CN104826637B - Preparation method of BiOBr/Bi2O3 heterojunction composite catalyst - Google Patents
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Abstract
The invention relates to a preparation method of a BiOBr/Bi2O3 heterojunction composite catalyst and belongs to the technical field of composite materials and photocatalysis. In the method, through in-situ hydrolysis on the surface of Bi2O3 to synthesize BiOBr, the BiOBr/Bi2O3, of which the surface is in a layered 3D nano-structure, is formed, wherein the support capacity of the BiOBr in the composite catalyst can be regulated through adjustment of the pH of the system and the molar ratio of Bi2O3 to HB3. An experimental result proves that when the pH of the system is 4-8 and the molar ratio of Bi2O3 to HB3 is 1:1.4-1:2, the support capacity of the BiOBr/Bi2O3 composite catalyst is 65-85%, wherein an excellent photo-catalytic performance is achieved when the support capacity of BiOBr is in the range. The catalyst has application potential in the field of waste water treatment and organic pollutant degradation. In addition, the catalyst is very easy to separate and is free of obvious loss after three times of recycle usage.
Description
Technical field
The invention belongs to field of compound material and photocatalysis technology field, are related to a kind of BiOBr/Bi2O3Hetero-junctions is compound to urge
The preparation method of agent.
Background technology
With global pollution and energy shortage problem, find sunlight as direct energy source environmental treatment technology into
For the study hotspot of today's society；Used as environmentally friendly photocatalyst, semi-conducting material is attract more and more people's
Sight.Since Honda-Fujishima in 1972 has found photochemistry electrode, TiO2In the time of nearly half a century in past
Breakthrough progress is had been achieved for as most popular research material.With deepening continuously for research, scientists are simultaneously
Being found that much can more preferably using the photocatalyst of sunlight：Ag/AgBr/BiOBr, Bi/BiOCl, Mn-BiOBr, Fe3O4/
BiOCl, Bi2S3/ BiOCl, Bi2O3/ BiOCl, BiOCl/BiVO4And BiOBr-g-C3N4 Deng.As time goes by, Bi bases
Conductor photocatalysis material is done washing the sight of this more and more people with its excellent layer structure and good chemical stability.
Certain achievement in research is had been achieved in previous decades using the organic pollution in photocatalyst for degrading water body,
Traditional photocatalytic process includes：Produce light induced electron and hole on conduction band and valence band respectively and afterwards in catalyst surface
The chemical reaction of upper generation.For the degraded of dyestuff, however it remains three kinds of possible catalytic mechanisms：Photocatalysis, photosensitization, light
Solution.Affecting the factor of degradating organic dye also has a lot, including the concentration of complex, the species of electrodeless ion, reaction temperature and
PH etc..Numerous with the semiconductor light-catalyst compared with low energy gap width, Bi2O3With its energy gap in 2.4-2.8 millis
The unquestionable only choosing for becoming new Shanxi photocatalyst.
BiOBr is a kind of indirect semiconductor material, and its band system can be about 2.69eV, and do not affected by synthesis condition and
Change.And the pattern and degree of crystallinity of BiOBr materials depends on the temperature and time of Hydrothermal Synthesiss.In degraded methyl orange dye
During this lamellar BiOBr show very high first catalysis activity.Therefore, by BiOBr and Bi2O3It is compounded to form a fixed structure
With the composite of pattern, BiOBr and Bi is made2O3Photocatalysis performance produce collaboration, obtain the material of excellent catalytic performance, have
Prestige has application prospect in terms of the degraded of wastewater treatment and organic pollution.
The content of the invention
It is an object of the invention to provide a kind of BiOBr/Bi2O3The preparation method of hetero-junctions composite catalyst.
First, BiOBr/Bi2O3The preparation of hetero-junctions composite catalyst
It is known that photocatalysis performance is tight with the pattern of material, size, structural nexuss, and the pattern of composite, knot
Structure depends on its preparation method.BiOBr/Bi of the present invention2O3The preparation of hetero-junctions composite catalyst, is by Bi2O3Surface is former
Position hydrolysis BiOBr, forms the BiOBr/Bi that surface is stratiform 3D nanostructured2O3.Specifically preparation technology is：By Bi2O3
In being completely dissolved in HBr solution, pH=4-8 is adjusted with ammonia, in 40 ~ 50 DEG C of h of stirring reaction 0.5 ~ 1, centrifugation, washing, be dried
Afterwards, the h of high-temperature calcination 1 ~ 4 at 200 ~ 400 DEG C, obtains final product BiOBr/Bi2O3Hetero-junctions composite catalyst.
