CN109701563A - A kind of preparation method of bismuth sulfide-bismuth oxybromide magnetism tri compound visible light catalyst - Google Patents
A kind of preparation method of bismuth sulfide-bismuth oxybromide magnetism tri compound visible light catalyst Download PDFInfo
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Abstract
The present invention relates to a kind of bismuth sulfide-bismuth oxybromide magnetism tri compound visible light catalyst preparation methods, belong to inorganic catalysis material technical field.It is primarily characterized in that and magnetic coupling Bi is prepared using one step hydro thermal method2S3/ BiOBr visible light catalyst, wherein the p-n heterojunction formed between catalyst effectively inhibits compound, the SrFe in light induced electron and hole12O19And Bi2S3Addition be conducive to make the optical response range of catalyst to broaden, and catalyst stability is strong, can recycle and reuse;Catalyst preparation conditions are mild, are not related to other organic matters, and the catalyst preparation used time is few, and magnetic composite is convenient for recycling.SrFe12O19/Bi2S3/ BiOBr irradiates 20min under visible light, makes the degradation rate for simulating organic pollutant rhodamine B up to 91.6%, magnetic Bi is not added2S3The degradation efficiency of/BiOBr is only 73.8%, and can be separated and recovered by simple externally-applied magnetic field, average recovery rate 82.3%, and catalyst after the recovery has good photocatalytic activity.
Description
Technical field
The present invention relates to a kind of bismuth sulfide-bismuth oxybromide magnetism tri compound visible light catalyst preparation methods, belong to
Inorganic catalysis material technical field.
Background technique
It is well known that photocatalysis technology has, low energy consumption, easy to operate, reaction condition is mild, at normal temperatures and pressures can
To carry out, research hotspot is had become in processing environment problem.Bismuth series photocatalyst is as a kind of novel visible light photocatalysis
There is layer structure and reasonable band gap width widely to be paid close attention to for agent, and bismuth based compound common at present has BiOX, vulcanization
Bismuth, bismuth oxide, bismuth molybdate, pucherite etc..BiOX (BiOX, X=Cl, Br, I) is used as p-type semiconductor, with preparation method
Simply, the features such as photocatalysis effect is good, nontoxic and receive much attention.Wherein bismuth oxybromide (BiOBr) visible light region have response,
And forbidden bandwidth is moderate, is a kind of indirect semiconductor, before these advantages make it have greatly application in visible light catalytic material
Scape.But there are the visible light utilization efficiencies low, hole BiOBr and electronics are easy the disadvantages of compound, conduction band positions are too positive, make it in environment
It is restricted with the application in the fields such as the energy.Therefore, modified to BiOBr to increase its visible light utilization efficiency, and hinder hole
Compound with electronics, the reducing power for improving light induced electron is fundamental starting point of the invention.
Bismuth sulfide (Bi2S3) it is a kind of important layered semiconductor material, in thermoelectricity, electronics and opto-electronic device and red
There is potential using value in external spectrum.In addition, its band-gap energy is 1.2eV-1.7eV, it is a kind of potentially to visible light
The photochemical catalyst of response.But since its valence band and conduction band positions are closer, photo-generate electron-hole recombination rate is high, therefore single
Bismuth sulfide photocatalysis efficiency it is lower.By Bi2S3Compound is formed for BiOBr modification, BiOBr can be enhanced to visible light
Responding ability.
Usually there is a problem of catalyst recycling hardly possible during photocatalytic degradation organic wastewater.Photochemical catalyst in order to prevent
Recycling is not thorough and generates secondary pollution, and reduces use cost, and photochemical catalyst is assigned magnetic, convenient for separating and recovering and recycling is
Very necessary.SrFe12O19As typical retentive material, saturation magnetization with higher, and photocatalysis is generated
Synergistic effect;Magnetic strontium ferrite is loaded into Bi2S3On-BiOBr compound, photocatalytic activity not only can be improved, but also be conducive to catalysis
The recycling of agent.
