CN109794271A - A kind of ultra-thin PbBiO of oxygen-enriched defect2The preparation method and its usage of Br nanometer sheet - Google Patents
A kind of ultra-thin PbBiO of oxygen-enriched defect2The preparation method and its usage of Br nanometer sheet Download PDFInfo
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Abstract
The invention belongs to field of photocatalytic material, disclose a kind of ultra-thin PbBiO of oxygen-enriched defect2The preparation method and its usage of Br nanometer sheet.It for bromine source, bismuth nitrate is bismuth source that this catalyst, which uses response type bromination 1- cetyl -3- methylimidazole, plumbi nitras is lead source, polyvinylpyrrolidone is surfactant, passes through solvent structure in water, mannitol and alcohol mixed solution.Product is through supercooling, filtering and washing, and ultra-thin PbBiO can be obtained in drying in air2Br nanometer sheet.The PbBiO2Br nanometer sheet material of the method for the present invention preparation shows single cell thickness about 1.2nm, with splendid photocatalysis performance, it can be achieved that efficient degradation to organic pollutant under radiation of visible light of the wavelength greater than 400nm.The synthetic method is low in cost, it is simple and easy, environmentally protective, be easy to control.
Description
Technical field
The invention belongs to material preparation and photocatalysis technology application field, kind of the oxygen-enriched ultra-thin PbBiO of defect is refered in particular to2Br nanometers
The preparation method and applications of piece.
Background technique
From 1972 in TiO2Since finding photocatalytic cleavage water on electrode, due to industrializing the adverse effect day to environment
Benefit enhancing, effective use of the solar energy during photocatalysis depollution of environment have caused extensive research interest.In the past
Decades in, developed various strategies to improve the degradation efficiencies that sunlight irradiates lower pollutant, such as: doping, half
Conductor is compound, photosensitizer, noble metal loading etc..By crystal face feature (such as atomic arrangement, electronic structure) to photocatalyst activity
The inspiration of influence, people produce greatly the defect for adjusting photochemical catalyst to optimize the light-catalyzed reaction activity of Driven by Solar Energy
Interest.But how Effective Regulation defect is come to expose more active sites be still the difficulty in photochemical catalyst preparation process
Point.
In the recent period, two-dimensional material is due to its specific surface area high relative to corresponding body phase material and more non-coordination surface originals
Son, in photoelectronics, energy stores, potential application in the fields such as catalysis and receive significant attention.In addition, two-dimensional material surface
Upper exposed atom is easy to from lattice evolution and forms vacancy, this largely will affect the physics and chemically of catalyst
Matter.Therefore, many researchs are dedicated to that stratified material is removed to obtain single layer samples, or directly synthesize ultrathin nanometer piece,
To explore the potentiality of their higher performances.
As a kind of novel stratiform quaternary oxide semiconductor, bromine oxygen bismuth lead (PbBiO2Br it) causes recently greatly
Concern, because it is with excellent photocatalysis performance, high chemistry and optical stability are at low cost and corrosion-resistant.
PbBiO2Br is by [PbBiO2]2+Layer and intersect at what double bromine atom layers therein were constituted along [001] direction.So far, respectively
The PbBiO of the micro-/micro-nano structure of kind2Br material is produced, such as flower-like microsphere, nanometer sheet, unformed block structure etc..However, mesh
Preceding related ultra-thin PbBiO2The preparation method of Br nanometer sheet and tactful document and the patent report not yet for introducing defect state structure
Road.For this purpose, probing into a kind of ultra-thin PbBiO of simple, effective preparation structure containing defect state2Br nanometer sheet, Lai Tigao photocatalysis
The efficiency of degradation of contaminant is meaningful.
Summary of the invention
Mild, simple, cheap, green the ultra-thin PbBiO of oxygen-enriched defect is prepared the object of the present invention is to provide a kind of2Br receives
The method of rice piece.And PbBiO is adjusted by hydro-thermal, adjusting solution acid-basicity2The thickness of Br and opposite oxygen defect concentration.And
It is used for improving the catalytic efficiency of Visible Light Induced Photocatalytic organic pollutants in water body.