In above-mentioned HBr solution, the concentration of HBr is 0.4 ~ 0.6 molL-1HBr。
The present invention can pass through the pH and Bi of adjustment system2O3Composite catalyst BiOBr/ is adjusted with the mol ratio of HBr
Bi2O3The load capacity of middle BiOBr.Experiment shows, in the pH=4-8, Bi of adjustment system2O3It is 1 with the mol ratio of HBr:1.4~1:2
When, composite catalyst BiOBr/Bi2O3The load capacity of middle BiOBr is between 65 ~ 85%, and BiOBr is in this loading range, table
Reveal excellent photocatalysis performance.
2nd, the crystal structure and morphology analysis of catalyst
1st, XRD analysis
Fig. 1 is the XRD figure of catalyst：(a) Bi2O3；(b)85% BiOBr/Bi2O3, pH=6；(c)75% BiOBr/
Bi2O3, pH=4； (d)75% BiOBr/Bi2O3, pH=6； (e)75% BiOBr/Bi2O3, pH=8； (f)65% BiOBr/
Bi2O3, pH=6.(g)BiOBr.It will be seen from figure 1 that the BiOBr/Bi of different loads amount2O3Complex all occurs in that similar
Diffraction maximum.Such as Fig. 1 a, synthesis can be with standard card JCPDS in 27.4 ° and 33.2 ° of diffraction maximums for occurring respectively：No.
In 41-1449（120）（200）Crystal face is corresponding, has no other diffraction maximums and occurs.The BiOBr and standard card JCPDS of synthesis：
No.73-2061 compares, and belongs to tetragonal phase, other impurity peaks does not also occur, compares all of complex, Wo Menfa
It is existing, Bi2O3Presence do not make the crystal formation of complex change.
2nd, sem analysis
Fig. 2 schemes for the SEM of catalyst：(a) pure Bi2O3；(b) pure BiOBr； (c) BiOBr /Bi2O3, from Fig. 2
A can be seen that Bi2O3It is made up of uniform 2 μm of nanometer sheet, but dispersibility is not fine.But scheme us from b
Can see, the favorable dispersibility of BiOBr, whole pattern presents the structure of single flower-like nanometer piece, is relatively large in diameter, 5
μm or so.Fig. 2 (c) shows that the pattern of complex is 3D layered nano-structure of the diameter in 2 ~ 5 μm of lamellar structure composition,
These granules are made up of irregular smooth nanometer sheet, and the coarse surface for being formed may increase its specific surface area, favorably
In its photocatalysis performance of raising.
3rd, infrared spectrum analysiss
Fig. 3 is BiOBr and 75% pH=6 BiOBr/Bi2O3Infrared spectrogram.From figure 3, it can be seen that in BiOBr and
75% pH=6 BiOBr /Bi2O3Infrared spectrogram in, 520 cm-1The most strong peak for occurring belongs to Bi-Oization in BiOBr
Learn the vibration peak of key；And 75% pH=6 BiOBr/Bi2O3In 432 cm-1That what is occurred is then Bi2O3Characteristic peak.75% BiOBr
/Bi2O3In the BiOBr that occurs simultaneously and Bi2O3Characteristic peak may certify that its presence.
4th, UV Diffuse Reflectance Spectroscopy analysis
Fig. 4 is the UV Diffuse Reflectance Spectroscopy of synthetic catalyst of the present invention.Shown in Fig. 4, compared to it has been reported that data
For, the ABSORPTION EDGE of BiOBr has the trend of red shift, and this may be relevant with synthetic method.BiOBr /Bi2O3The ABSORPTION EDGE of complex
Equally in visible region, compared to pure BiOBr, ABSORPTION EDGE shows the trend for expanding.The ABSORPTION EDGE of pure BiOBr is 455
Nm, corresponding energy gap is 2.68 eV, and ABSORPTION EDGE of the complex of the present invention in visible region has the trend of red shift, forbidden band
Width is most too narrow to 2.12 eV（Shown in Fig. 5）.These phenomenons show, it is more that the architectural feature of hetero-junctions can actually induce generation
Light induced electron and hole, perhaps this can improve its photocatalysis performance.
