CN107243317B - A kind of preparation method of porous bismuth ferrite photocatalysis regenerable sorbent - Google Patents
A kind of preparation method of porous bismuth ferrite photocatalysis regenerable sorbent Download PDFInfo
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- CN107243317B CN107243317B CN201710466619.5A CN201710466619A CN107243317B CN 107243317 B CN107243317 B CN 107243317B CN 201710466619 A CN201710466619 A CN 201710466619A CN 107243317 B CN107243317 B CN 107243317B
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Abstract
A kind of preparation method of porous bismuth ferrite photocatalysis regenerable sorbent, it is related to a kind of preparation method of regenerable sorbent.The invention aims to solve existing bismuth ferrite nano powder under visible light not having dyestuff stronger adsorption capacity, the problem of needing the pattern by complicated experimentation change bismuth ferrite nano powder, limiting the large-scale application of bismuth ferrite photocatalytic adsorbent.Method: one, bismuth ferrite precursor solution is prepared；Two, biscuit fragment is immersed in bismuth ferrite precursor solution, temperature is to 600 DEG C~800 DEG C again, 2h~4h is calcined at being again 600 DEG C~800 DEG C in temperature, obtain porous bismuth ferrite photocatalysis regenerable sorbent, the present invention is using the porous bismuth ferrite photocatalysis regenerable sorbent of Template synthesis, simple process, easy to operate.The present invention is suitable for preparing porous bismuth ferrite photocatalysis regenerable sorbent.
Description
Technical field
The present invention relates to a kind of preparation methods of regenerable sorbent.
Background technique
Waste water from dyestuff as common one of waste water in nowadays life, due to its coloration is deep, organic pollutant content is high,
The features such as complicated component, difficult for biological degradation, and with the organic matter of bio-toxicity containing there are many, it is serious to affect people
Life, destroy natural water environment.Photocatalysis technology in terms of have broad application prospects, be
Solve a kind of ideal green technology of energy and environmental problem.
Bismuth ferrite BiFeO3With good photocatalysis property, forbidden bandwidth is about 2.1eV, and its structure and physico
It learns property to stablize, there is better photocatalysis degradation organic contaminant performance, however the bismuth ferrate nano powder routinely prepared
Body does not have stronger adsorption capacity to dyestuff under visible light.Current main research direction is by complicated experimentation
Change the pattern of bismuth ferrate nano material, and then enhances its absorption and catalytic capability, but this significantly limits BiFeO3Light
The large-scale application of catalyst-sorbent, currently, bismuth ferrite catalyst material, most of light applied under laboratory simulation system
Catalyzing oxidizing degrading, is not possible to realize industrial dyestuff composite waste is effectively treated.Moreover, usually these prepare bismuth ferrite
Catalyst material can not effectively adsorb mixed dye sewage under complicated acid or alkali environment, drop its activity significantly
It is low.Therefore, it is necessary to take effective preparation strategy, prepares to have and be adsorbed by force under complex environment and the ferrous acid of Photocatalytic Regeneration ability
Bismuth material adsorb it can to waste water from dyestuff under conditions of complexity, and can be recycled for multiple times.
Traditional adsorbent is poor to the adsorption effect of dyestuff, and general adsorbance is between 10%~20%.
Summary of the invention
The invention aims to solve existing bismuth ferrite nano powder under visible light not having dyestuff stronger suction
Attached ability, it is impossible to be used in problem of the processing containing industrial dye waste water and traditional adsorbent adsorption effect difference, and one kind is provided
The preparation method of porous bismuth ferrite photocatalysis regenerable sorbent.
A kind of preparation method of porous bismuth ferrite photocatalysis regenerable sorbent, is specifically realized by the following steps:
One, it prepares bismuth ferrite precursor solution: molysite and bismuth salt is dissolved into dilute nitre that mass fraction is 20%~22%
In acid, yellow transparent solution is obtained, then low whipping speed is to be stirred to react 30min~40min under 150r/min~200r/min,
Obtain bismuth ferrite precursor solution；
The volume ratio for the dust technology that the quality and mass fraction of molysite described in step 1 are 20%~22% is (2.5g
~2.9g): (60mL~80mL)；
The volume ratio for the dust technology that the quality and mass fraction of bismuth salt described in step 1 are 20%~22% is (2.1g
~2.4g): (60mL~80mL)；
Two, biscuit fragment is immersed in 3min~6min in bismuth ferrite precursor solution, then the biscuit after immersion is taken out
Be put into Muffle furnace, then by Muffle furnace with 3 DEG C/min~5 DEG C/min heating rate from room temperature to 600 DEG C~800 DEG C,
2h~4h is calcined at being again 600 DEG C~800 DEG C in temperature, then by Muffle furnace cooled to room temperature, obtains porous bismuth ferrite light
Catalysis of renewable adsorbent completes a kind of preparation method of porous bismuth ferrite photocatalysis regenerable sorbent；
The quality of biscuit fragment described in step 2 and the volume ratio of bismuth ferrite precursor solution are (22g~25g):
(60mL~80mL).
