CN103433019A - Sm-doped BiVO4 photocatalyst as well as preparation method and application thereof - Google Patents

Sm-doped BiVO4 photocatalyst as well as preparation method and application thereof Download PDF

Info

Publication number
CN103433019A
CN103433019A CN2013103568375A CN201310356837A CN103433019A CN 103433019 A CN103433019 A CN 103433019A CN 2013103568375 A CN2013103568375 A CN 2013103568375A CN 201310356837 A CN201310356837 A CN 201310356837A CN 103433019 A CN103433019 A CN 103433019A
Authority
CN
China
Prior art keywords
bivo
photochemical catalyst
preparation
doping
stirs
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN2013103568375A
Other languages
Chinese (zh)
Other versions
CN103433019B (en
Inventor
谈国强
罗洋洋
张丽丽
董国华
任慧君
夏傲
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Yancheng Qinglong Jinbang water Co.,Ltd.
Original Assignee
Shaanxi University of Science and Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shaanxi University of Science and Technology filed Critical Shaanxi University of Science and Technology
Priority to CN201310356837.5A priority Critical patent/CN103433019B/en
Publication of CN103433019A publication Critical patent/CN103433019A/en
Application granted granted Critical
Publication of CN103433019B publication Critical patent/CN103433019B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Landscapes

  • Catalysts (AREA)

Abstract

The invention discloses an Sm-doped BiVO4 photocatalyst as well as a preparation method and application thereof. The Sm-doped BiVO4 photocatalyst takes BiVO4 as a main component and is of a tetragonal zircon phase structure; a crystal lattice of the BiVO4 contains Sm<3+>. The preparation method comprises the following steps: respectively dissolving bismuth nitrate pentahydrate and ammonium metavanadate into water to obtain bismuth salt solution and vanadium salt solution; adding the vanadium salt solution into the bismuth salt solution under the condition that the mol ratio of Bi to V is 1:1 to obtain a mixed solution; adjusting the pH value of the mixed solution to be 8; adding samarium nitrate hexahydrate, wherein the mol ratio of Sm to Bi is (2.04-13.64):100; preserving heat at the power of 300W and the temperature of 180DEG C for 40 minutes by using a microwave hydrothermal method to obtain the Sm-doped BiVO4 photocatalyst. According to the preparation method disclosed by the invention, the Sm-doped BiVO4 photocatalyst is further synthesized; the preparation method has the advantages of fewer flows, simplicity in operation, short reaction time and mild reaction condition; the synthesized Sm-doped BiVO4 photocatalyst has higher photocatalytic activity and can be used for degrading environmental pollutants.