6th, nitrogen adsorption desorption test
The specific surface area size and pore-size distribution of sample can be obtained by the test of nitrogen adsorption desorption.Table 1 is the ratio table of sample
Area, pore volume, aperture and energy gap tables of data.
Knowable to the data of table 1,75% BiOBr/Bi2O3 (pH=6) specific surface area of sample is 49.96 m2·g-1, greatly
In other samples, as can be seen that BiOBr and Bi from graph of pore diameter distribution2O3Average pore size be distributed in 10 ~ 25 nm, and its
The pore-size distribution of remaining complex is in 5 ~ 12 nm.Comprehensive all of data, 75% BiOBr/Bi2O3 (pH=6) specific surface of sample
Product is maximum, and aperture is also less, therefore it is presumed that, the sample may have most excellent catalytic performance.
3rd, the absorption of catalyst and degradation property are tested
1st, photocatalytic degradation capability test
Using methyl orange organic molecule as BiOBr/Bi2O3The test of complex photocatalyst for degrading ability：Take 60 mg
Catalyst is in the methyl orange aqueous solution of 60 mL（10 mg/L）In, after 5 minutes, the min of dark reaction 30 is ensureing to reach suction for ultrasound
Attached-desorption equilibrium, afterwards in the Xe lamps of 300W（λ >420 nm optical filters）Irradiation, whole course of reaction is all entered at room temperature
OK, take after different irradiation times 5-6 mL solution be placed in a centrifuge 7000 revs/min be centrifuged 3 minutes, take
Clear liquid, using ultraviolet spectrophotometer its concentration is tested.
Fig. 6 is different catalysts in visible ray（λ > 420 nm）Methyl orange concentration during catalytic degradation（MO）Concentration
（C/C0）Time history plot.Original methyl orange concentration is beginning concentration（C0）, from fig. 6 it can be seen that in visible ray
Irradiation under, the reduction degree of MO concentration is clearly.After the min of dark reaction 30, reaction reaches adsorption desorption balance.Passing through
After the min of radiation of visible light 48,75% BiOBr/Bi2O3 (pH=6) it is 93.8% to the removal rate of methyl orange, but identical
Experiment condition under 85% BiOBr/Bi2O3 And 65% BiOBr/Bi (pH=6)2O3 (pH=6) removal rate of methyl orange is distinguished
For 73% and 70%.As a result show, BiOBr/Bi2O3Load percentage in the nanostructured of complex hetero-junctions can be directly affected
Degradation capability of the catalyst to methyl orange.From Fig. 6, we can obtain a result, and catalyst is distinguished the degradation effect of methyl orange
For：75 % BiOBr/Bi2O3 pH=6(ca. 93.8%) > 75% BiOBr/Bi2O3 pH=8 (ca. 86%) >75%
BiOBr/Bi2O3pH=4 (ca.82%;) >Pure BiOBr (ca.80%)>Pure Bi2O3(ca.77%) > 85%
BiOBr/Bi2O3 pH=6 (ca.73%) > 65% BiOBr/Bi2O3pH=6(ca.70%).These results indicate that BiOBr/
Bi2O3If Bi in complex2O3Amount it is not enough, light induced electron and hole cannot be efficiently separated, also cannot bloom urge
Change ability.On the other hand, excessive Bi2O3It is also possible to reduce photocatalysis efficiency, because the Bi of excess2O3It is possible to become light
Raw electronics and the complex centre in hole.
2nd, the acid-base value of solution is for the impact of photo-catalysis capability
In this experiment, we equally have studied the impact of the acid-base value for photo-catalysis capability of solution.When adjust pH be 4,
6th, 8 not etc. when, the photo-catalysis capability of catalyst is also different, and this may be relevant with the degree of crystallinity of sample, is catalyzed in correspondence Fig. 1
The XRD phenetic analysis of agent, when pH is adjusted to 6 from 4, photo-catalysis capability is reduced, correspondence（120）The characteristic peak of crystal face it is strong
Degree is also reduced, and when being adjusted to 8, photo-catalysis capability is improved, correspondence（120）The intensity of the characteristic peak of crystal face is also enhanced.