The principle of the present invention and advantage:
One, porous bismuth ferrite photocatalysis regenerable sorbent prepared by the present invention is made it have porous by addition template
Structure can greatly enhance its adsorption capacity, and have good cyclical stability and Photocatalytic Regeneration ability, to a variety of dyestuffs
Composite waste can have good adsorption effect；
Two, the present invention is using the porous bismuth ferrite photocatalysis regenerable sorbent of Template synthesis, simple process, easy to operate；
Compared with conventional adsorbent, conventional adsorbent is to the adsorbance of dyestuff between 10%-20%, and by temperature, pH value etc. influences
It is larger, and many adsorbents can all generate by-product, cause secondary pollution to environment；The porous bismuth ferrite light that the present invention introduces
Catalysis of renewable adsorbent, simple process pollutes small, is influenced by temperature and pH value smaller, strong operability does not have simultaneously
Secondary pollution generates；
Three, porous bismuth ferrite photocatalysis regenerable sorbent prepared by the present invention has porous structure and biggish specific surface
Product, aperture concentrate on 20~220nm, and specific surface area is 69.5~72.5m2/g；
Four, invention significantly improves bismuth ferrites to the adsorption capacity and adsorption rate of a variety of dyestuff composite wastes, and
With good photocatalysis absorption regeneration ability and cyclical stability；The porous renewable suction of bismuth ferrite photocatalysis prepared by the present invention
The attached dose of combined sewage to five kinds of dyestuffs such as methylene blue, adsorption effect is followed up to 91.2%, and at five in 30 minutes
Adsorption effect is not substantially change in the ring period；
Five, porous bismuth ferrite photocatalysis regenerable sorbent prepared by the present invention can wrap the waste water from dyestuff of complex situations
The waste water for including mixed dye wastewater and different pH value is effectively adsorbed, and is inhaled to the combined sewage of five kinds of dyestuffs such as methylene blue
Attached effect in 150 minutes up to 90% or more, and for waste water that pH is 2,7,12 three different pH values at 150 minutes
Interior, adsorption effect is attained by 93% or more.
The present invention is suitable for preparing porous bismuth ferrite photocatalysis regenerable sorbent.
Detailed description of the invention
Fig. 1 is that the transmitted electron for 20000 times of porous bismuth ferrite photocatalysis regenerable sorbent amplification for testing a preparation is aobvious
Micro mirror photo；
Fig. 2 is the high-resolution transmission for testing 600000 times of the porous bismuth ferrite photocatalysis regenerable sorbent amplification of a preparation
Electron micrograph；
Fig. 3 is the N for testing the porous bismuth ferrite photocatalysis regenerable sorbent of a preparation2Adsorption/desorption isotherms；
Fig. 4 is the graph of pore diameter distribution for testing the porous bismuth ferrite photocatalysis regenerable sorbent of a preparation；
Fig. 5 is adsorption effect of the porous bismuth ferrite photocatalysis regenerable sorbent to mixed dye sewage for testing a preparation
Figure；
Fig. 6 is the cyclical stability histogram for testing the porous bismuth ferrite photocatalysis regenerable sorbent of a preparation, in Fig. 6
1 for for the first time circulation porous bismuth ferrite photocatalysis regenerable sorbent degrade mixed dye wastewater 150min when adsorption rate, 2
For second circulation porous bismuth ferrite photocatalysis regenerable sorbent degrade mixed dye wastewater 150min when adsorption rate, 3
For third time circulation porous bismuth ferrite photocatalysis regenerable sorbent degrade mixed dye wastewater 150min when adsorption rate, 4
For the 4th time recycle porous bismuth ferrite photocatalysis regenerable sorbent degrade mixed dye wastewater 150min when adsorption rate, 5
For the 5th time recycle porous bismuth ferrite photocatalysis regenerable sorbent degrade mixed dye wastewater 150min when adsorption rate；
Fig. 7 is absorption of the porous bismuth ferrite photocatalysis regenerable sorbent of one preparation of test to dye wastewater under different pH
Effect picture.