Description

A kind of Sm doping BiVO 4photochemical catalyst and its preparation method and application
Technical field
The invention belongs to field of functional materials, be specifically related to a kind of Sm doping BiVO 4photochemical catalyst and its preparation method and application.
Background technology
Along with modern civilization and scientific and technological develop rapidly, environmental pollution is more and more serious, Environmental Pollution and Control has become the important topic of global common concern, and in nearly twenty or thirty year, the mankind's problem of curbing environmental pollution that develops into of Photocatalyst provides an effective approach.Although with TiO 2for the light of representative urges material list to reveal good photocatalysis performance, but often there is visible light-responded narrow range, can't efficiently utilize the problem of sunshine, therefore, further improving TiO 2in the time of photocatalysis performance, the searching of novel visible responsive photocatalyst is also showed to desirability and urgency.
BiVO 4as a kind of novel semi-conductor photochemical catalyst with visible light activity of in recent years finding, obtained paying close attention to widely.Ke Dingning etc. are by Bi (NO 3) 35H 2o and NH 4vO 3be dissolved in respectively in salpeter solution, solution adds CTAB after mixing again, obtains well-crystallized's monoclinic phase pucherite under hydrothermal condition, yet, BiVO 4the electronics that optical excitation generates in body is difficult to migration, very easily and hole-recombination, the photo-quantum efficiency of catalyst and visible light activity is reduced.In order to improve BiVO 4photo-quantum efficiency and visible light activity, often it is carried out to modification.
Doping can improve pure phase BiVO 4light-catalyzed reaction efficiency and selective, at present to BiVO 4the method of carrying out doping vario-property mostly is infusion process, in traditional solid reaction process, chemical coprecipitation, sol-gel process and hydro-thermal method etc., prepares pure phase BiVO 4after, then select suitable source metal to adopt the method for dipping to be adulterated to it, the method flow process is many, complex process.
Summary of the invention
The object of the present invention is to provide a kind of Sm doping BiVO 4photochemical catalyst and its preparation method and application, the method is simple to operate, and the reaction time is short, reaction condition gentleness, and the Sm of preparation doping BiVO 4photochemical catalyst has higher photocatalytic activity.
For achieving the above object, the technical solution used in the present invention is:
A kind of Sm doping BiVO 4photochemical catalyst, its main component is BiVO 4, be cubic zircon phase structure, and BiVO 4lattice in contain Sm 3+, wherein the mol ratio of Sm element and Bi element is (2.04～13.64): 100.
Its pattern is the Square-edge column.
A kind of Sm doping BiVO 4the preparation method of photochemical catalyst comprises the following steps:
Step 1: by Bi (NO 3) 35H 2o is soluble in water, stirs, and obtains the bismuth salting liquid; By NH 4vO 3be dissolved in the water of 100 ℃, heating stirs, and obtains vanadic salts solution;
Step 2: the mol ratio by Bi and V is that 1:1 is added to vanadic salts solution in the bismuth salting liquid, stirs, and obtains mixed liquor;
Step 3: the pH value of regulating mixed liquor is 8, stirs;
Step 4: by Sm (NO 3) 36H 2o joins in the mixed liquor of having regulated after the pH value, stirs, and obtains precursor liquid, and wherein the mol ratio of Sm and Bi is (2.04～13.64): 100;
Step 5: precursor liquid is added in microwave hydrothermal reaction kettle, the microwave hydrothermal reaction kettle sealing is placed in microwave assisted hydrothermal synthesis apparatus, setting pressure is 1.2MPa, under the microwave power of 300W, from room temperature, is warming up to 100 ℃, at 100 ℃ of insulation 8min; Then be warming up to 150 ℃ from 100 ℃, at 150 ℃ of insulation 8min; Be warming up to 180 ℃, end reaction after 180 ℃ of insulation 40min from 150 ℃ again;
Step 6: question response is cooled to room temperature after finishing, and takes out the sediment in microwave hydrothermal reaction kettle, washing, and drying, obtain Sm doping BiVO 4photochemical catalyst.
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.
In described step 1 by Bi (NO 3) 35H 2o stirring soluble in water 20min; By NH 4vO 3be dissolved in the water of 100 ℃, add thermal agitation 20min under 90-100 ℃; Stirring in described step 2 is to stir 15min on magnetic stirring apparatus.
The NaOH solution that is 5mol/L by concentration in described step 3 is regulated the pH value of mixed liquor, and the rate of addition of NaOH solution is less than or equal to 1mL/min.
Stirring in described step 3 is to stir 25min on magnetic stirring apparatus; Stirring in described step 4 is to stir 20min on magnetic stirring apparatus.
In described step 5, the packing ratio of microwave hydrothermal reaction kettle is 55%.
Washing in described step 6 is extremely neutral by deionized water and absolute ethanol washing sediment; Described drying is at 75 ℃ of lower freeze-day with constant temperature 24h.
The Sm BiVO that adulterates 4the application of photochemical catalyst aspect the photocatalytic degradation environmental contaminants.
With respect to prior art, beneficial effect of the present invention is:
