CN103464138B - Ytterbium doped bismuth vanadate visible light photocatalyst, and preparation method and application thereof - Google Patents
Ytterbium doped bismuth vanadate visible light photocatalyst, and preparation method and application thereof Download PDFInfo
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Abstract
Provided are an ytterbium doped bismuth vanadate visible light photocatalyst, and a preparation method and an application thereof. The main ingredient of the photocatalyst is BiVO4 which has a tetragonal zircon-type structure, and a lattice of BiVO4 contains Yb<3+>. The preparation method comprises the steps: respectively dissolving bismuth nitrate pentahydrate and ammonium metavanadate in water to prepare a bismuth salt solution and a vanadium salt solution, adding the vanadium salt solution into the bismuth salt solution according to a molar ratio of Bi to V of 1:1 to obtain a mixed solution, adjusting the pH value of the mixed solution to 8, then adding ytterbium nitrate hexahydrate into the mixed solution according to a molar ratio of Yb to Bi of (4-10):100, carrying out a microwave hydrothermal method with the power of 300 W and carrying out heat preservation at the temperature of 180 DEG C for 40 min to prepare the ytterbium doped bismuth vanadate visible light photocatalyst. The microwave hydrothermal synthesis technology is employed for rapid synthesis of the ytterbium doped bismuth vanadate visible light photocatalyst; the photocatalyst has good photocatalytic activity, can be used for degradation of organic compounds; and the preparation method has the advantages of simple process, convenient operation and short preparation period.
Description
Technical field
The invention belongs to material science, be specifically related to a kind of ytterbium doping pucherite visible-light photocatalyst and its preparation method and application.
Background technology
BiVO
4be a kind of to visible light-responded semiconductor light-catalyst, mainly contain these three kinds of crystal formations of monocline scheelite type structure, cubic scheelite type structure and cubic Zircon cut structure.Photocatalysis performance and its crystal structure of large quantity research proof pucherite are closely related.Because of monoclinic phase BiVO
4energy gap less (2.40eV), can absorb more visible ray and show higher photocatalysis efficiency, and this becomes one of focus of people's research, and Tetragonal BiVO
4photocatalysis efficiency is very low and be left in the basket under visible light.But the monocline scheelite type structure BiVO of pure phase
4light induced electron and the separative efficiency in hole lower, cause its photocatalysis effect unsatisfactory, therefore, people adopt the means such as ion doping, Metal Supported, semiconductor coupling to carry out modification to it in recent years, improve monoclinic phase BiVO to a certain extent
4photocatalysis performance.The people such as the Zhang Aiping monoclinic phase Ln-BiVO that adopted hydro-thermal method to obtain
4, Ln=Eu, Gd, Er, its photocatalysis efficiency improves greatly, and [Zhang Aiping, Zhang Jinzhi, Ln adulterate BiVO
4the preparation of (Ln=Eu, Gd, Er) photochemical catalyst and activity research, Chinese Journal of Inorganic Chemistry, 25 (2009) 2040-2047].
Summary of the invention
The object of the present invention is to provide a kind of ytterbium doping pucherite visible-light photocatalyst and its preparation method and application, the method reaction time is short, and technological process is simple, and obtained ytterbium doping pucherite visible-light photocatalyst has good visible light photocatalysis active.
For achieving the above object, the technical solution used in the present invention is:
A kind of ytterbium doping pucherite visible-light photocatalyst, its main component is BiVO
4, be cubic Zircon cut structure, and BiVO
4lattice in containing Yb
3+, wherein the mol ratio of Yb element and Bi element is (4 ~ 10): 100.