Specific embodiment
Specific embodiment 1: present embodiment is a kind of preparation side of porous bismuth ferrite photocatalysis regenerable sorbent
Method is specifically realized by the following steps:
One, it prepares bismuth ferrite precursor solution: molysite and bismuth salt is dissolved into dilute nitre that mass fraction is 20%~22%
In acid, yellow transparent solution is obtained, then low whipping speed is to be stirred to react 30min~40min under 150r/min~200r/min,
Obtain bismuth ferrite precursor solution；
The volume ratio for the dust technology that the quality and mass fraction of molysite described in step 1 are 20%~22% is (2.5g
~2.9g): (60mL~80mL)；
The volume ratio for the dust technology that the quality and mass fraction of bismuth salt described in step 1 are 20%~22% is (2.1g
~2.4g): (60mL~80mL)；
Two, biscuit fragment is immersed in 3min~6min in bismuth ferrite precursor solution, then the biscuit after immersion is taken out
Be put into Muffle furnace, then by Muffle furnace with 3 DEG C/min~5 DEG C/min heating rate from room temperature to 600 DEG C~800 DEG C,
2h~4h is calcined at being again 600 DEG C~800 DEG C in temperature, then by Muffle furnace cooled to room temperature, obtains porous bismuth ferrite light
Catalysis of renewable adsorbent completes a kind of preparation method of porous bismuth ferrite photocatalysis regenerable sorbent；
The quality of biscuit fragment described in step 2 and the volume ratio of bismuth ferrite precursor solution are (22g~25g):
(60mL~80mL).
The principle and advantage of present embodiment:
One, the porous bismuth ferrite photocatalysis regenerable sorbent of present embodiment preparation is made it have by addition template
Porous structure can greatly enhance its adsorption capacity, and have good cyclical stability and Photocatalytic Regeneration ability, to a variety of dyes
The composite waste of material can have good adsorption effect；
Two, present embodiment is using the porous bismuth ferrite photocatalysis regenerable sorbent of Template synthesis, simple process, easily behaviour
Make；Compared with conventional adsorbent, conventional adsorbent to the adsorbance of dyestuff between 10%-20%, and by temperature, the shadows such as pH value
Sound is larger, and many adsorbents can all generate by-product, cause secondary pollution to environment；The porous bismuth ferrite that the present invention introduces
Photocatalysis regenerable sorbent, simple process pollutes small, is influenced by temperature and pH value smaller, strong operability does not have simultaneously
There is secondary pollution generation；
Three, the porous bismuth ferrite photocatalysis regenerable sorbent of present embodiment preparation has porous structure and biggish ratio
Surface area, aperture concentrate on 20~220nm, and specific surface area is 69.5~72.5m2/g；
Four, present embodiment significantly improves bismuth ferrite to the adsorption capacity and adsorption rate of a variety of dyestuff composite wastes,
And there is good photocatalysis absorption regeneration ability and cyclical stability；Porous bismuth ferrite photocatalysis prepared by the present invention can be again
Raw adsorbent is to the combined sewages of five kinds of dyestuffs such as methylene blue, and adsorption effect is up to 91.2% in 30 minutes, and five
Adsorption effect is not substantially change in a cycle period；
Five, the porous bismuth ferrite photocatalysis regenerable sorbent of present embodiment preparation can be useless to the dyestuff of complex situations
Water, the waste water including mixed dye wastewater and different pH value are effectively adsorbed, the mixing to five kinds of dyestuffs such as methylene blue
Sewage adsorption effect in 150 minutes up to 90% or more, and for waste water that pH is 2,7,12 three different pH values 150
In minute, adsorption effect is attained by 93% or more.
Present embodiment is suitable for preparing porous bismuth ferrite photocatalysis regenerable sorbent.
Specific embodiment 2: the differences between this implementation mode and the specific implementation mode are that: molysite described in step 1
For Fe(NO3)39H2O, iron chloride, frerrous chloride or ferric sulfate.Other steps are same as the specific embodiment one.
