in conjunction with accompanying drawing; but the present invention is not limited thereto; all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Experimental technique described in following embodiment, if no special instructions, is ordinary method; Described reagent and material, if no special instructions, all can obtain from commercial channels.
Reactant B i (the NO used in the present invention 3) 35H 2o, thanomin etc. are commercially available analytical pure.
Embodiment 1
Step 1: by thanomin and deionized water 0.8:1 mixing by volume, obtain mixing solutions after magnetic agitation 7min;
Step 2: by Bi (NO 3) 35H 2o joins in above-mentioned mixing solutions, after magnetic agitation 25min, then supersound process 13min, obtain white suspension liquid, be hydro-thermal reaction precursor liquid.Bi (NO in precursor liquid 3) 3concentration be 0.1mol/L;
Step 3: precursor liquid is proceeded in hydrothermal reaction kettle, the filling ratio of hydrothermal reaction kettle is 74%, puts into constant temperature blast drying oven, stopped reaction after being incubated 16 hours at 140 DEG C;
Step 4: after question response temperature is down to room temperature, takes out hydrothermal reaction kettle, the white depositions that centrifugation goes out to be obtained by reacting, and after adopting deionized water and absolute ethanol washing throw out to neutrality, at 75 DEG C, hour dry 15h, namely obtains Bi 2o 2cO 3nano belt, as shown in Figure 1, its purity is high as seen, and impurity peaks is few for its XRD figure.SEM figure as shown in Figure 2, as seen its for width be 100-400nm, length is 10-20 μm, and thickness is the nano strip of 20-30nm.
Embodiment 2
Step 1: by thanomin and deionized water 1:1 mixing by volume, obtain mixing solutions after magnetic agitation 6min;
Step 2: by Bi (NO 3) 35H 2o joins in above-mentioned mixing solutions, after magnetic agitation 22min, then supersound process 12min, obtain white suspension liquid, be hydro-thermal reaction precursor liquid.Bi (NO in precursor liquid 3) 3concentration be 0.08mol/L;
Step 3: precursor liquid is proceeded in hydrothermal reaction kettle, the filling ratio of hydrothermal reaction kettle is 72%, puts into constant temperature blast drying oven, stopped reaction after being incubated 18 hours at 130 DEG C;
Step 4: after question response temperature is down to room temperature, takes out hydrothermal reaction kettle, the white depositions that centrifugation goes out to be obtained by reacting, and after adopting deionized water and absolute ethanol washing throw out to neutrality, at 78 DEG C, hour dry 11h, namely obtains Bi 2o 2cO 3nano belt, its XRD detected result is similar to embodiment 1 with SEM detected result.
Embodiment 3
Step 1: by thanomin and deionized water 1.5:1 mixing by volume, obtain mixing solutions after magnetic agitation 5min;
Step 2: by Bi (NO 3) 35H 2o joins in above-mentioned mixing solutions, after magnetic agitation 20min, then supersound process 10min, obtain white suspension liquid, be hydro-thermal reaction precursor liquid.Bi (NO in precursor liquid 3) 3concentration be 0.05mol/L;
Step 3: precursor liquid is proceeded in hydrothermal reaction kettle, the filling ratio of hydrothermal reaction kettle is 70%, puts into constant temperature blast drying oven, stopped reaction after being incubated 20 hours at 120 DEG C;
Step 4: after question response temperature is down to room temperature, takes out hydrothermal reaction kettle, the white depositions that centrifugation goes out to be obtained by reacting, and after adopting deionized water and absolute ethanol washing throw out to neutrality, at 80 DEG C, hour dry 10h, namely obtains Bi 2o 2cO 3nano belt, its XRD detected result is similar to embodiment 1 with SEM detected result.
Comparative example 1
Step 1: by thanomin and deionized water 3:1 mixing by volume, obtain mixing solutions after magnetic agitation 8min;
Step 2: by Bi (NO 3) 35H 2o joins in above-mentioned mixing solutions, after magnetic agitation 28min, then supersound process 14min, obtain white suspension liquid, be hydro-thermal reaction precursor liquid.Bi (NO in precursor liquid 3) 3concentration be 0.12mol/L;
Step 3: precursor liquid is proceeded in hydrothermal reaction kettle, the filling ratio of hydrothermal reaction kettle is 76%, puts into constant temperature blast drying oven, stopped reaction after being incubated 16 hours at 140 DEG C;
Step 4: after question response temperature is down to room temperature, takes out hydrothermal reaction kettle, the white depositions that centrifugation goes out to be obtained by reacting, and after adopting deionized water and absolute ethanol washing throw out to neutrality, hour dry 12h at 78 DEG C, the product obtained is Bi 2o 3and Bi 2o 2cO 3mixture.
Comparative example 2
Step 1: by thanomin and deionized water 0.3:1 mixing by volume, obtain mixing solutions after magnetic agitation 10min;
Step 2: by Bi (NO 3) 35H 2o joins in above-mentioned mixing solutions, after magnetic agitation 30min, then supersound process 15min, obtain white suspension liquid, be hydro-thermal reaction precursor liquid.Bi (NO in precursor liquid 3) 3concentration be 0.15mol/L;
Step 3: precursor liquid is proceeded in hydrothermal reaction kettle, the filling ratio of hydrothermal reaction kettle is 80%, puts into constant temperature blast drying oven, stopped reaction after being incubated 15 hours at 140 DEG C;
Step 4: after question response temperature is down to room temperature, takes out hydrothermal reaction kettle, the white depositions that centrifugation goes out to be obtained by reacting, and after adopting deionized water and absolute ethanol washing throw out to neutrality, at 80 DEG C, hour dry 10h, namely obtains lath-shaped Bi 2o 2cO 3powder.