It has not yet to see about magnetic Bi2S3The research of/BiOBr composite catalyst is reported.Existing Bi2S3/BiOBr
The preparation method of composite photo-catalyst, such as: in volume 290 page 233-239 of " Applied Surface Science " the 2014th
" Photocatalytic activities of Bi2S3/BiOBr nanocomposites synthesized by a
Facile hydrothermal process " (documents 1), preparation method are with bismuth nitrate, thiocarbamide, ethylene glycol and bromine
Change potassium is raw material, reacts in water heating kettle and obtains for 24 hours, and this method has the disadvantage that (1) using inorganic reagent and organic reagent
Hybrid reaction prepare sample, occur that pattern is uneven (shape appearance figure that Wen Zhongwei provides product), and the reaction time is too long;(2) sample
Gas chromatography (thiocarbamide, ethylene glycol, ethyl alcohol) has been used in product preparation process, can generate peculiar smell and stink, while generating highly concentrated
Nitrogenous organic wastewater is spent, environmental-friendly requirement is not met;(3) lower to the degradation rate of methyl orange under visible light, 0.05g is compound
Catalyst degradation 40mL concentration is 3.05 × 10-5mol·L-1The methyl orange solution of (10mg/L), 2h degradation rate only 60%.(4)
The recovery method and the rate of recovery of catalyst are not provided.
For another example the document: " One-pot in volume 5 page 16239-16249 of " RSC Advances " the 2015th
synthesis of heterostructured Bi2S3/BiOBr microspheres with highly efficient
Visible light photocatalytic performance " (documents 2), preparation method are with bismuth nitrate, sulphur
Urea and potassium bromide are raw material, prepare Bi using solvent-thermal method2S3/BiOBr.This method has the disadvantage that (1) entirely synthesized
Cheng Jun is carried out in 2-methyl cellosolve (solvent), and solvent-thermal method prepares the higher cost of catalyst, and manufacturing cycle is longer, synthesis
With drying is each needs 12h;(2) limited activity of the composite catalyst, under visible light illumination, 100mg catalyst degradation 100ml are dense
When degree is the rhodamine B of 50mg/L, 80min degradation rate is 98.6%;(3) use thioacetamide as sulphur source, 2- methoxyl group second
Alcohol causes to generate stink substances in reaction process as solvent, and the solvent for filtering generation after reaction is hazardous waste, is not inconsistent
Close clean manufacturing requirement.
For another example in the 69-77 pages of volume 224 of document " Materials Science and Engineering B " 2017
“In situ synthesis of a nanoplate-like Bi-based heterojunction for
Photocatalytic degradation of ciprofloxaci " (documents 3) preparation method: is first added with water-bath
Thermal method prepares single BiOBr, after be added thioacetamide in the BiOBr of preparation, then using water bath heating by from
Sub- exchange reaction prepares Bi2S3/BiOBr.This method has the disadvantage that (1) takes and two-step method is wanted to prepare, and each step requires
Heating reaction, drying, experiment flow are cumbersome and time-consuming for a long time.(2) degradation of the composite catalyst prepared to Ciprofloxacin
Ciprofloxacin aqueous solution not high, that 50mg compound is 10mg/L to 100mL concentration, it is seen that 3h degradation rate is less than under light
80%.(3) gas chromatography (thioacetamide, ethylene glycol, ethyl alcohol) has been used in sample preparation procedure, can have been generated and stink,
And the nitrogenous organic wastewater of high concentration is generated, do not meet environmental-friendly requirement.Therefore, SrFe is prepared using hydro-thermal method12O19, and it is excellent
Change Bi2S3The preparation method of/BiOBr, then SrFe12O19With Bi2S3The compound improvement Bi of/BiOBr2S3The catalytic effect of/BiOBr returns
Yield and magnetic stability are very necessary.
Summary of the invention
The invention belongs to semiconductor visible light catalysis material field, it is related to preparing magnetic coupling using one step hydro thermal method
Bi2S3/ BiOBr visible light catalyst makes to urge wherein the p-n heterojunction formed effectively inhibits the compound of light induced electron and hole
The optical response range of agent broadens, and catalyst stability is strong, can be recycled, preparation condition is mild, and the used time is few, magnetic coupling
Material is convenient for recycling.