Specific embodiment 3: one of present embodiment and specific embodiment one or two difference are: institute in step 1
The bismuth salt stated is five nitric hydrate bismuths or bismuth chloride.Other steps are the same as one or two specific embodiments.
Specific embodiment 4: one of present embodiment and specific embodiment one to three difference are: institute in step 2
The biscuit stated is common soda cracker.Other steps are identical as specific embodiment one to three.
Specific embodiment 5: one of present embodiment and specific embodiment one to four difference are: institute in step 1
The volume ratio for the dust technology that the quality and mass fraction for the molysite stated are 20%~22% is (2.5g~2.7g): (60mL~
70mL).Other steps are identical as specific embodiment one to four.
Specific embodiment 6: one of present embodiment and specific embodiment one to five difference are: institute in step 1
The volume ratio for the dust technology that the quality and mass fraction for the bismuth salt stated are 20%~22% is (2.1g~2.3g): (60mL~
70mL).Other steps are identical as specific embodiment one to five.
Specific embodiment 7: one of present embodiment and specific embodiment one to six difference are: will in step 2
Biscuit fragment is immersed in 3min~5min in bismuth ferrite precursor solution, then the biscuit taking-up after immersion is put into Muffle furnace,
Again by Muffle furnace with the heating rate of 5 DEG C/min from room temperature to 600 DEG C~700 DEG C, then temperature be 600 DEG C~700 DEG C
Lower calcining 2h~3h, then by Muffle furnace cooled to room temperature, obtain porous bismuth ferrite photocatalysis regenerable sorbent, that is, complete
A kind of preparation method of porous bismuth ferrite photocatalysis regenerable sorbent.Other steps are identical as specific embodiment one to six.
Specific embodiment 8: one of present embodiment and specific embodiment one to seven difference are: will in step 2
Biscuit fragment is immersed in 4min~5min in bismuth ferrite precursor solution, then the biscuit taking-up after immersion is put into Muffle furnace,
Again by Muffle furnace with the heating rate of 5 DEG C/min from room temperature to 600 DEG C~650 DEG C, then temperature be 600 DEG C~650 DEG C
Lower calcining 2h~2.5h, then by Muffle furnace cooled to room temperature, obtain porous bismuth ferrite photocatalysis regenerable sorbent, i.e., it is complete
At a kind of preparation method of porous bismuth ferrite photocatalysis regenerable sorbent.Other steps and one to seven phase of specific embodiment
Together.
Specific embodiment 9: one of present embodiment and specific embodiment one to eight difference are: single in step 2
The volume of a biscuit fragment is 60cm3~80cm3.Other steps are identical as specific embodiment one to eight.
Specific embodiment 10: one of present embodiment and specific embodiment one to nine difference are: institute in step 2
The quality for the biscuit fragment stated and the volume ratio of bismuth ferrite precursor solution are (22g~24g): (60mL~70mL).Other steps
Suddenly identical as specific embodiment one to nine.
The beneficial effect of the invention is verified by the following experiments:
Test one: a kind of preparation method of porous bismuth ferrite photocatalysis regenerable sorbent is specifically realized by the following steps
:
One, prepare bismuth ferrite precursor solution: it is 20% that 2.7g molysite and 2.3g bismuth salt, which are dissolved into 70mL mass fraction,
Dust technology in, obtain yellow transparent solution, then low whipping speed is to be stirred to react 30min under 180r/min, obtains bismuth ferrite
Precursor solution；
Molysite described in step 1 is Fe(NO3)39H2O；
Bismuth salt described in step 1 is five nitric hydrate bismuths；
Two, 24g biscuit fragment is immersed in 5min in bismuth ferrite precursor solution obtained in step 1, then will be after immersion
Biscuit taking-up be put into Muffle furnace, then by Muffle furnace with the heating rate of 5 DEG C/min from room temperature to 600 DEG C, then in temperature
Degree is to calcine 2h at 600 DEG C, then by Muffle furnace cooled to room temperature, obtain porous bismuth ferrite photocatalysis regenerable sorbent,
Complete a kind of preparation method of porous bismuth ferrite photocatalysis regenerable sorbent；
Biscuit described in step 2 is common soda cracker, and the volume of single biscuit fragment is 60cm3~80cm3。