A preparation method for ytterbium doping pucherite visible-light photocatalyst, comprises the following steps:
Step 1: by Bi (NO
3)
35H
2o is soluble in water, stirs, and obtains bismuth salting liquid; By NH
4vO
3be dissolved in the water of 90 ~ 100 DEG C, heating stirs, and obtains vanadic salts solution; Be that vanadic salts solution joins in bismuth salting liquid by 1:1 according to the mol ratio of Bi and V, stir, obtain mixed liquor;
Step 2: the pH value regulating mixed liquor is 8, stirs;
Step 3: by Yb (NO
3)
36H
2in mixed liquor after O joins and have adjusted pH value, stir, obtain precursor liquid, wherein the mol ratio of Yb and Bi is (4 ~ 10): 100;
Step 4: precursor liquid is put into microwave hydrothermal reaction kettle, then put into microwave hydrothermal reaction after microwave hydrothermal reaction kettle being sealed, setting microwave power is 300W, from room temperature to 100 DEG C, at 100 DEG C of insulation 6min; Then 150 DEG C are warming up to from 100 DEG C, at 150 DEG C of insulation 6min; Be warming up to 180 DEG C from 150 DEG C again, after 180 DEG C of insulation 35min, terminate reaction, then naturally cool to room temperature;
Step 5: taken out by the sediment reacting generation through step 4, washing, drying, obtain ytterbium doping pucherite visible-light photocatalyst.
Bi (NO in described bismuth salting liquid
3)
35H
2the concentration of O is 0.4mol/L; NH in vanadic salts solution
4vO
3concentration be 0.4mol/L.
By Bi (NO in described step 1
3)
35H
2the O required time that stirs soluble in water is 30min; By NH
4vO
3being dissolved in the water of 90 ~ 100 DEG C heating required time that stirs is 15min; Vanadic salts solution being added drop-wise in bismuth salting liquid the required time that stirs is 30min.
Regulate the pH value of mixed liquor by the NaOH solution that concentration is 5mol/L in described step 2.
Required time that stirs in described step 2 is 30min; Required time that stirs in described step 3 is 30min.
In described step 4, the packing ratio of reactor is 50% ~ 60%.
Washing in described step 5 is after spending deionized water to neutrality, then uses absolute ethanol washing.
Drying in described step 5 is dry 10 ~ 12h at 60 ~ 70 DEG C.
Ytterbium doping pucherite visible-light photocatalyst is used for the application of degradation of organic substances.
Compared with prior art, the present invention has following beneficial effect:
The preparation method of ytterbium doping pucherite visible-light photocatalyst provided by the invention, with five water bismuth nitrate (Bi (NO
3)
35H
2o) be bismuth source, ammonium metavanadate (NH
4vO
3) be vanadium source, preparation BiVO
4, then with six water ytterbium nitrate (Yb (NO
3)
36H
2o) be ytterbium source, to BiVO
4carry out Yb
3+doping.The present invention is by Yb
3+introduce BiVO
4lattice in, improve pure BiVO
4the efficiency of photocatalysis to degrade organic matter under visible light.The present invention adopts microwave-hydrothermal method one-step synthesis ytterbium doping pucherite visible-light photocatalyst, combine the advantage of heating using microwave and hydro-thermal method, its reaction condition is gentle, reaction time is short, technological process is simple, and production efficiency is high, easy to operate, manufacturing cycle is short, the crystal phase structure of target crystal and morphology controllable.
Ytterbium doping pucherite visible-light photocatalyst provided by the invention is cubic Zircon cut structure, and its main component is BiVO
4, and BiVO
4lattice in containing Yb
3+, the Tetragonal BiVO reported with previous literature
4result without photocatalytic activity is significantly different, and ytterbium doping pucherite visible-light photocatalyst prepared by the present invention has good visible light photocatalysis active, the monoclinic phase BiVO that do not adulterate that the photocatalytic activity under its visible ray is obtained under the same terms
4photocatalytic activity, can be used in degradation of organic substances, have a good application prospect.
Accompanying drawing explanation
Fig. 1 is the different Yb of the present invention
3+the XRD spectra of the ytterbium doping pucherite visible-light photocatalyst prepared under doping, wherein a is unadulterated BiVO
4xRD collection of illustrative plates, b ~ e is respectively the XRD collection of illustrative plates of ytterbium doping pucherite visible-light photocatalyst prepared by embodiment 1 ~ embodiment 4.