Under institute's test condition, the degradation rate of methyl orange obeys first order reaction rule：
r = dc/dt = kKc/(1+Kc)
R represents degradation rate, and c represents the concentration of methyl orange after the reaction t times, and t is the response time, and k represents that speed is normal
Number, K represents and reacts synergistic absorption constant, when initial concentration it is very little（0.01 g/L）, above formula can be with letter
Turn to
ln(c0/c) = kKt = kappt
kappRepresent first order reaction speed constant.
The k calculated in the testappAs shown in fig. 7,75 % BiOBr/Bi2O3Observed rate constant urge more than other
Agent, about 0.0462 min-1, compared to 1.83 times of pure BiOBr.With the increase of BiOBr load percentages, catalyst
Catalytic performance also gradually step up, declined again after optimal proportion is reached.
3rd, different light application times are for the impact of photo-catalysis capability
In order to further study Adsorption of Methyl Orange degradation process, we have studied catalyst pattern product of the present invention and do not sharing the same light
According to ultraviolet-visible absorption spectroscopy figure under the time.Fig. 8 is 75 % BiOBr/Bi2O3 PH=6 samples methyl during absorption degradation
Orange absorption spectrum is schemed over time.It is obvious that there is an absworption peak at 464 nm from Fig. 8, with visible
The prolongation of light irradiation time, the intensity of absworption peak is gradually lowered and occurs the trend of blue shift, the color of corresponding methyl orange also from
It is orange gradually become it is colourless.According to document, this blue-shifted phenomenon is mostly due to the methyl orange quilt in photocatalytic process
Light degradation is intermediate product, the reason that afterwards intermediate product is partly degraded again.This fully demonstrates BiOBr/Bi again2O3
Complex has excellent catalytic capability under the irradiation of visible ray to methyl orange.
4th, spectrofluorimetry
The complex BiOBr/Bi using spectrofluorimetry2O3It is compound several with pure BiOBr photo-generate electron-holes pair
Rate, accordingly we can also speculate the size of semi-conducting material photocatalysis performance.Fig. 9 is the luminescence generated by light figure of catalyst.From figure
In can see, excitation wavelength be 320 nm when, BiOBr/Bi2O3And Bi2O3Occurs stronger absorption at 430 nm
Peak, compared to pure BiOBr, the intensity of emission peak substantially weakens, illustrate and between the heterojunction structure that exists construct really drop
The low recombination probability of light induced electron and hole.
5th, the chemical stability test of catalyst
Whether catalyst is stably an important indicator for weighing its researching value, in order to verify its stability, is carried out
The circulation experiment of photocatalytic degradation MO, each circular response adds the MO solution constant volume of isodose to same volume after terminating,
Into the circular response of next round after adsorption equilibrium.Figure 10 is 75 % BiOBr/Bi2O3 PH=6 catalytic cycle experimental result pictures,
Catalytic cycle still remains afterwards good catalysis activity using three times, shows catalyst stabilization preferably, with researching value.
6th, photocatalytic mechanism is explained
Knowable to document, the pollutant that BiOBr can effectively degrade in organic water body under the irradiation of ultraviolet light.For this
The reason for excellent performance of the photocatalyst of invention synthesis, is analyzed, and a kind of reason is likely due to the pattern with layer structure to be made
Its specific surface area can adsorb more dyestuff than larger, while specific surface area is big, can increase more avtive spots, so as to
Be conducive to the raising of photocatalysis performance.On the other hand, because photocatalytic process is being combined and separating based on Pair production, and
The bandgap structure of catalyst and light induced electron and hole pair it is compound with separate it is closely bound up.The position of quasiconductor valence band can lead to
Cross below equation to be calculated：EVB = X – Ee+ 0.5 Eg, EVBThe edge current potential of valence band is represented, X represents that the electricity of quasiconductor is born
Property, it be constitute quasiconductor all atoms electronegativity geometric mean, EeRepresent the standard energy of the free electron of hydrogen（About
For 4.5 eV）, Eg represents the band gap width of quasiconductor, therefore, the edge current potential of rewinding can pass through ECB = EVB- Eg is calculated
Obtain, accordingly, valence band location is in -0.39 Ev and -0.29 eV.While electronics and hole are between different quasiconductors
Transfer increased life-span of carrier, improve the efficiency of catalyst surface electric charge transfer, therefore, constructed hetero-junctions connects
The transmission in Lian Chu holes can be effectively improved.Additionally, used as the dominant response part in catalytic reaction, BiOBr is located at complex
Outside, therefore, reactivity site is not limited to the forming position of hetero-junctions.