Fig. 1 is that the transmitted electron for 20000 times of porous bismuth ferrite photocatalysis regenerable sorbent amplification for testing a preparation is aobvious
Micro mirror photo；
Fig. 2 is the high-resolution transmission for testing 600000 times of the porous bismuth ferrite photocatalysis regenerable sorbent amplification of a preparation
Electron micrograph；
As can be seen that the porous bismuth ferrite photocatalysis of one preparation of test can be again from the transmission electron microscope photo of Fig. 1
Raw adsorbent is nanoparticle structure, and there are many apparent cavernous structures for nano grain surface, it was demonstrated that test one is prepared porous
Bismuth ferrite photocatalysis regenerable sorbent is porous structure；
By the high resolution transmission electron microscopy photo of Fig. 2 this it appears that the shape in hole, and nanometer monocrystalline
Grain has high degree of crystallization, while having observed that interplanar distance is 0.232 nanometer, and the feature for being attributed to 111 crystal face of bismuth ferrite is spread out
Penetrate striped；
Fig. 3 is the N for testing the porous bismuth ferrite photocatalysis regenerable sorbent of a preparation2Adsorption/desorption isotherms；
Fig. 4 is the graph of pore diameter distribution for testing the porous bismuth ferrite photocatalysis regenerable sorbent of a preparation；
As can be seen that the aperture master of the porous bismuth ferrite photocatalysis regenerable sorbent of one preparation of test from Fig. 3 and Fig. 4
It wants integrated distribution between 20nm~220nm, belongs to porous structure, the specific surface area of adsorbent is larger, is 71.5m2/g。
Degradation property test one:
Porous bismuth ferrite photocatalysis regenerable sorbent prepared by test one is added in 100mL mixed dye wastewater,
Dark absorption 150min, the mixed dye for obtaining the porous bismuth ferrite photocatalysis regenerable sorbent after adsorbing containing first time are useless
Water；Every 30min takes out 5mL dyestuff and is centrifuged 10min during dark absorption 150min, and Aspirate supernatant is divided light with UV, visible light
Degree instrument surveys its absorbance, and the absorption of the porous bismuth ferrite photocatalysis regenerable sorbent of one preparation of test is calculated according to formula (1)
The histogram of rate, adsorption time and adsorption rate is as shown in Figure 5；Mixed dye wastewater described in degradation property test one is industry
It is formed with methylene blue, crystal violet, malachite green, basic yellow, alkaline bright blue and water, wherein the concentration of industrial methylene blue is
10mg/L, the concentration of crystal violet are 10mg/L, and the concentration of malachite green is 10mg/L, and the concentration of basic yellow is 10mg/L, alkalinity
The concentration of gorgeous indigo plant is 10mg/L；
Relationship between absorbance and adsorption rate are as follows:
(At=adsorption rate in formula (1)；A0For stoste absorbance；AxFor the absorbance of supernatant after sampling in every 30 minutes)
Fig. 5 is adsorption effect of the porous bismuth ferrite photocatalysis regenerable sorbent to mixed dye sewage for testing a preparation
Figure；
From figure 5 it can be seen that the porous bismuth ferrite photocatalysis regenerable sorbent of one preparation of test is to mixed dye dirt
The adsorption rate of water (being 91% to the adsorption effect of mixed dye sewage in 30min), and the fine (2.5h of adsorption effect quickly
96.5%) adsorption effect to mixed dye sewage is.Prove the porous renewable absorption of bismuth ferrite photocatalysis of one preparation of test
Agent has excellent adsorption effect to mixed dye sewage.
Photocatalytic Regeneration experiment one: using the xenon lamp of a 300W as light source, degradation property is tested one by simulated solar irradiation
The obtained mixed dye wastewater containing the porous bismuth ferrite photocatalysis regenerable sorbent after adsorbing for the first time is placed in distance
At the xenon lamp 20cm of 300W, Photocatalytic Regeneration experiment is carried out at room temperature, it is more after all being adsorbed for the first time after illumination 120min
Hole bismuth ferrite photocatalysis centrifugal drying obtains the porous bismuth ferrite photocatalysis regenerable sorbent recycled for the first time.
