CN104028264B - A kind of four-prism shape bismuth system oxysalt Bi 2wO 6preparation method - Google Patents

A kind of four-prism shape bismuth system oxysalt Bi 2wO 6preparation method Download PDF

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CN104028264B
CN104028264B CN201410258706.8A CN201410258706A CN104028264B CN 104028264 B CN104028264 B CN 104028264B CN 201410258706 A CN201410258706 A CN 201410258706A CN 104028264 B CN104028264 B CN 104028264B
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oxysalt
prism shape
bismuth system
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distilled water
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CN104028264A (en
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陈刚
李春梅
孙净雪
董红军
吕查德
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Harbin Institute of Technology
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Abstract

A kind of four-prism shape bismuth system oxysalt Bi 2wO 6preparation method, it relates to bismuth system oxysalt Bi 2wO 6preparation method.The present invention will solve the existing Bi prepared with molten-salt growth method 2wO 6the technical problem of degradation capability difference.Four-prism shape bismuth system oxysalt Bi 2wO 6, be the four-prism shape particle of the corner angle rounding assembled by nanometer sheet parallel orientation.Method for making: by Na 2wO 42H 2o solution is added dropwise to Bi (NO 3) 3emulsion in, stirring reaction, obtains mixed liquor, and centrifugation goes out solid formation, obtains presoma after drying; Presoma and fused salt are that after 1:3 ~ 7 mix, being placed on temperature is keep reaction 4 ~ 6h in the stove of 340 ~ 360 DEG C, obtains four-prism shape bismuth system oxysalt Bi in mass ratio 2wO 6, it can be used for photocatalysis field as photochemical catalyst.

Description

A kind of four-prism shape bismuth system oxysalt Bi 2wO 6preparation method
Technical field
The present invention relates to bismuth system oxysalt Bi 2wO 6preparation method.
Background technology
In today of 21 century, along with the develop rapidly of economy, incident environmental problem has become human society problem the severeest.Utilize the organic pollution in solar energy photocatalytic degradation of sewage to solve this problem more and more to get more and more people's extensive concerning.Traditional photochemical catalyst TiO 2because it has larger band gap magnitude, only under the irradiation of ultraviolet light, just can show photocatalysis characteristic, and ultraviolet light only accounts for 3% ~ 4% of sunshine, which limits TiO 2the practical application of this photochemical catalyst.Therefore, the efficient visible light responsible photocatalytic material of development of new, the pollutant effectively utilized in sunshine degradation of sewage is one of main path solving environmental pollution.
In recent years, a kind of novel have visible light catalytic material Bi that is visible light-responded and the good narrow band gap of visible light catalysis activity 2wO 6(energy gap is only about 2.8eV), causes researchers and pays close attention to widely.Bismuth tungstate is a kind of simple layer structure oxide, has WO 6and Bi 2o 2the perovskite-like lamellar structure of composition, mainly has following feature: good Uv and visible light response; Heat endurance; Advantage of lower cost; Environmental friendliness.Therefore, Bi is researched and developed 2wO 6catalysis material, will increase the utilization rate of solar energy, in the improvement of problem of environmental pollution and the Application and Development of new forms of energy, have great meaning.
The method preparing photochemical catalyst bismuth tungstate has a variety of; wherein molten-salt growth method due to its manufacture craft simple; required synthesis temperature is low; time is short; output is high; high and the salt of sample crystallinity can be recycled, and is considered to most probable realizes the method that industrial scale produces photochemical catalyst to advantages such as environment can not pollute.In recent years, Qianjiang China waited people to report the Bi prepared by molten-salt growth method 2wO 6ceramic powder, but obtained Bi 2wO 6for irregular sheet-like morphology, and its degradation property is poor, and the efficiency of Visible Light Induced Photocatalytic rhodamine B only can reach 40% in 2h.
Summary of the invention
The present invention will solve the existing Bi prepared with molten-salt growth method 2wO 6the technical problem of degradation capability difference, and provide a kind of four-prism shape bismuth system oxysalt Bi 2wO 6preparation method.
A kind of four-prism shape bismuth system oxysalt Bi of the present invention 2wO 6, be the four-prism shape particle of the corner angle rounding assembled by nanometer sheet parallel orientation.