Bi of the invention2S3/BiOBr/SrFe12O19Composite visible light catalyst the preparation method is as follows:
Weigh the Bi (NO of 2mmol3)3It is molten to obtain in the nitric acid solution of 2mol/L that 10mL concentration is dissolved into the PVP of 0.1g
Liquid A, the NaBr for weighing 2mmol, which is dissolved into the sodium hydroxide solution that 10mL concentration is 2mol/L, obtains solution B, weighs
0.3mmol vulcanized sodium is dissolved into 10mL water and obtains solution C;Solution A is added in solution B, and with the hydroxide of 2mol/L
It is 5~9, after 30min is sufficiently stirred that sodium solution, which adjusts pH, and solution C is added, and after 1h is stirred by ultrasonic, adds 0.03~0.12g's
SrFe12O19, it is sufficiently stirred to obtain suspension D;Suspension D is put into 100mL reaction kettle, reacts 4h at 140~180 DEG C,
Room temperature is naturally cooled to, is filtered, is washed with deionized and is put into 60 DEG C of oven drying 8h for several times to get to Bi2S3/BiOBr/
SrFe12O19Composite visible light catalyst.
The present invention by adopting the above technical scheme, mainly has the following effects:
(1) the magnetic coupling Bi of the method for the present invention preparation2S3/BiOBr/SrFe12O19Visible light catalyst is a step hydro-thermal
Synthesis, simple compared with documents 1, documents 2 and 3 step of documents, reaction condition is mild, and the reaction time is short, and is not required to
Want organic solvent.
(2) the magnetic coupling Bi of the method for the present invention preparation2S3/BiOBr/SrFe12O19The epigranular of visible light catalyst,
Stability is good, can be separated and recovered by simple externally-applied magnetic field, average recovery rate 82.3%, and may be reused.
(3) the magnetic coupling Bi of the method for the present invention preparation2S3/BiOBr/SrFe12O19The catalytic performance of visible light catalyst,
Relative to single Bi2S3And BiOBr, catalytic effect increase significantly, and irradiate 20min under visible light, rhodamine B
For degradation rate up to 91.6%, this result is substantially better than the result of documents 1 Yu documents 2.
Detailed description of the invention
Fig. 1 is the Bi that embodiment 2 is prepared2S3/BiOBr、Bi2S3/BiOBr/SrFe12O19The X of composite visible light catalyst
X ray diffration pattern x (XRD).
Fig. 2 is the Bi that embodiment 2 is prepared2S3/BiOBr/SrFe12O19The infrared spectrogram of composite visible light catalyst
(FTIR)。
Fig. 3 is the Bi that embodiment 2 is prepared2S3/BiOBr、Bi2S3/BiOBr/SrFe12O19Composite visible light catalyst pair
Rhodamine B Photocatalytic Degradation Property test curve.
Fig. 4 is Bi prepared by embodiment 22S3/BiOBr/SrFe12O19The VSM map of composite visible light catalyst.
Fig. 5 is Bi prepared by embodiment 22S3/BiOBr/SrFe12O19The recycling and reusing of composite visible light catalyst is degraded
Effect contrast figure.
Specific embodiment
With reference to embodiment, the present invention is further illustrated.
Embodiment 1
A kind of preparation of bismuth sulfide-bismuth oxybromide magnetism tri compound visible light catalyst, the specific steps are as follows:
Weigh the Bi (NO of 2mmol3)3It is molten to obtain in the nitric acid solution of 2mol/L that 10mL concentration is dissolved into the PVP of 0.1g
Liquid A, the NaBr for weighing 2mmol, which is dissolved into the sodium hydroxide solution that 10mL concentration is 2mol/L, obtains solution B, weighs
0.3mmol vulcanized sodium is dissolved into 10mL water and obtains solution C;Solution A is added in solution B, and with the hydroxide of 2mol/L
It is 5, after 30min is sufficiently stirred that sodium solution, which adjusts pH, and solution C is added, and after 1h is stirred by ultrasonic, adds the SrFe of 0.03g12O19,
It is sufficiently stirred to obtain suspension D;Suspension D is put into 100mL reaction kettle, 4h is reacted at 140 DEG C, naturally cools to room
Temperature filters, and is washed with deionized and is put into 60 DEG C of oven drying 8h for several times to get to Bi2S3/BiOBr/SrFe12O19It is compound
Visible light catalyst.