Degradation property test two: the porous bismuth ferrite photocatalysis for the first time circulation that Photocatalytic Regeneration experiment one is obtained can
Reproducing adsorbent is added in 100mL mixed dye wastewater, secretly adsorbs 150min, obtains the porous iron after adsorbing containing second
The mixed dye wastewater of sour bismuth photocatalysis regenerable sorbent, degradation effect is as shown in 1 in Fig. 6；Institute in degradation property test two
The mixed dye wastewater stated is industrial methylene blue, crystal violet, malachite green, basic yellow, alkaline bright blue and water form, wherein
The concentration of industrial methylene blue is 10mg/L, and the concentration of crystal violet is 10mg/L, and the concentration of malachite green is 10mg/L, alkalinity
Yellow concentration is 10mg/L, and the concentration of alkaline bright blue is 10mg/L；
Photocatalytic Regeneration experiment two: using the xenon lamp of a 300W as light source, degradation property is tested two by simulated solar irradiation
The obtained mixed dye wastewater containing the porous bismuth ferrite photocatalysis regenerable sorbent after second of absorption is placed in distance
Photocatalytic Regeneration experiment, illumination are carried out at room temperature at the xenon lamp 20cm of 300W? it is porous after adsorbing all second after min
Bismuth ferrite photocatalysis centrifugal drying obtains the porous bismuth ferrite photocatalysis regenerable sorbent of second of circulation.
Degradation property test three: the porous bismuth ferrite photocatalysis for second of circulation that Photocatalytic Regeneration experiment two is obtained can
Reproducing adsorbent is added in 100mL mixed dye wastewater, secretly adsorbs 150min, obtains the porous iron after adsorbing containing third time
The mixed dye wastewater of sour bismuth photocatalysis regenerable sorbent, degradation effect is as shown in 2 in Fig. 6；Institute in degradation property test three
The mixed dye wastewater stated is industrial methylene blue, crystal violet, malachite green, basic yellow, alkaline bright blue and water form, wherein
The concentration of industrial methylene blue is 10mg/L, and the concentration of crystal violet is 10mg/L, and the concentration of malachite green is 10mg/L, alkalinity
Yellow concentration is 10mg/L, and the concentration of alkaline bright blue is 10mg/L；
Photocatalytic Regeneration experiment three: using the xenon lamp of a 300W as light source, degradation property is tested three by simulated solar irradiation
The obtained mixed dye wastewater containing the porous bismuth ferrite photocatalysis regenerable sorbent after third time absorption is placed in distance
Photocatalytic Regeneration experiment, illumination are carried out at room temperature at the xenon lamp 20cm of 300W? it is porous after adsorbing all third times after min
Bismuth ferrite photocatalysis centrifugal drying obtains the porous bismuth ferrite photocatalysis regenerable sorbent that third time recycles；
Degradation property test four: the porous bismuth ferrite photocatalysis for the third time circulation that Photocatalytic Regeneration experiment three is obtained can
Reproducing adsorbent is added in 100mL mixed dye wastewater, secretly adsorbs 150min, is obtained containing the porous iron after the 4th absorption
The mixed dye wastewater of sour bismuth photocatalysis regenerable sorbent, degradation effect is as shown in 3 in Fig. 6；Institute in degradation property test four
The mixed dye wastewater stated is industrial methylene blue, crystal violet, malachite green, basic yellow, alkaline bright blue and water form, wherein
The concentration of industrial methylene blue is 10mg/L, and the concentration of crystal violet is 10mg/L, and the concentration of malachite green is 10mg/L, alkalinity
Yellow concentration is 10mg/L, and the concentration of alkaline bright blue is 10mg/L；
Photocatalytic Regeneration experiment four: using the xenon lamp of a 300W as light source, degradation property is tested four by simulated solar irradiation
The obtained mixed dye wastewater containing the porous bismuth ferrite photocatalysis regenerable sorbent after the 4th absorption is placed in distance
Photocatalytic Regeneration experiment, illumination are carried out at room temperature at the xenon lamp 20cm of 300W? it will be porous after all the 4th absorption after min
Bismuth ferrite photocatalysis centrifugal drying obtains the porous bismuth ferrite photocatalysis regenerable sorbent of the 4th circulation；
Degradation property test five: the porous bismuth ferrite photocatalysis for the 4th circulation that Photocatalytic Regeneration experiment four is obtained can
Reproducing adsorbent is added in 100mL mixed dye wastewater, secretly adsorbs 150min, is obtained containing the porous iron after the 5th absorption