Fig. 2 is the different Yb of the present invention
3+the ytterbium doping pucherite visible-light photocatalyst prepared under doping is under visible light to the degradation rate curve of rhodamine B, and wherein a is unadulterated monoclinic phase BiVO
4catalyst is to the degradation rate curve of rhodamine B, and b ~ e is respectively the ytterbium doping pucherite visible-light photocatalyst of embodiment 1 ~ embodiment 4 preparation to the degradation curve of rhodamine B, and RhB is the degradation rate curve of rhodamine B when not adding photochemical catalyst under visible ray.
Detailed description of the invention
Below in conjunction with specific embodiments and the drawings, the present invention is described in further detail.
Embodiment 1:
A kind of ytterbium doping pucherite visible-light photocatalyst, its main component is BiVO
4, be cubic Zircon cut structure, and BiVO
4lattice in containing Yb
3+, wherein the mol ratio of Yb element and Bi element is 4:100.
A preparation method for ytterbium doping pucherite visible-light photocatalyst, comprises the following steps:
Step 1: by 0.01mol Bi (NO
3)
35H
2o is dissolved in 25mL deionized water, stirs 30min, obtains Bi (NO
3)
35H
2o concentration is the bismuth salting liquid of 0.4mol/L; By 0.01mol NH
4vO
3be dissolved in the deionized water of 25mL90 DEG C, add thermal agitation 15min, obtain NH
4vO
3concentration is the vanadic salts solution of 0.4mol/L; Be that vanadic salts dropwise joins in bismuth salting liquid by 1:1 according to the mol ratio of Bi and V, stir 30min, obtain mixed liquor;
Step 2: regulate the pH value of mixed liquor to be 8 by the NaOH solution that concentration is 5mol/L, stir 30min;
Step 3: by six water ytterbium nitrate (Yb (NO
3)
36H
2o) be that 4:100 joins in the mixed liquor after have adjusted pH value according to the mol ratio of Yb and Bi, stir 30min, obtain precursor liquid;
Step 4: microwave hydrothermal reaction kettle precursor liquid being put into polytetrafluoroethylene (PTFE) material, the packing ratio of microwave hydrothermal reaction kettle is 55%, microwave hydrothermal reaction is put into after microwave hydrothermal reaction kettle being sealed, select micro-wave digestion (temperature control) scheme, setting microwave power is 300W, from room temperature to 100 DEG C, at 100 DEG C of insulation 6min; Then 150 DEG C are warming up to from 100 DEG C, at 150 DEG C of insulation 6min; Be warming up to 180 DEG C from 150 DEG C again, after 180 DEG C of insulation 35min, terminate reaction, then naturally cool to room temperature;
Step 5: the sediment that will react generation through step 4 takes out, and after spending deionized water to neutrality, then uses absolute ethanol washing 3 times, then at 70 DEG C dry 10h, obtain ytterbium doping pucherite visible-light photocatalyst.
Embodiment 2:
A kind of ytterbium doping pucherite visible-light photocatalyst, its main component is BiVO
4, be cubic Zircon cut structure, and BiVO
4lattice in containing Yb
3+, wherein the mol ratio of Yb element and Bi element is 6:100.
A preparation method for ytterbium doping pucherite visible-light photocatalyst, comprises the following steps:
Step 1: by 0.01mol Bi (NO
3)
35H
2o is dissolved in 25mL deionized water, stirs 30min, obtains Bi (NO
3)
35H
2o concentration is the bismuth salting liquid of 0.4mol/L; By 0.01mol NH
4vO
3be dissolved in the deionized water of 25mL95 DEG C, add thermal agitation 15min, obtain NH
4vO
3concentration is the vanadic salts solution of 0.4mol/L; Be that vanadic salts dropwise joins in bismuth salting liquid by 1:1 according to the mol ratio of Bi and V, stir 30min, obtain mixed liquor;
Step 2: regulate the pH value of mixed liquor to be 8 by the NaOH solution that concentration is 5mol/L, stir 30min;
Step 3: by six water ytterbium nitrate (Yb (NO
3)
36H
2o) be that 6:100 joins in the mixed liquor after have adjusted pH value according to the mol ratio of Yb and Bi, stir 30min, obtain precursor liquid;
Step 4: microwave hydrothermal reaction kettle precursor liquid being put into polytetrafluoroethylene (PTFE) material, the packing ratio of microwave hydrothermal reaction kettle is 50%, microwave hydrothermal reaction is put into after microwave hydrothermal reaction kettle being sealed, select micro-wave digestion (temperature control) scheme, setting microwave power is 300W, from room temperature to 100 DEG C, at 100 DEG C of insulation 6min; Then 150 DEG C are warming up to from 100 DEG C, at 150 DEG C of insulation 6min; Be warming up to 180 DEG C from 150 DEG C again, after 180 DEG C of insulation 35min, terminate reaction, then naturally cool to room temperature;
Step 5: the sediment that will react generation through step 4 takes out, and after spending deionized water to neutrality, then uses absolute ethanol washing 3 times, then at 65 DEG C dry 12h, obtain ytterbium doping pucherite visible-light photocatalyst.