Technical solution of the present invention:
A kind of ultra-thin PbBiO of oxygen-enriched defect2The preparation method of Br nanometer sheet, comprising the following steps:
(1) use plumbi nitras or lead acetate for lead source；Bismuth nitrate, bismuth acetate or bismuth and ammonium citrate are bismuth source；Then add again
Enter a certain amount of polyvinylpyrrolidone, in the in the mixed solvent wiring solution-forming A of sweet dew alcohol and water；
(2) using bromo ionic liquid or inorganic bromide as bromine source, the wiring solution-forming B in alcohol solvent；
(3) it by the solution B in step (2), is added dropwise in the solution A in step (1), and persistently stir to get mixing
Solution C；
(4) solution C is poured into the autoclave equipped with village in polytetrafluoroethylene (PTFE) and is reacted a few hours, cooling, centrifugation, then
It is washed respectively with deionized water and dehydrated alcohol, drying obtains the ultra-thin PbBiO of oxygen-enriched defect2Br nanometer sheet catalyst.
In step (1), lead source in mixed solution A: bismuth source: polyvinylpyrrolidone: mannitol: the amount ratio of water are as follows:
0.5mmol:0.5mmol:0.2g:3mmol:30mL。
In step (2), the amount ratio of bromo ionic liquid or inorganic bromide and dehydrated alcohol are as follows: 0.5mmol:10mL.Step
Suddenly in (2), described for bromo ionic liquid is bromination 1- cetyl -3- methylimidazole, bromination 1- dodecyl -3- methyl
Imidazoles, bromination 1- myristyl -3- methylimidazole, bromination 1- hexyl -2,3- methylimidazole, bromination 1- hexyl -3- methylimidazole,
Bromination 1- allyl -3- butyl imidazole, bromination 1- allyl -3- ethyl imidazol(e), bromination 1- allyl -3- methylimidazole, bromination
1- decyl -3- methylimidazole, bromination 1- carboxyethyl -3- methylimidazole, bromination 1- carboxymethyl -3- methylimidazole, bromination 1- amine third
Base -3- methylimidazole, bromination 1- amine ethyl-3-methylimidazole, bromination 1- benzyl -3- methylimidazole, bromination 1- octyl -3- methyl
Imidazoles, bromination N- butyl-N- crassitude, bromination 1- amyl -3- methylimidazole, bromination N- octylpyridinium, bromination 1- butyl -
3- methylimidazole, bromination 1- propyl -3- methylimidazole, 1-ethyl-3-methyllimidazolium bromide, bromination 1- ethyl diethyldithiocarbamate ether -3- first
Base imidazoles, bromination 1- ethyl-methyl ether -2-methylimidazole, bromination 1- vinyl -3- butyl imidazole, bromination 1- vinyl -3- second
Base imidazoles, bromination 1- ethyl acetate base -3- methylimidazole, bromination N- butyl-pyridinium, bromination N- ethylpyridine, bromination N- hexyl pyrrole
Pyridine；The inorganic bromide is potassium bromide or sodium bromide.
In step (3), lead source: bismuth source: the ratio between the amount of substance in bromine source are as follows: 1:1:1；The time persistently stirred is 30-60
Minute.
In step (4), the reaction temperature of autoclave is 140-180 DEG C, and the reaction time is 12-24 hours.
In step (4), drying temperature is 50-60 DEG C, and drying time is 12-24 hours.
The ultra-thin PbBiO of oxygen-enriched defect of the present invention2Br nanometer sheet catalyst thickness about 1.2nm.
The ultra-thin PbBiO of oxygen-enriched defect prepared by the present invention2Br nanosheet photocatalyst is used for photocatalytically degradating organic dye
Rhodamine B.
The invention has the benefit that
The controllable PbBiO for being prepared for oxygen-enriched defect report unit cell thickness of the mild solvent-thermal method of first passage2Br nanometer sheet.
Compared to the PbBiO of few oxygen defect single cell thickness2Br nanometer sheet and bulk PbBiO2Br, oxygen-enriched defect monocrystalline
The PbBiO of born of the same parents' thickness2Br nanometer sheet shows the activity of excellent visible light photocatalytic degradation rhodamine B and Ciprofloxacin.