The mixed dye wastewater of sour bismuth photocatalysis regenerable sorbent, degradation effect is as shown in 4 in Fig. 6；Institute in degradation property test five
The mixed dye wastewater stated is industrial methylene blue, crystal violet, malachite green, basic yellow, alkaline bright blue and water form, wherein
The concentration of industrial methylene blue is 10mg/L, and the concentration of crystal violet is 10mg/L, and the concentration of malachite green is 10mg/L, alkalinity
Yellow concentration is 10mg/L, and the concentration of alkaline bright blue is 10mg/L；
Photocatalytic Regeneration experiment five: using the xenon lamp of a 300W as light source, degradation property is tested five by simulated solar irradiation
The obtained mixed dye wastewater containing the porous bismuth ferrite photocatalysis regenerable sorbent after the 5th absorption is placed in distance
Photocatalytic Regeneration experiment, illumination are carried out at room temperature at the xenon lamp 20cm of 300W? it will be porous after all the 5th absorption after min
Bismuth ferrite photocatalysis centrifugal drying obtains the porous bismuth ferrite photocatalysis regenerable sorbent of the 5th circulation；
Degradation property test six: the porous bismuth ferrite photocatalysis for the 5th circulation that Photocatalytic Regeneration experiment five is obtained can
Reproducing adsorbent is added in 100mL mixed dye wastewater, secretly adsorbs 150min, is obtained containing the porous iron after the 6th absorption
The mixed dye wastewater of sour bismuth photocatalysis regenerable sorbent, degradation effect is as shown in 5 in Fig. 6；Institute in degradation property test six
The mixed dye wastewater stated is industrial methylene blue, crystal violet, malachite green, basic yellow, alkaline bright blue and water form, wherein
The concentration of industrial methylene blue is 10mg/L, and the concentration of crystal violet is 10mg/L, and the concentration of malachite green is 10mg/L, alkalinity
Yellow concentration is 10mg/L, and the concentration of alkaline bright blue is 10mg/L；
Fig. 6 is the cyclical stability histogram for testing the porous bismuth ferrite photocatalysis regenerable sorbent of a preparation, in Fig. 6
1 for for the first time circulation porous bismuth ferrite photocatalysis regenerable sorbent degrade mixed dye wastewater 150min when adsorption rate, 2
For second circulation porous bismuth ferrite photocatalysis regenerable sorbent degrade mixed dye wastewater 150min when adsorption rate, 3
For third time circulation porous bismuth ferrite photocatalysis regenerable sorbent degrade mixed dye wastewater 150min when adsorption rate, 4
For the 4th time recycle porous bismuth ferrite photocatalysis regenerable sorbent degrade mixed dye wastewater 150min when adsorption rate, 5
For the 5th time recycle porous bismuth ferrite photocatalysis regenerable sorbent degrade mixed dye wastewater 150min when adsorption rate；
As can be seen from Figure 6, it is steady to show excellent circulation for the porous bismuth ferrite photocatalysis regenerable sorbent of one preparation of test
Qualitative, degradation effect is not substantially change in five cycle periods.Prove that the porous bismuth ferrite photocatalysis of one preparation of test can be again
Raw adsorbent has stable circulation degradation effect, can be repeated several times regeneration.It is convenient and efficient, be conducive to actual production and answer
With.
Degradation property test seven: porous bismuth ferrite photocatalysis regenerable sorbent prepared by test one is added separately to pH
In the 100mL mixed dye wastewater that value is 2,5,7,9 and 12,150min is secretly adsorbed, degradation effect is as shown in Figure 7；Degradation property
Test seven described in mixed dye wastewater be industrial methylene blue, crystal violet, malachite green, basic yellow, alkaline bright blue and
Water composition, wherein the concentration of industrial methylene blue is 10mg/L, the concentration of crystal violet is 10mg/L, and the concentration of malachite green is
10mg/L, the concentration of basic yellow are 10mg/L, and the concentration of alkaline bright blue is 10mg/L；
Fig. 7 is absorption of the porous bismuth ferrite photocatalysis regenerable sorbent of one preparation of test to dye wastewater under different pH
Effect picture.
As can be seen from Figure 7, absorption of (pH=2,5,7,9, the 12) adsorbent to dye wastewater in the case where different pH values
Effect is attained by 93% or more, it was demonstrated that either in the acidic environment porous ferrous acid that still under alkaline environment prepared by test one
Bismuth photocatalysis regenerable sorbent can show excellent absorption property.