Above-mentioned four-prism shape bismuth system oxysalt Bi 2wO 6preparation method, carry out according to the following steps:
One, by Bi (NO 3) 35H 2o and Na 2wO 42H 2the mol ratio of O is 2:1, takes Bi (NO 3) 35H 2o and Na 2wO 42H 2o;
Two, take distilled water as solvent, Bi (NO step one taken 3) 35H 2o joins in distilled water, uses ultrasonic vibration process, obtains Bi (NO 3) 3emulsion; By Na 2wO 42H 2o distilled water dissolves, and obtains Na 2wO 42H 2o solution;
Three, under constantly stirring, by the Na that step 2 is prepared 2wO 42H 2o solution is added dropwise to Bi (NO 3) 3emulsion in, after dropwising, stir 1 ~ 2 hour, obtain mixed liquor;
Four, centrifugation after mixed liquor distilled water washing step 3 obtained, then that solid formation is dry, obtain presoma;
Five, by KNO 3and NaNO 3mol ratio be that 1:1 is by KNO 3and NaNO 3be mixed, ground and mixed is even, obtains salt-mixture;
Six, be 1:3 ~ 7 by the mass ratio of presoma and salt-mixture, by presoma and salt-mixture ground and mixed even, obtain mixed-powder;
Seven, be placed in crucible by the mixed-powder that step 6 obtains, being placed on temperature is keep reaction 4 ~ 6h in the stove of 340 ~ 360 DEG C; After reaction terminates, the material absolute ethyl alcohol in crucible and/or distilled water cyclic washing, then put dry in an oven, obtain four-prism shape bismuth system oxysalt Bi 2wO 6.
The bismuth-containing oxygen hydrochlorate Bi that the present invention adopts molten-salt growth method to prepare 2wO 6photochemical catalyst, the method is a kind of cheap simple, can realize at short notice obtaining high-crystallinity, the uniform Bi of pattern 2wO 6.Sample productive rate is higher simultaneously, and up to 75%, the fused salt as reaction also can be recycled, and this is just for industrial-scale production improves theory support.This method appropriate design selects the allocation ratio of fused salt and the temperature conditions of molten salt react ion to prepare the Bi of four-prism shape 2wO 6it can as the catalyst of light-catalyzed reaction, have visible light-responded preferably, this catalyst shows the photocatalysis performance of higher degradating organic dye rhodamine B under visible light simultaneously, under the radiation of visible light of λ >400nm, degradable organic pollution rhodamine B only needs 40 minutes, and is degradation of dye instead of simply cycloreversion reaction completely.Bi of the present invention 2wO 6the Photocatalytic Degradation Property of catalyst significantly improves.Bi of the present invention 2wO 6photocatalysis field can be acted on.
Accompanying drawing explanation
Fig. 1 is the bismuth system oxysalt Bi that in test 1 prepared by molten-salt growth method 2wO 6the XRD spectra of photochemical catalyst;
Fig. 2 is the bismuth system oxysalt Bi that in test 1 prepared by molten-salt growth method 2wO 6the SEM spectrogram of photochemical catalyst;
Fig. 3 is the bismuth system oxysalt Bi that in test 1 prepared by molten-salt growth method 2wO 6the TEM spectrogram in four-prism front;
Fig. 4 is the bismuth system oxysalt Bi that in test 1 prepared by molten-salt growth method 2wO 6the TEM spectrogram of four-prism body side surface;
Fig. 5 is the bismuth system oxysalt Bi that in test 1 prepared by molten-salt growth method 2wO 6the degradable organic pollutant spectrogram of photochemical catalyst;
Fig. 6 is the bismuth system oxysalt Bi that in test 1 prepared by molten-salt growth method 2wO 6the ultraviolet-visible absorption spectra figure of the different degradation times of photochemical catalyst;
Fig. 7 is the bismuth system oxysalt Bi that in test 2 prepared by molten-salt growth method 2wO 6the SEM spectrogram of photochemical catalyst;
Fig. 8 is the bismuth system oxysalt Bi that in test 3 prepared by molten-salt growth method 2wO 6the SEM spectrogram of photochemical catalyst.
Detailed description of the invention
Detailed description of the invention one: a kind of four-prism shape bismuth system oxysalt Bi of present embodiment 2wO 6, be the four-prism shape particle of the corner angle rounding assembled by nanometer sheet parallel orientation.
The length of side of the four-prism bottom surface of the four-prism shape particle of present embodiment is 1 ~ 2 μm, and height is 0.8 ~ 1.2 μm; The thickness of nanometer sheet is 8 ~ 12nm.