Detailed description of the invention:
Fig. 1 is prepared PbBiO2The XRD diagram of Br catalyst.
Fig. 2 is the ultra-thin PbBiO of oxygen-enriched defect2SEM, TEM and AFM of Br nanometer sheet scheme.
Fig. 3 is few ultra-thin PbBiO of oxygen defect2SEM, TEM and AFM of Br nanometer sheet scheme.
Fig. 4 is body phase PbBiO2The SEM of Br nano particle schemes.
Fig. 5 is prepared PbBiO2Electron paramagnetic resonance (EPR) map of Br catalyst.
Fig. 6 is prepared PbBiO2The high-resolution O 1s map of Br catalyst.
Fig. 7 is to prepare PbBiO under radiation of visible light2Degradation curve of the Br catalyst to rhodamine B.
Fig. 8 is to prepare PbBiO under radiation of visible light2Degradation curve of the Br catalyst to Ciprofloxacin.
Specific embodiment:
The present invention is described in further details with specific embodiment with reference to the accompanying drawings of the specification.
Embodiment 1:
PbBiO2The preparation and its Photocatalytic Performance Study of Br catalyst, include the next steps:
Take that 0.5mmol plumbi nitras, 0.5mmol bismuth nitrate, that 0.2g polyvinylpyrrolidone is added to 30mL mannitol is water-soluble
Wiring solution-forming A in liquid (0.1mol/L).In another container, 0.5mmol bromination 1- cetyl -3- methylimidazole is taken, it is molten
Solution wiring solution-forming B in 10mL dehydrated alcohol.Solution B is added dropwise in solution A, obtained mixed solution continues to stir
After 30 minutes, mixed solution is poured into the 50mL autoclave equipped with village in polytetrafluoroethylene (PTFE), it is small that 24 are reacted at 160 DEG C
When.Then just kettle will be answered to be cooled to room temperature, precipitating is centrifuged, is respectively washed three times with water and dehydrated alcohol, last product is 60
It is 12 hours dry in DEG C, obtain the ultra-thin PbBiO of oxygen-enriched defect2Br nanometer sheet (ROV-PbBiO2Br)。
Embodiment 2:
Take the ultra-thin PbBiO of the oxygen-enriched defect of 0.5g2Br nanometer sheet is by ultrasound and is dispersed with stirring in 20mL deionized water, will
Obtained mixing suspension is poured into the 25mL autoclave equipped with village in polytetrafluoroethylene (PTFE), is reacted 12 hours at 140 DEG C.
Then just kettle will be answered to be cooled to room temperature, precipitating is centrifuged, is respectively washed three times with water and dehydrated alcohol, last product is in 60 DEG C
It is 12 hours dry, obtain few ultra-thin PbBiO of oxygen defect2Br nanometer sheet (POV-PbBiO2Br)。
Embodiment 3:
Take that 0.5mmol plumbi nitras, 0.5mmol bismuth nitrate, that 0.2g polyvinylpyrrolidone is added to 30mL mannitol is water-soluble
Wiring solution-forming A in liquid (0.1mol/L).In another container, 0.5mmol bromination 1- cetyl -3- methylimidazole is taken, it is molten
Solution wiring solution-forming B in 10mL dehydrated alcohol.Solution B is added dropwise in solution A, solution C is obtained.5mL ammonium hydroxide is taken, is added dropwise
Into solution C, after obtained mixed solution continues stirring 30 minutes, mixed solution is poured into equipped with village in polytetrafluoroethylene (PTFE)
In 50mL autoclave, reacted 24 hours at 180 DEG C.Then just kettle will be answered to be cooled to room temperature, will precipitating centrifugation, with water and
Dehydrated alcohol respectively washs three times, and last product is 12 hours dry in 60 DEG C, obtains body phase PbBiO2Br nano particle
(Bulk-PbBiO2Br)。
Fig. 1 is PbBiO prepared by the embodiment of the present invention 1~32The XRD diagram of Br.As can be seen that three catalyst are in
Existing diffraction maximum is consistent with standard card JCPDS No.38-1008, shows that prepared catalyst is pure PbBiO2Br material
Material.