Description of the drawings
Fig. 1 is the XRD figure of catalyst：(a) Bi2O3; (b)85% BiOBr/Bi2O3, pH=6; (c)75% BiOBr/
Bi2O3, pH=4; (d)75% BiOBr/Bi2O3, pH=6; (e)75% BiOBr/Bi2O3, pH=8; (f)65% BiOBr/
Bi2O3, pH=6; (g)BiOBr。
Fig. 2 schemes for the SEM of catalyst：(a) pure Bi2O3;(b) pure BiOBr; (c)85% BiOBr /Bi2O3, pH
=6。
Fig. 3 is BiOBr and 75% pH=6 BiOBr/Bi2O3Infrared spectrogram.
Fig. 4 is the uv drses figure of catalyst.
Fig. 5 is the energy gap figure of catalyst.
Fig. 6 is for catalyst in visible ray in the degradation effect figure to methyl orange.
Fig. 7 is the observed rate constant figure of catalyst.
Fig. 8 is 75 % BiOBr/Bi2O3 PH=6 samples ultraviolet-visible absorption spectroscopy figure under different light application times.
Fig. 9 is the luminescence generated by light figure of catalyst.
Figure 10 is 75 % BiOBr/Bi2O3The loop test figure of pH=6 samples.
Specific embodiment
Embodiment 1
（1）Bismuth oxide（Bi2O3）Preparation：By 2.425 g Bi (NO3)3·5H2O and 0.6g NaOH are put into grind together
In alms bowl, mixed grinding, until the powder for yellow occur；Then this yellow powder is dissolved in into the beaker equipped with 30 ml distilled water
In, after 60 DEG C of h of stirring in water bath 5, to be washed 3-5 time respectively with distilled water and ethanol, 80 DEG C of dryings obtain the Bi of yellow2O3Powder
End.
（2） BiOBr/Bi2O3The preparation of complex：Take 0.8 g Bi2O3It is dissolved in 0.5 molL of 15.6 ml-1HBr
In, it is stirred vigorously, it is allowed to be completely dissolved；Afterwards, pH=8 is adjusted with diluted strong aqua ammonia, stirs 15 minutes afterwards, 40 DEG C
The h of stirring in water bath 0.5, after centrifugation, washing, being dried, by the pulverulent solids for obtaining；Crucible is put into, Muffle furnace is proceeded to
300 DEG C of 1 h of calcining, obtain BiOBr/Bi2O3Complex.The mass percent of BiOBr is 85%, Bi in complex2O3Quality
Percent is 15%（It is denoted as 85% BiOBr/Bi2O3）.It is 73% to the degradation rate of methyl orange.
Embodiment 2
（1）Bismuth oxide（Bi2O3）Preparation：With embodiment 1.
（2） BiOBr/Bi2O3The preparation of complex：Take 0.8 g Bi2O3It is dissolved in 0.5 molL of 13.6 ml-1HBr
In, it is stirred vigorously, it is allowed to be completely dissolved；Afterwards, pH=6 is adjusted with diluted strong aqua ammonia, stirs 15 minutes afterwards, 40 DEG C
The h of stirring in water bath 0.5, after centrifugation, washing, being dried, by the pulverulent solids for obtaining；Crucible is put into, Muffle furnace is proceeded to
300 DEG C of 1 h of calcining, obtain BiOBr/Bi2O3Complex.The mass percent of BiOBr is 75%, Bi in complex2O3Quality
Percent is 25%（It is denoted as 75% BiOBr/Bi2O3）.It is 93.8% to the degradation rate of methyl orange.