Embodiment 3:
A kind of ytterbium doping pucherite visible-light photocatalyst, its main component is BiVO
4, be cubic Zircon cut structure, and BiVO
4lattice in containing Yb
3+, wherein the mol ratio of Yb element and Bi element is 8:100.
A preparation method for ytterbium doping pucherite visible-light photocatalyst, comprises the following steps:
Step 1: by 0.01mol Bi (NO
3)
35H
2o is dissolved in 25mL deionized water, stirs 30min, obtains Bi (NO
3)
35H
2o concentration is the bismuth salting liquid of 0.4mol/L; By 0.01mol NH
4vO
3be dissolved in the deionized water of 25mL95 DEG C, add thermal agitation 15min, obtain NH
4vO
3concentration is the vanadic salts solution of 0.4mol/L; Be that vanadic salts dropwise joins in bismuth salting liquid by 1:1 according to the mol ratio of Bi and V, stir 30min, obtain mixed liquor;
Step 2: regulate the pH value of mixed liquor to be 8 by the NaOH solution that concentration is 5mol/L, stir 30min;
Step 3: by six water ytterbium nitrate (Yb (NO
3)
36H
2o) be that 8:100 joins in the mixed liquor after have adjusted pH value according to the mol ratio of Yb and Bi, stir 30min, obtain precursor liquid;
Step 4: microwave hydrothermal reaction kettle precursor liquid being put into polytetrafluoroethylene (PTFE) material, the packing ratio of microwave hydrothermal reaction kettle is 60%, microwave hydrothermal reaction is put into after microwave hydrothermal reaction kettle being sealed, select micro-wave digestion (temperature control) scheme, setting microwave power is 300W, from room temperature to 100 DEG C, at 100 DEG C of insulation 6min; Then 150 DEG C are warming up to from 100 DEG C, at 150 DEG C of insulation 6min; Be warming up to 180 DEG C from 150 DEG C again, after 180 DEG C of insulation 35min, terminate reaction, then naturally cool to room temperature;
Step 5: the sediment that will react generation through step 4 takes out, and after spending deionized water to neutrality, then uses absolute ethanol washing 3 times, then at 60 DEG C dry 11h, obtain ytterbium doping pucherite visible-light photocatalyst.
Embodiment 4:
A kind of ytterbium doping pucherite visible-light photocatalyst, its main component is BiVO
4, be cubic Zircon cut structure, and BiVO
4lattice in containing Yb
3+, wherein the mol ratio of Yb element and Bi element is 10:100.