Fig. 2 is oxygen-enriched defect PbBiO2SEM (Fig. 2 a), TEM (Fig. 2 b and 2c) and AFM (Fig. 2 d) figure of Br.From Fig. 2 a
With 2b as can be seen that prepared oxygen-enriched defect PbBiO2Br material is nanometer chip architecture.Fig. 2 c and 2d show oxygen-enriched defect
PbBiO2The thickness of Br nanometer sheet is about 1.2 nanometers.
Fig. 3 is few oxygen defect PbBiO2SEM (Fig. 3 a), TEM (Fig. 3 b and 3c) and AFM (Fig. 3 d) figure of Br.From Fig. 3 a
With 3b as can be seen that prepared oxygen-enriched defect PbBiO2Br material is nanometer chip architecture.Fig. 3 c and 3d show oxygen-enriched defect
PbBiO2The thickness of Br nanometer sheet is about 1.2 nanometers.
Fig. 4 is body phase PbBiO2The SEM of Br schemes.As can be seen from Figure 4 body phase PbBiO2The thickness of Br is about 100 nanometers
Fig. 5 is prepared PbBiO2The EPR map of Br material.Sample shows epr signal at g=2.001, and it can be known
The electronics on oxygen defect Wei not captured.ROV PbBiO2Highest signal strength, Bulk PbBiO is presented in Br material2Br material
Signal strength be minimum.This shows ROV PbBiO2Br material has highest oxygen defect concentration, POV PbBiO2Br times
It, and Bulk PbBiO2The oxygen defect concentration of Br material is minimum.
Fig. 6 is prepared PbBiO2The XPS high-resolution map of the O 1s of Br material.531.1eV corresponds to attached with oxygen defect
Close oxygen atom, the oxygen atom that 529.3eV corresponds near non-oxygen defect calculates ratio shared by two peaks, to compare catalyst
The size of middle oxygen vacancy concentration.As can be seen that ROV PbBiO in figure2The ratio that peak area in Br material at 531.1eV accounts for is most
(43.88%) greatly, POV PbBiO2Br takes second place (36.10%), Bulk PbBiO2Br minimum (27.78%).This also demonstrates ROV
PbBiO2Br material contains most oxygen defect concentration.
Fig. 7 is prepared PbBiO2Br material under visible light illumination scheme by the active of rhodamine B degradation.By 120 minutes
Radiation of visible light, the rich ultra-thin PbBiO of defect2Br nano material can realize 100% degradation of target contaminant.Few defect is ultra-thin
PbBiO2Br nano material and body phase PbBiO2Br material only realizes 70.2% He of target contaminant (rhodamine B) respectively
20.24% degradation.
Fig. 8 is prepared PbBiO2Br material degrade under visible light illumination Ciprofloxacin activity figure.By 150 minutes
Radiation of visible light, the rich ultra-thin PbBiO of defect2Br nano material can realize 41.73% degradation of target contaminant.Few defect is super
Thin PbBiO2Br nano material and body phase PbBiO2Br material only realizes 27.09% He of target contaminant (Ciprofloxacin) respectively
5.56% degradation.
Claims (9)
1. a kind of ultra-thin PbBiO of oxygen-enriched defect2The preparation method of Br nanometer sheet, which comprises the following steps:
(1) use plumbi nitras or lead acetate for lead source；Bismuth nitrate, bismuth acetate or bismuth and ammonium citrate are bismuth source；Then one is added
Quantitative polyvinylpyrrolidone, in the in the mixed solvent wiring solution-forming A of sweet dew alcohol and water；
(2) using bromo ionic liquid or inorganic bromide as bromine source, the wiring solution-forming B in alcohol solvent；
(3) it by the solution B in step (2), is added dropwise in the solution A in step (1), and persistently stir to get mixed solution
C；
(4) solution C is poured into the autoclave equipped with village in polytetrafluoroethylene (PTFE) and is reacted a few hours, cooling, centrifugation, then spend
Ionized water and dehydrated alcohol wash respectively, and drying obtains the ultra-thin PbBiO of oxygen-enriched defect2Br nanometer sheet catalyst.