Detailed description of the invention two: the four-prism shape bismuth system oxysalt Bi described in detailed description of the invention one 2wO 6preparation method, carry out according to the following steps:
One, by Bi (NO 3) 35H 2o and Na 2wO 42H 2the mol ratio of O is 2:1, takes Bi (NO 3) 35H 2o and Na 2wO 42H 2o;
Two, take distilled water as solvent, Bi (NO step one taken 3) 35H 2o joins in distilled water, uses ultrasonic vibration process, obtains Bi (NO 3) 3emulsion; By Na 2wO 42H 2o distilled water dissolves, and obtains Na 2wO 42H 2o solution;
Three, under constantly stirring, by the Na that step 2 is prepared 2wO 42H 2o solution is added dropwise to Bi (NO 3) 3emulsion in, after dropwising, stir 1 ~ 2 hour, obtain mixed liquor;
Four, centrifugation after mixed liquor distilled water washing step 3 obtained, then that solid formation is dry, obtain presoma;
Five, by KNO 3and NaNO 3mol ratio be that 1:1 is by KNO 3and NaNO 3be mixed, ground and mixed is even, obtains salt-mixture;
Six, be 1:3 ~ 7 by the mass ratio of presoma and salt-mixture, by presoma and salt-mixture ground and mixed even, obtain mixed-powder;
Seven, be placed in crucible by the mixed-powder that step 6 obtains, being placed on temperature is keep reaction 4 ~ 6h in the stove of 300 DEG C ~ 400 DEG C; After reaction terminates, the material absolute ethyl alcohol in crucible and/or distilled water cyclic washing, then put dry in an oven, obtain four-prism shape bismuth system oxysalt Bi 2wO 6.
Detailed description of the invention three: present embodiment and detailed description of the invention two are unlike Bi (NO in step 2 3) 35H 2the amount of substance of O and the ratio of distilled water volume are 1mol:(5 ~ 10) mL.Other is identical with detailed description of the invention one.
Detailed description of the invention four: present embodiment and detailed description of the invention two or three are unlike Na in step 2 2wO 42H 2the amount of substance of O and the ratio of distilled water volume are 1mol:(10 ~ 15) mL.Other is identical with detailed description of the invention one or two.
Detailed description of the invention five: one of present embodiment and detailed description of the invention two to four are at 80 ~ 100 DEG C unlike temperature dry in step 4.Other is identical with one of detailed description of the invention two to four.
Detailed description of the invention six: one of present embodiment and detailed description of the invention two to five are 1:5 unlike the mass ratio of presoma in step 6 and salt-mixture.Other is identical with one of detailed description of the invention two to five.
In this molten-salt growth method preparation process, the ratio of presoma and salt-mixture is very crucial parameter, and the pattern of ratio on product of presoma and salt-mixture has larger impact.
Detailed description of the invention seven: one of present embodiment and detailed description of the invention two to six are 350 DEG C unlike the reaction temperature in step 7.Other is identical with one of detailed description of the invention two to six.
In this molten-salt growth method preparation process, the selection of reaction temperature is also a key.
With following verification experimental verification beneficial effect of the present invention:
Test 1: the four-prism shape bismuth system oxysalt Bi of this test 2wO 6preparation method, carry out according to the following steps:
One, Bi (NO is taken 3) 3.5H 2o (1mmol, 0.485g), Na 2wO 4.2H 2o (0.5mmol, 0.169g); KNO 3(0.1mol, 10.1g) and NaNO 3(0.1mol, 8.5g);
Two, take distilled water as solvent, Bi (NO step one taken 3) 3.5H 2o adds 7mL distilled water, ultrasonic vibration process 30 minutes, obtains white Bi (NO 3) 3emulsion; By Na 2wO 4.2H 2o (0.5mmol) adds in 6mL water and dissolves, and obtains Na 2wO 4.2H 2o solution;
Three, under constantly stirring, by the Na that step 2 is prepared 2wO 4.2H 2o solution is slowly added dropwise to Bi (NO 3) 3emulsion in, after dropwising, stir 1 hour, obtain mixture;
Four, centrifugation after mixture distilled water cyclic washing step 3 obtained, dry in 80 DEG C of baking ovens afterwards, obtain presoma;
Five, 10.1gKNO is taken 3(0.1mol) and 8.5gNaNO 3(0.1mol); KNO 3and NaNO 3together, ground and mixed 30 minutes, makes it mix, obtains KNO solids mixing 3and NaNO 3salt-mixture;
Six, the salt-mixture ground and mixed that presoma 1g step 4 obtained and 5g step 5 obtain 30 minutes, obtains mixture;
Seven, be placed in crucible by the mixture that step 6 obtains, being placed on temperature is keep reaction 4h in the Muffle furnace of 350 DEG C; After reaction terminates, the material in crucible first uses absolute ethanol washing 3 times, then washs 3 times with distilled water, to be finally placed in 80 DEG C of baking ovens dry 12 hours, to obtain four-prism shape bismuth system oxysalt Bi 2wO 6.