A preparation method for ytterbium doping pucherite visible-light photocatalyst, comprises the following steps:
Step 1: by 0.01mol Bi (NO
3)
35H
2o is dissolved in 25mL deionized water, stirs 30min, obtains Bi (NO
3)
35H
2o concentration is the bismuth salting liquid of 0.4mol/L; By 0.01mol NH
4vO
3be dissolved in the deionized water of 25mL100 DEG C, add thermal agitation 15min, obtain NH
4vO
3concentration is the vanadic salts solution of 0.4mol/L; Be that vanadic salts dropwise joins in bismuth salting liquid by 1:1 according to the mol ratio of Bi and V, stir 30min, obtain mixed liquor;
Step 2: regulate the pH value of mixed liquor to be 8 by the NaOH solution that concentration is 5mol/L, stir 30min;
Step 3: by six water ytterbium nitrate (Yb (NO
3)
36H
2o) be that 10:100 joins in the mixed liquor after have adjusted pH value according to the mol ratio of Yb and Bi, stir 30min, obtain precursor liquid;
Step 4: microwave hydrothermal reaction kettle precursor liquid being put into polytetrafluoroethylene (PTFE) material, the packing ratio of microwave hydrothermal reaction kettle is 60%, microwave hydrothermal reaction is put into after microwave hydrothermal reaction kettle being sealed, select micro-wave digestion (temperature control) scheme, setting microwave power is 300W, from room temperature to 100 DEG C, at 100 DEG C of insulation 6min; Then 150 DEG C are warming up to from 100 DEG C, at 150 DEG C of insulation 6min; Be warming up to 180 DEG C from 150 DEG C again, after 180 DEG C of insulation 35min, terminate reaction, then naturally cool to room temperature;
Step 5: the sediment that will react generation through step 4 takes out, and after spending deionized water to neutrality, then uses absolute ethanol washing 3 times, then at 70 DEG C dry 10h, obtain ytterbium doping pucherite visible-light photocatalyst.
Fig. 1 is different Yb
3+the XRD collection of illustrative plates of the ytterbium doping pucherite visible-light photocatalyst prepared under doping, wherein a is unadulterated BiVO
4xRD collection of illustrative plates, unadulterated BiVO
4be according to preparation method of the present invention, undope Yb (NO in step 3
3)
36H
2o obtains; B ~ e is respectively the XRD collection of illustrative plates of the ytterbium doping pucherite visible-light photocatalyst prepared according to the method for embodiment 1 ~ embodiment 4.As can be seen from Figure 1, unadulterated BiVO
4all diffraction maximums consistent with PDF card (JCPDS NO.75-2480), illustrate that it is monocline scheelite type structure; All diffraction maximums of the ytterbium doping pucherite visible-light photocatalyst after doping are all coincide with PDF card (JCPDS NO.14-0133), and illustrate that it is cubic Zircon cut structure, this illustrates Yb
3+doping is to BiVO
4crystal structure have a significant impact.
Fig. 2 is different Yb
3+degradation rate-the time graph of the ytterbium doping pucherite visible-light photocatalyst rhodamine B degradation prepared under doping, wherein a is unadulterated BiVO
4degradation curve, unadulterated BiVO
4be according to preparation method of the present invention, undope Yb (NO in step 3
3)
36H
2o obtains; B ~ e is respectively the degradation curve of the ytterbium doping pucherite visible-light photocatalyst prepared according to the method for embodiment 1 ~ embodiment 4.The C of ordinate in Fig. 2
t/ C
0for the ratio of the concentration after certain rhodamine B degraded and its initial concentration in moment.As can be seen from Figure 2, under visible light illumination, the photocatalytic activity of ytterbium doping pucherite visible-light photocatalyst is all obviously better than the monoclinic phase BiVO that do not adulterate
4photocatalytic activity, wherein the ytterbium doping degradation rate of pucherite visible-light photocatalyst to rhodamine B solution prepared of embodiment 3 is the highest, and after radiation of visible light 120min, rhodamine B degradation rate can reach 96.7%.Therefore the ytterbium doping pucherite visible-light photocatalyst that prepared by the present invention can be used in degradation of organic substances.
The foregoing is only one embodiment of the present invention, it not whole or unique embodiment, the conversion of those of ordinary skill in the art by reading description of the present invention to any equivalence that technical solution of the present invention is taked, is claim of the present invention and contains.