Embodiment 3
（1）Bismuth oxide（Bi2O3）Preparation：With embodiment 1.
（2） BiOBr/Bi2O3The preparation of complex：Take 0.8 g Bi2O3It is dissolved in 0.5 molL of 13.6 ml-1HBr
In, it is stirred vigorously, it is allowed to be completely dissolved；Afterwards, pH=4 is adjusted with diluted strong aqua ammonia, stirs 15 minutes afterwards, 40 DEG C
The h of stirring in water bath 0.5, after centrifugation, washing, being dried, by the pulverulent solids for obtaining；Crucible is put into, Muffle furnace is proceeded to
300 DEG C of 1 h of calcining, obtain BiOBr/Bi2O3Complex.The mass percent of BiOBr is 75%, Bi in complex2O3Quality
Percent is 25%（It is denoted as 75% BiOBr/Bi2O3）.It is 82% to the degradation rate of methyl orange.
Embodiment 4
（1）Bismuth oxide（Bi2O3）Preparation：With embodiment 1.
（2） BiOBr/Bi2O3The preparation of complex：Take 0.8 g Bi2O3It is dissolved in 0.5 molL of 13.6 ml-1HBr
In, it is stirred vigorously, it is allowed to be completely dissolved；Afterwards, pH=8 is adjusted with diluted strong aqua ammonia, stirs 15 minutes afterwards, 40 DEG C
The h of stirring in water bath 0.5, after centrifugation, washing, being dried, by the pulverulent solids for obtaining；Crucible is put into, Muffle furnace is proceeded to
300 DEG C of 1 h of calcining, obtain BiOBr/Bi2O3Complex.The mass percent of BiOBr is 75%, Bi in complex2O3Quality
Percent is 25%（It is denoted as 75% BiOBr/Bi2O3）.It is 86% to the degradation rate of methyl orange.
Embodiment 5
（1）Bismuth oxide（Bi2O3）Preparation：With embodiment 1.
（2） BiOBr/Bi2O3The preparation of complex：Take 0.8 g Bi2O3It is dissolved in 0.5 molL of 11.0 ml-1HBr
In, it is stirred vigorously, it is allowed to be completely dissolved；Afterwards, it is 6 to adjust pH with diluted strong aqua ammonia, stirs 15 minutes afterwards, 40 DEG C
The h of stirring in water bath 0.5, after centrifugation, washing, being dried, by the pulverulent solids for obtaining；Crucible is put into, Muffle furnace is proceeded to
300 DEG C of 1 h of calcining, obtain BiOBr/Bi2O3Complex.The mass percent of BiOBr is 65%, Bi in complex2O3Quality
Percent is 35%（It is denoted as 65% BiOBr/Bi2O3）, it is 70% to the degradation rate of methyl orange.
Claims (2)
1. a kind of BiOBr/Bi2O3The preparation method of hetero-junctions composite catalyst, is by Bi2O3In being completely dissolved in HBr solution,
HBr is made under stirring in Bi2O3Surface in situ hydrolysis BiOBr, forms the BiOBr/ that surface is stratiform 3D nanostructured
Bi2O3；Specifically preparation technology is：By Bi2O3In being dissolved in HBr solution, pH=4-8 is adjusted with ammonia, it is anti-in 40 ~ 50 DEG C of stirrings
0.5 ~ 1 h is answered, is centrifuged, washing after being dried, calcines 1 ~ 4 h at 200 ~ 400 DEG C, obtains final product BiOBr/Bi2O3Hetero-junctions is combined
Catalyst；Bi2O3It is 1 with the mol ratio of HBr:1.4~1:2.
2. BiOBr/Bi as claimed in claim 12O3The preparation method of hetero-junctions composite catalyst, it is characterised in that：Above-mentioned HBr
In solution, the concentration of HBr is 0.4 ~ 0.6 molL-1。
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| CN103316701B (en) * | 2013-07-02 | 2015-04-15 | 辽宁石油化工大学 | Method for preparing Bi2S3/BiOCl heterojunction photocatalyst |
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