The four-prism shape bismuth system oxysalt Bi that this test obtains 2wO 6xRD spectra as shown in Figure 1, wherein a be this test preparation Bi 2wO 6xRD spectra, b is 73-1126 Bi in PDF card 2wO 6standard spectrogram, contrast known, this test preparation bismuth system oxysalt Bi 2wO 6really be Bi 2wO 6, and well-crystallized.
Fig. 2 is the bismuth system oxysalt Bi that this test obtains 2wO 6stereoscan photograph, as can be seen from Figure 2, this test preparation Bi 2wO 6shape be the four-prism of corner angle rounding, the length of side of its bottom surface is 2 μm, and height is 1 μm.
Fig. 3 is the bismuth system oxysalt Bi that this test obtains 2wO 6the transmission electron microscope photo in four-prism front, as can be seen from Figure 3, the four-prism of this corner angle rounding is assembled by uniform ultrathin nanometer sheet orientation and is formed;
Fig. 4 is the bismuth system oxysalt Bi that this test obtains 2wO 6the transmission electron microscope photo of four-prism body side surface; The thickness of nanometer sheet is about 10nm as can be seen from Figure 4.
By Bi prepared by this test 2wO 6carry out Degrading experiment, process of the test is as follows: by 0.05gBi 2wO 6sample joins in the rhodamine B solution of 100ml, and under dark room conditions, even magnetic agitation stirs 1h to reach adsorption equilibrium, and now rhodamine B concentration is C 0the degrading activity of detecting catalyst under radiation of visible light more afterwards, light source is 300W xenon lamp, optical filter is used to filter ultraviolet light (λ >400nm), along with the carrying out of reaction, from reactant liquor, got 3ml liquid at interval of 10 minutes, obtain settled solution through centrifugation (10000 revs/min), concentration is C.1-C/C 0embody the degradation rate of rhodamine B under this time.Meanwhile, to taking-up solution testing ultraviolet-visible absorption spectroscopy, paint and prepare C/C 0curve over time.Wherein the ultraviolet-visible absorption spectra figure of different degradation time is as shown in Figure 5, in figure, and the ultraviolet-visible absorption spectra figure that a is degradation time when being 0 minute; The ultraviolet-visible absorption spectra figure that b is degradation time when being 10 minutes; The ultraviolet-visible absorption spectra figure that c is degradation time when being 20 minutes; The ultraviolet-visible absorption spectra figure that d is degradation time when being 30 minutes; The ultraviolet-visible absorption spectra figure that e is degradation time when being 40 minutes.As can be seen from Figure 5, along with the increase of degradation time, absorption intensity reduces, and illustrates that rhdamine B is constantly degraded until degrade completely.It can also be seen that from ultraviolet-visible absorption spectroscopy figure, rhodamine B is degraded completely, instead of simple cycloreversion reaction.
C/C 0curve as shown in Figure 6 over time, and in Fig. 6, a is with the Bi of this test preparation 2wO 6c/C 0curve over time, b carries out degraded check experiment with P25 powder, the C/C obtained 0curve over time.As can be seen from Figure 6, the Bi of preparation 2wO 6its degrading activity of sample, far above P25, confirms four-prism Bi further 2wO 6sample has higher photocatalytic activity, can be used as a kind of desirable catalysis material.
Test 2: this test with test 1 unlike in step 6, by the Bi that 1g step 4 is obtained 2wO 6the salt-mixture ground and mixed that the presoma of photochemical catalyst and 7g step 5 obtain 30 minutes, obtains mixture; Other step and parameter are all identical with test 1.