Embodiment 2
A kind of preparation of bismuth sulfide-bismuth oxybromide magnetism tri compound visible light catalyst, the specific steps are as follows:
Weigh the Bi (NO of 2mmol3)3It is molten to obtain in the nitric acid solution of 2mol/L that 10mL concentration is dissolved into the PVP of 0.1g
Liquid A, the NaBr for weighing 2mmol, which is dissolved into the sodium hydroxide solution that 10mL concentration is 2mol/L, obtains solution B, weighs
0.3mmol vulcanized sodium is dissolved into 10mL water and obtains solution C;Solution A is added in solution B, and with the hydroxide of 2mol/L
It is 7, after 30min is sufficiently stirred that sodium solution, which adjusts pH, and solution C is added, and after 1h is stirred by ultrasonic, adds the SrFe of 0.06g12O19,
It is sufficiently stirred to obtain suspension D;Suspension D is put into 100mL reaction kettle, 4h is reacted at 160 DEG C, naturally cools to room
Temperature filters, and is washed with deionized and is put into 60 DEG C of oven drying 8h for several times to get to Bi2S3/BiOBr/SrFe12O19It is compound
Visible light catalyst.
Embodiment 3
A kind of preparation of bismuth sulfide-bismuth oxybromide magnetism tri compound visible light catalyst, the specific steps are as follows:
Weigh the Bi (NO of 2mmol3)3It is molten to obtain in the nitric acid solution of 2mol/L that 10mL concentration is dissolved into the PVP of 0.1g
Liquid A, the NaBr for weighing 2mmol, which is dissolved into the sodium hydroxide solution that 10mL concentration is 2mol/L, obtains solution B, weighs
0.3mmol vulcanized sodium is dissolved into 10mL water and obtains solution C;Solution A is added in solution B, and with the hydroxide of 2mol/L
It is 9, after 30min is sufficiently stirred that sodium solution, which adjusts pH, and solution C is added, and after 1h is stirred by ultrasonic, adds the SrFe of 0.12g12O19,
It is sufficiently stirred to obtain suspension D;Suspension D is put into 100mL reaction kettle, 4h is reacted at 180 DEG C, naturally cools to room
Temperature filters, and is washed with deionized and is put into 60 DEG C of oven drying 8h for several times to get to Bi2S3/BiOBr/SrFe12O19It is compound
Visible light catalyst.
Experimental result
Bi prepared by embodiment 22S3/BiOBr/SrFe12O19Catalytic degradation activity is best.In order to facilitate comparison, it is prepared for
Bi2S3/ BiOBr sample.Bi2S3/ BiOBr preparation method is to be added without SrFe in embodiment 212O19。
The Bi that embodiment 2 is prepared2S3/BiOBr、Bi2S3/BiOBr/SrFe12O19XRD spectrum it is as shown in Figure 1.It can be with
Find out, compound Bi2S3The diffraction maximum of BiOBr in/BiOBr almost coincide with the diffraction maximum of its standard card (73-2061), is
The BiOBr of tetragonal structure.Its mainly expose crystal face have [001], [011], [012], [110], [020], [014], [114] and
[212], corresponding 2 θ be 10.946 °, 25.260 °, 31.810 °, 32.311 °, 39.432 °, 50.841 °, 56.355 ° and
57.309 °, it is offset not find that the position of diffraction maximum has, illustrates compound Bi2S3Afterwards without the crystal structure of change BiOBr.But
It is the failure to discovery Bi2S3Characteristic diffraction peak, it may be possible to due to Bi2S3Content it is relatively fewer, it is also possible to due to reaction temperature
It is too low to exist in the form of unformed, fail to expose diffraction maximum;Remaining does not have miscellaneous peak appearance.Bi2S3/BiOBr/SrFe12O19It is multiple
Close that expose BiOBr [001], [011], [012], [110], [020], [014], [114] in object simultaneously corresponding with [212] crystal face
Standard diffraction peak, while two peaks at 30.325 ° and 34.182 ° respectively correspond SrFe12O19Characteristic peak crystal face
[114] and [110], illustrate that there are SrFe12O19And without other miscellaneous peaks.
The Bi that embodiment 2 is prepared2S3/BiOBr/SrFe12O19FTIR spectrum as shown in Fig. 2, wherein 554.0cm-1With
604.0cm-1Left and right is SrFe12O19Characteristic absorption peak, 490cm-1It is the characteristic absorption peak of Bi-O, 1390cm-1It is in air
CO2Typical symmetrical stretching vibration, 1400cm-1It is nearby the stretching vibration peak of Bi-S, 1600cm-1Neighbouring is physical absorption
The flexural vibrations peak of the H-O-H of water, 3440cm-1It is nearby the stretching vibration peak of catalyst surface-OH.From FT-IR figure again
Secondary proof SrFe other than BiOBr12O19Presence, and also demonstrate the Bi for failing to detect in XRD2S3Presence.