Claims (6)
1. a kind of preparation method of porous bismuth ferrite photocatalysis regenerable sorbent, it is characterised in that a kind of porous bismuth ferrite light is urged
What the preparation method of change regenerable sorbent was specifically realized by the following steps:
One, it prepares bismuth ferrite precursor solution: molysite and bismuth salt being dissolved into the dust technology that mass fraction is 20%~22%,
Yellow transparent solution is obtained, then low whipping speed is to be stirred to react 30min~40min under 150r/min~200r/min, is obtained
Bismuth ferrite precursor solution；
Molysite described in step 1 is Fe(NO3)39H2O, iron chloride, frerrous chloride or ferric sulfate；
Bismuth salt described in step 1 is five nitric hydrate bismuths or bismuth chloride；
The volume ratio for the dust technology that the quality of molysite described in step 1 and mass fraction are 20%~22% be (2.5g~
2.9g): (60mL~80mL)；
The volume ratio for the dust technology that the quality of bismuth salt described in step 1 and mass fraction are 20%~22% be (2.1g~
2.4g): (60mL~80mL)；
Two, biscuit fragment is immersed in 3min~6min in bismuth ferrite precursor solution, then the biscuit taking-up after immersion is put into
In Muffle furnace, then by Muffle furnace with 3 DEG C/min~5 DEG C/min heating rate from room temperature to 600 DEG C~800 DEG C, then
Temperature is 2h~4h to be calcined at 600 DEG C~800 DEG C, then by Muffle furnace cooled to room temperature, obtain porous bismuth ferrite photocatalysis
Regenerable sorbent completes a kind of preparation method of porous bismuth ferrite photocatalysis regenerable sorbent；
Biscuit described in step 2 is common soda cracker；
The volume of single biscuit fragment is 60cm in step 23~80cm3；
The quality of biscuit fragment described in step 2 and the volume ratio of bismuth ferrite precursor solution are (22g~25g): (60mL
~80mL).
2. a kind of preparation method of porous bismuth ferrite photocatalysis regenerable sorbent according to claim 1, feature exist
In molysite described in step 1 quality and mass fraction be 20%~22% dust technology volume ratio be (2.5g~
2.7g): (60mL~70mL).
3. a kind of preparation method of porous bismuth ferrite photocatalysis regenerable sorbent according to claim 1, feature exist
In bismuth salt described in step 1 quality and mass fraction be 20%~22% dust technology volume ratio be (2.1g~
2.3g): (60mL~70mL).
4. a kind of preparation method of porous bismuth ferrite photocatalysis regenerable sorbent according to claim 1, feature exist
Biscuit fragment is immersed in 3min~5min in bismuth ferrite precursor solution in step 2, then the biscuit taking-up after immersion is put
Enter in Muffle furnace, then by Muffle furnace with the heating rate of 5 DEG C/min from room temperature to 600 DEG C~700 DEG C, then in temperature be
2h~3h is calcined at 600 DEG C~700 DEG C, then by Muffle furnace cooled to room temperature, it is renewable to obtain porous bismuth ferrite photocatalysis
Adsorbent completes a kind of preparation method of porous bismuth ferrite photocatalysis regenerable sorbent.
5. a kind of preparation method of porous bismuth ferrite photocatalysis regenerable sorbent according to claim 1, feature exist
Biscuit fragment is immersed in 4min~5min in bismuth ferrite precursor solution in step 2, then the biscuit taking-up after immersion is put
Enter in Muffle furnace, then by Muffle furnace with the heating rate of 5 DEG C/min from room temperature to 600 DEG C~650 DEG C, then in temperature be
2h~2.5h is calcined at 600 DEG C~650 DEG C, then by Muffle furnace cooled to room temperature, obtaining porous bismuth ferrite photocatalysis can be again
Raw adsorbent, that is, complete a kind of preparation method of porous bismuth ferrite photocatalysis regenerable sorbent.
6. a kind of preparation method of porous bismuth ferrite photocatalysis regenerable sorbent according to claim 1, feature exist
The quality of biscuit fragment described in step 2 and the volume ratio of bismuth ferrite precursor solution are (22g~24g): (60mL~
70mL)。
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