The bismuth system oxysalt Bi that this test obtains 2wO 6stereoscan photograph as shown in Figure 7, as can be seen from Figure 7, this test preparation Bi 2wO 6, its shape has the four-prism of corner angle rounding, and the length of side of its bottom surface is 2 μm, and height is 1 μm, also has the particle of irregular pattern.The Bi of preparation 2wO 6sample can make rhodamine B degradable in 70 minutes.
Test 3: this test with test 1 unlike in step 6, by the Bi that 1g step 4 is obtained 2wO 6the salt-mixture ground and mixed that the presoma of photochemical catalyst and 3g step 5 obtain 30 minutes, obtains mixture; Other step and parameter are all identical with test 1.
The bismuth system oxysalt Bi that this test obtains 2wO 6stereoscan photograph as shown in Figure 8, as can be seen from Figure 8, this test preparation Bi 2wO 6, its shape has the four-prism of corner angle rounding, and the length of side of its bottom surface is 2 μm, and height is 1 μm, also has the particle of irregular pattern.The Bi2WO6 sample of preparation can make rhodamine B degradable in 80 minutes.
Test 1,2 and 3, the presoma of employing is different from the ratio of salt-mixture, when wherein the ratio of presoma and salt-mixture is 1:5, the Bi obtained 2wO 6pattern be the four-prism shape of the corner angle rounding of well-crystallized, and test the Bi obtained in 2 and 3 2wO 6have the particle of other shapes, crystallization is not fine, and compared with well-crystallized, degradation effect is slightly poor.

Claims (6)

1. a four-prism shape bismuth system oxysalt Bi 2wO 6preparation method, it is characterized in that the method is carried out according to the following steps:
One, by Bi (NO 3) 35H 2o and Na 2wO 42H 2the mol ratio of O is 2:1, takes Bi (NO 3) 35H 2o and Na 2wO 42H 2o;
Two, take distilled water as solvent, Bi (NO step one taken 3) 35H 2o joins in distilled water, uses ultrasonic vibration process, obtains Bi (NO 3) 3emulsion; By Na 2wO 42H 2o distilled water dissolves, and obtains Na 2wO 42H 2o solution;
Three, under constantly stirring, by the Na that step 2 is prepared 2wO 42H 2o solution is added dropwise to Bi (NO 3) 3emulsion in, after dropwising, stir 1 ~ 2 hour, obtain mixed liquor;
Four, centrifugation after mixed liquor distilled water washing step 3 obtained, then that solid formation is dry, obtain presoma;
Five, by KNO 3and NaNO 3mol ratio be that 1:1 is by KNO 3and NaNO 3be mixed, ground and mixed is even, obtains salt-mixture;
Six, be 1:3 ~ 7 by the mass ratio of presoma and salt-mixture, by presoma and salt-mixture ground and mixed even, obtain mixed-powder;
Seven, be placed in crucible by the mixed-powder that step 6 obtains, being placed on temperature is keep reaction 4 ~ 6h in the stove of 340 ~ 360 DEG C; After reaction terminates, the material absolute ethyl alcohol in crucible and/or distilled water cyclic washing, then put dry in an oven, obtain four-prism shape bismuth system oxysalt Bi 2wO 6, this Bi 2wO 6it is the four-prism shape particle of the corner angle rounding assembled by nanometer sheet parallel orientation.
2. a kind of four-prism shape bismuth system oxysalt Bi according to claim 1 2wO 6preparation method, it is characterized in that Bi (NO in step 2 3) 35H 2the amount of substance of O and the ratio of distilled water volume are 1mol:(5 ~ 10) mL.
3. a kind of four-prism shape bismuth system oxysalt Bi according to claim 1 and 2 2wO 6preparation method, it is characterized in that Na in step 2 2wO 42H 2the amount of substance of O and the ratio of distilled water volume are 1mol:(10 ~ 15) mL.
4. a kind of four-prism shape bismuth system oxysalt Bi according to claim 1 and 2 2wO 6preparation method, to it is characterized in that in step 4 that dry temperature is at 80 ~ 100 DEG C.
5. a kind of four-prism shape bismuth system oxysalt Bi according to claim 1 and 2 2wO 6preparation method, it is characterized in that the mass ratio of presoma and salt-mixture in step 6 is 1:5.
6. a kind of four-prism shape bismuth system oxysalt Bi according to claim 1 and 2 2wO 6preparation method, it is characterized in that the reaction temperature in step 7 is 350 DEG C.
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