The Bi that embodiment 2 is prepared2S3/BiOBr、Bi2S3/BiOBr/SrFe12O19Visible light catalyst it is dense to 100mL
Test results are shown in figure 3 for rhodamine B (RhB) light degradation property of degree 20mg/L.Work as Bi2S3/ BiOBr after illumination 20min,
Photocatalytic degradation efficiency only has 73.8%, compound 10%SrFe12O19Bi2S3/BiOBr/SrFe12O19Degradation efficiency is reached for
91.6%, illustrate as compound suitable SrFe12O19The photocatalysis performance of photochemical catalyst can be enhanced, on the one hand, due to
SrFe12O19Forbidden bandwidth is lower can be excited under visible light, improve the response intensity to light;It can under illumination condition
To generate light induced electron and hole, and SrFe12O19Position of energy band and compound Bi2S3/ BiOBr is different, can between them
Band difference is generated, the separation of photo-generate electron-hole is conducive to;On the other hand, magnetisable material itself can generate one it is relatively stable
Magnetic field, composite magnetic photochemical catalyst be excited by light occur electron transition when, magnetic field can promote the shunting of light induced electron, thus
The effective separative efficiency for improving light induced electron and hole.
Fig. 4 is the Bi that embodiment 2 is prepared2S3/BiOBr/SrFe12O19Visible light catalyst VSM map, catalyst
Saturation magnetization (Ms) and remanent magnetization (Mr) be respectively 4.247emu/g, 1.521emu/g, coercivity (Hc) is
971.62G, the stronger coercivity of catalyst are derived from its good anti-demagnetization performance, are a kind of retentive materials.In externally-applied magnetic field
Under the action of be conducive to the recycling of catalyst, the averaged rate of recovery of catalyst is 82.3%.
Fig. 5 is the Bi that embodiment 2 is prepared2S3/BiOBr/SrFe12O19Visible light catalyst circulation rear catalyst
Degradation efficiency figure illustrates catalyst it can be seen from the figure that degradation efficiency does not significantly decrease after catalyst circulation use
With preferable stability and reusable.
Claims (4)
1. it is characterized by comprising as follows for a kind of bismuth sulfide-bismuth oxybromide magnetism tri compound visible light catalyst preparation method
Step:
Weigh the Bi (NO of 2mmol3)3It is dissolved into the nitric acid solution that 10mL concentration is 2mol/L with the PVP of 0.1g and obtains solution A,
The NaBr for weighing 2mmol, which is dissolved into the sodium hydroxide solution that 10mL concentration is 2mol/L, obtains solution B, weighs 0.3mmol sulphur
Change sodium, which is dissolved into 10mL water, obtains solution C;Solution A is added in solution B, and is adjusted with the sodium hydroxide solution of 2mol/L
PH is 5~9, after 30min is sufficiently stirred, and solution C is added, and after 1h is stirred by ultrasonic, adds the SrFe of 0.03~0.12g12O19,
It is sufficiently stirred to obtain suspension D;Suspension D is put into 100mL reaction kettle, 4h, natural cooling are reacted at 140~180 DEG C
It to room temperature, filters, is washed with deionized and is put into 60 DEG C of oven drying 8h for several times to get to Bi2S3/BiOBr/SrFe12O19
Composite visible light catalyst.
2. bismuth sulfide according to claim 1-bismuth oxybromide magnetism tri compound visible light catalyst preparation method,
It is characterized in that step is simple, reaction condition is mild, and the reaction time is short, and does not need organic solvent.
3. bismuth sulfide according to claim 1-bismuth oxybromide magnetism tri compound visible light catalyst preparation method,
It is characterized in that the epigranular of catalyst, stability is good, can separate and recover by simple externally-applied magnetic field, average recovery rate is
82.3%, and may be reused.
4. bismuth sulfide according to claim 1-bismuth oxybromide magnetism tri compound visible light catalyst preparation method,
It is characterized in that catalyst irradiates 20min under visible light, the degradation rate of rhodamine B can be made up to 91.6%, catalysis with higher
Activity.
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