Claims (7)

1. a preparation method for bismuthyl carbonate nano belt, is characterized in that, comprises the following steps:
1) by thanomin and deionized water thanomin by volume: the ratio mixing of deionized water=(0.6-1.7): 1, obtains mixing solutions after magnetic agitation;
2) by Bi (NO 3) 35H 2o joins in described mixing solutions, carries out magnetic agitation and supersound process, obtains white suspension liquid, is hydro-thermal reaction precursor liquid, the Bi (NO in described precursor liquid 3) 3concentration be 0.05-0.15mol/L;
3) described hydro-thermal reaction precursor liquid is proceeded in hydrothermal reaction kettle, stopped reaction be incubated 15-20 hour at 120-140 DEG C after;
4), after question response temperature is down to room temperature, hydrothermal reaction kettle is taken out, the white depositions that centrifugation goes out to be obtained by reacting, throw out is washed, dry, namely obtain bismuthyl carbonate nano belt.
2. the preparation method of bismuthyl carbonate nano belt according to claim 1, is characterized in that: described step 1) in thanomin and the volume ratio of deionized water be (0.8-1.5): 1, the magnetic agitation time is 5-10min.
3. the preparation method of bismuthyl carbonate nano belt according to claim 1, is characterized in that: described step 2) in the magnetic agitation time be 20-30min, sonication treatment time is 10-15min.
4. the preparation method of bismuthyl carbonate nano belt according to claim 1, is characterized in that: described step 2) in Bi (NO in precursor liquid 3) 3concentration be 0.1mol/L.
5. the preparation method of bismuthyl carbonate nano belt according to claim 1, is characterized in that: described step 3) in hydrothermal reaction kettle liner be tetrafluoroethylene material, hydrothermal reaction kettle packing ratio is 60%-80%.
6. the preparation method of bismuthyl carbonate nano belt according to claim 1, is characterized in that: described step 4) in washing deionized water and dehydrated alcohol by white depositions washing to neutral, described drying is dry 10-20h at 70 DEG C-80 DEG C.
7. according to the preparation method of the described bismuthyl carbonate nano belt of one of claim 1-6, it is characterized in that: obtained Bi 2o 2cO 3the crystal formation of nano belt conforms to card JCPDSNo.84-1752, and the width of described bismuthyl carbonate nano belt is 100-400nm, and length is 10-20 μm, and thickness is 20-30nm.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106391076A (en) * 2016-09-14 2017-02-15 江南大学 Gray Bi2O2CO3 photocatalyst and preparation method thereof
CN106423286A (en) * 2016-09-14 2017-02-22 江南大学 BiOCOOH-Bi2O2CO3 compound photocatalyst and preparation method thereof
CN106732524A (en) * 2017-02-24 2017-05-31 云南大学 A kind of α/β bismuth oxide phase heterojunction photocatalyst and its preparation method and purposes

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CN101817555A (en) * 2010-03-25 2010-09-01 山东大学 Bismuthyl carbonate micro flowery material with graded structure and preparation method thereof
CN102275987A (en) * 2011-05-25 2011-12-14 中国地质大学（武汉） Nano/micro-scale sheet bismuthyl carbonate material and preparation method thereof
CN103708551A (en) * 2013-12-26 2014-04-09 湛江师范学院 Preparation method of bismuth oxycarbonate flower-like microsphere thermally synthesized by ethylene glycol-water mixed solvent
CN104229883A (en) * 2014-09-24 2014-12-24 浙江大学 Preparation method of bismuth oxycarbonate microtablets and bismuth oxycarbonate microtablets
CN104229882A (en) * 2014-09-24 2014-12-24 浙江大学 Preparation method and product of bismuth oxycarbonate microspheres

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101817555A (en) * 2010-03-25 2010-09-01 山东大学 Bismuthyl carbonate micro flowery material with graded structure and preparation method thereof
CN102275987A (en) * 2011-05-25 2011-12-14 中国地质大学（武汉） Nano/micro-scale sheet bismuthyl carbonate material and preparation method thereof
CN103708551A (en) * 2013-12-26 2014-04-09 湛江师范学院 Preparation method of bismuth oxycarbonate flower-like microsphere thermally synthesized by ethylene glycol-water mixed solvent
CN104229883A (en) * 2014-09-24 2014-12-24 浙江大学 Preparation method of bismuth oxycarbonate microtablets and bismuth oxycarbonate microtablets
CN104229882A (en) * 2014-09-24 2014-12-24 浙江大学 Preparation method and product of bismuth oxycarbonate microspheres

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106391076A (en) * 2016-09-14 2017-02-15 江南大学 Gray Bi2O2CO3 photocatalyst and preparation method thereof
CN106423286A (en) * 2016-09-14 2017-02-22 江南大学 BiOCOOH-Bi2O2CO3 compound photocatalyst and preparation method thereof
CN106423286B (en) * 2016-09-14 2018-08-24 江南大学 A kind of BiOCOOH-Bi2O2CO3Composite photo-catalyst and preparation method thereof
CN106391076B (en) * 2016-09-14 2018-10-16 江南大学 A kind of grey Bi2O2CO3Photochemical catalyst and preparation method thereof
CN106732524A (en) * 2017-02-24 2017-05-31 云南大学 A kind of α/β bismuth oxide phase heterojunction photocatalyst and its preparation method and purposes
CN106732524B (en) * 2017-02-24 2021-01-01 云南大学 Alpha/beta-bismuth oxide phase heterojunction photocatalyst and preparation method and application thereof

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