Claims (8)
1. a preparation method for ytterbium doping pucherite visible-light photocatalyst, is characterized in that, comprise the following steps:
Step 1: by Bi (NO
3)
35H
2o is soluble in water, stirs, and obtains bismuth salting liquid; By NH
4vO
3be dissolved in the water of 90 ~ 100 DEG C, heating stirs, and obtains vanadic salts solution; Be that vanadic salts solution joins in bismuth salting liquid by 1:1 according to the mol ratio of Bi and V, stir, obtain mixed liquor; Wherein Bi (NO in bismuth salting liquid
3)
35H
2the concentration of O is 0.4mol/L; NH in vanadic salts solution
4vO
3concentration be 0.4mol/L;
Step 2: regulate the pH value of mixed liquor to be 8 by the NaOH solution that concentration is 5mol/L, stir;
Step 3: by Yb (NO
3)
36H
2in mixed liquor after O joins and have adjusted pH value, stir, obtain precursor liquid, wherein the mol ratio of Yb and Bi is (4 ~ 10): 100;
Step 4: precursor liquid is put into microwave hydrothermal reaction kettle, then put into microwave hydrothermal reaction after microwave hydrothermal reaction kettle being sealed, setting microwave power is 300W, from room temperature to 100 DEG C, at 100 DEG C of insulation 6min; Then 150 DEG C are warming up to from 100 DEG C, at 150 DEG C of insulation 6min; Be warming up to 180 DEG C from 150 DEG C again, after 180 DEG C of insulation 35min, terminate reaction, then naturally cool to room temperature;
Step 5: taken out by the sediment reacting generation through step 4, washing, drying, obtain ytterbium doping pucherite visible-light photocatalyst.
2. the preparation method of ytterbium doping pucherite visible-light photocatalyst according to claim 1, is characterized in that: by Bi (NO in described step 1
3)
35H
2the O required time that stirs soluble in water is 30min; By NH
4vO
3being dissolved in the water of 90 ~ 100 DEG C heating required time that stirs is 15min; Vanadic salts solution being added drop-wise in bismuth salting liquid the required time that stirs is 30min.
3. the preparation method of ytterbium doping pucherite visible-light photocatalyst according to claim 1, is characterized in that: the required time that stirs in described step 2 is 30min; Required time that stirs in described step 3 is 30min.
4. the preparation method of ytterbium doping pucherite visible-light photocatalyst according to claim 1, is characterized in that: in described step 4, the packing ratio of reactor is 50% ~ 60%.
5. the preparation method of ytterbium doping pucherite visible-light photocatalyst according to claim 1, is characterized in that: the washing in described step 5 is after spending deionized water to neutrality, then uses absolute ethanol washing.
6. the preparation method of ytterbium doping pucherite visible-light photocatalyst according to claim 1, is characterized in that: the drying in described step 5 is dry 10 ~ 12h at 60 ~ 70 DEG C.
7., according to the ytterbium doping pucherite visible-light photocatalyst that the preparation method of the ytterbium doping pucherite visible-light photocatalyst in claim 1-6 described in any one obtains, it is characterized in that: its main component is BiVO
4, be cubic Zircon cut structure, and BiVO
4lattice in containing Yb
3+, wherein the mol ratio of Yb element and Bi element is (4 ~ 10): 100.
8. the ytterbium doping pucherite visible-light photocatalyst that the preparation method adulterating pucherite visible-light photocatalyst according to the ytterbium in claim 1-6 described in any one obtains is for the application of degradation of organic substances.
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| CN105148899B (en) * | 2015-09-29 | 2017-12-22 | 陕西科技大学 | A kind of rare earth codope BiVO with upper transfer characteristic4Photochemical catalyst and its preparation method and application |
| CN108212187B (en) * | 2018-01-26 | 2021-02-19 | 湖北文理学院 | Fe doped Bi2O2CO3Preparation method of photocatalyst and Fe-doped Bi2O2CO3Photocatalyst and process for producing the same |
| CN110075824A (en) * | 2019-04-18 | 2019-08-02 | 西安建筑科技大学 | A kind of preparation and its application of Yb doping vario-property zinc stannate optoelectronic pole |
| CN112058257B8 (en) * | 2020-09-30 | 2023-06-02 | 攀枝花学院 | Rare earth Tb doped bismuth vanadate photocatalyst and preparation method thereof |
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