2. a kind of oxygen-enriched ultra-thin PbBiO of defect as described in claim 12The preparation method of Br nanometer sheet, which is characterized in that step
Suddenly in (1), lead source in mixed solution A: bismuth source: polyvinylpyrrolidone: mannitol: the amount ratio of water are as follows: 0.5mmol:
0.5mmol:0.2g:3mmol:30mL。
3. a kind of oxygen-enriched ultra-thin PbBiO of defect as described in claim 12The preparation method of Br nanometer sheet, which is characterized in that step
Suddenly in (2), the amount ratio of bromo ionic liquid or inorganic bromide and dehydrated alcohol are as follows: 0.5mmol:10mL.
4. a kind of oxygen-enriched ultra-thin PbBiO of defect as claimed in claim 1 or 32The preparation method of Br nanometer sheet, which is characterized in that
In step (2), described for bromo ionic liquid is bromination 1- cetyl -3- methylimidazole, bromination 1- dodecyl -3- first
Base imidazoles, bromination 1- myristyl -3- methylimidazole, bromination 1- hexyl -2,3- methylimidazole, bromination 1- hexyl -3- methyl miaow
Azoles, bromination 1- allyl -3- butyl imidazole, bromination 1- allyl -3- ethyl imidazol(e), bromination 1- allyl -3- methylimidazole, bromine
Change 1- decyl -3- methylimidazole, bromination 1- carboxyethyl -3- methylimidazole, bromination 1- carboxymethyl -3- methylimidazole, bromination 1- amine
Propyl -3- methylimidazole, bromination 1- amine ethyl-3-methylimidazole, bromination 1- benzyl -3- methylimidazole, bromination 1- octyl -3- first
Base imidazoles, bromination N- butyl-N- crassitude, bromination 1- amyl -3- methylimidazole, bromination N- octylpyridinium, bromination 1- fourth
Base -3- methylimidazole, bromination 1- propyl -3- methylimidazole, 1-ethyl-3-methyllimidazolium bromide, bromination 1- ethyl diethyldithiocarbamate ether -3-
Methylimidazole, bromination 1- ethyl-methyl ether -2-methylimidazole, bromination 1- vinyl -3- butyl imidazole, bromination 1- vinyl -3-
Ethyl imidazol(e), bromination 1- ethyl acetate base -3- methylimidazole, bromination N- butyl-pyridinium, bromination N- ethylpyridine, bromination N- hexyl
Pyridine；The inorganic bromide is potassium bromide or sodium bromide.
5. a kind of oxygen-enriched ultra-thin PbBiO of defect as described in claim 12The preparation method of Br nanometer sheet, which is characterized in that step
Suddenly in (3), lead source: bismuth source: the ratio between the amount of substance in bromine source are as follows: 1:1:1；The time persistently stirred is 30-60 minutes.
6. a kind of oxygen-enriched ultra-thin PbBiO of defect as described in claim 12The preparation method of Br nanometer sheet, which is characterized in that step
Suddenly in (4), the reaction temperature of autoclave is 140-180 DEG C, and the reaction time is 12-24 hours.
7. a kind of oxygen-enriched ultra-thin PbBiO of defect as described in claim 12The preparation method of Br nanometer sheet, which is characterized in that step
Suddenly in (4), drying temperature is 50-60 DEG C, and drying time is 12-24 hours.
8. a kind of ultra-thin PbBiO of oxygen-enriched defect2Br nanometer sheet, which is characterized in that be by any one of claim 1~7 system
Made from Preparation Method, the ultra-thin PbBiO2Br nanometer sheet is rich in oxygen defect and thickness about 1.2nm.
9. a kind of oxygen-enriched ultra-thin PbBiO of defect as claimed in claim 82The purposes of Br nanometer sheet, which is characterized in that used
In photocatalytically degradating organic dye rhodamine B or Ciprofloxacin.
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