Sm doping BiVO provided by the invention 4the preparation method of photochemical catalyst, with five water bismuth nitrate (Bi (NO 3) 35H 2o) be the bismuth source, ammonium metavanadate (NH 4vO 3) be the vanadium source, preparation BiVO 4, then with six water samaric nitrate (Sm (NO 3) 36H 2o) be the samarium source, to BiVO 4carry out Sm 3+doping, prepare Sm doping BiVO 4photochemical catalyst.The present invention is by Sm 3+introduce BiVO 4lattice in, improved pure phase BiVO 4the efficiency of photocatalysis to degrade organic matter under visible ray.The present invention adopts microwave-hydrothermal method one-step synthesis Sm doping BiVO 4photochemical catalyst, combine the advantage of heating using microwave and hydro-thermal method, and its flow process is simple and easy, simple to operate, and the reaction time is short, the reaction condition gentleness, and firing rate is fast, and homogeneous heating has overcome the hydro-thermal container and has heated inhomogeneous shortcoming, has improved operating efficiency.
Sm doping BiVO provided by the invention 4photochemical catalyst is cubic zircon phase structure, and its main component is BiVO 4, and BiVO 4lattice in contain Sm 3+, there is high photocatalytic activity, be mainly used in photocatalytic degradation environmental contaminants aspect, improved pure phase BiVO 4photocatalysis performance, reached pure phase BiVO 4carry out the purpose of doping vario-property, have broad application prospects.
Further, Sm doping BiVO provided by the invention 4the photochemical catalyst particle size distribution is even, has Square-edge column pattern.
The accompanying drawing explanation
Fig. 1 is the Sm doping BiVO of the embodiment of the present invention 3 preparations 4the FE-SEM figure of photochemical catalyst;
Fig. 2 is the different Sm of the present invention 3+the Sm doping BiVO prepared under doping 4the XRD spectra of photochemical catalyst, wherein a is unadulterated BiVO 4the XRD collection of illustrative plates, b～g is respectively the Sm doping BiVO of embodiment 1～embodiment 6 preparation 4the XRD collection of illustrative plates of photochemical catalyst;
Fig. 3 is the different Sm of the present invention 3+the Sm doping BiVO prepared under doping 4degradation rate-the time graph of the rhodamine B degradation of photochemical catalyst, the degradation curve that wherein RhB is rhodamine B self while not adding catalyst; A is unadulterated BiVO 4degradation curve, b～g is respectively the Sm doping BiVO of embodiment 1～embodiment 6 preparation 4the degradation curve of photochemical catalyst;
The specific embodiment
Below in conjunction with specific embodiments and the drawings, the present invention is described in further detail.
Embodiment 1:
A kind of Sm doping BiVO 4photochemical catalyst, its main component is BiVO 4, be cubic zircon phase structure, and BiVO 4lattice in contain Sm 3+, wherein the mol ratio of Sm element and Bi element is 2.04:100.
A kind of Sm doping BiVO 4the preparation method of photochemical catalyst comprises the following steps:
Step 1: by Bi (NO 3) 35H 2o is dissolved in deionized water, stirs 20min on magnetic stirring apparatus, obtains Bi (NO 3) 35H 2the bismuth salting liquid that O concentration is 0.4mol/L; By NH 4vO 3be dissolved in the deionized water of 100 ℃, add thermal agitation 20min under 100 ℃, obtain NH 4vO 3the vanadic salts solution that concentration is 0.4mol/L;
Step 2: the mol ratio by Bi and V is that 1:1 slowly is added drop-wise to vanadic salts solution in the bismuth salting liquid, stirs 15min on magnetic stirring apparatus, obtains mixed liquor;
Step 3: take the rate of addition of 1mL/min to dripping the NaOH solution that concentration is 5mol/L in mixed liquor, the pH that regulates mixed liquor is 8, and stirs 25min on magnetic stirring apparatus;
Step 4: by Sm (NO 3) 36H 2o joins in the mixed liquor of having regulated after the pH value, stirs 20min on magnetic stirring apparatus, is mixed with precursor liquid, and wherein the mol ratio of Sm and Bi is 2.04:100;
Step 5: precursor liquid is added in microwave hydrothermal reaction kettle, the packing ratio of controlling microwave hydrothermal reaction kettle is 55%, then the microwave hydrothermal reaction kettle sealing is placed in the microwave hydrothermal synthesizer, select the microwave temperature controlling mode, setting pressure is 1.2MPa, under the microwave power of 300W, be warming up to 100 ℃ from room temperature, at 100 ℃ of insulation 8min; Then be warming up to 150 ℃ from 100 ℃, at 150 ℃ of insulation 8min; Be warming up to 180 ℃, end reaction after 180 ℃ of insulation 40min from 150 ℃ again;
Step 6: question response is cooled to room temperature after finishing, and takes out the sediment in microwave hydrothermal reaction kettle, extremely neutral by deionized water and absolute ethanol washing, then, at 75 ℃ of lower freeze-day with constant temperature 24h, obtains Sm doping BiVO4 photochemical catalyst.
Embodiment 2:
A kind of Sm doping BiVO 4photochemical catalyst, its main component is BiVO 4, be cubic zircon phase structure, and BiVO 4lattice in contain Sm 3+, wherein the mol ratio of Sm element and Bi element is 4.17:100.
A kind of Sm doping BiVO 4the preparation method of photochemical catalyst comprises the following steps:
Step 1: by Bi (NO 3) 35H 2o is dissolved in deionized water, stirs 20min on magnetic stirring apparatus, obtains Bi (NO 3) 35H 2the bismuth salting liquid that O concentration is 0.4mol/L; By NH 4vO 3be dissolved in the deionized water of 100 ℃, add thermal agitation 20min under 90 ℃, obtain NH 4vO 3the vanadic salts solution that concentration is 0.4mol/L;
Step 2: the mol ratio by Bi and V is that 1:1 slowly is added drop-wise to vanadic salts solution in the bismuth salting liquid, stirs 15min on magnetic stirring apparatus, obtains mixed liquor;
Step 3: take the rate of addition of 0.5mL/min to dripping the NaOH solution that concentration is 5mol/L in mixed liquor, the pH that regulates mixed liquor is 8, and stirs 25min on magnetic stirring apparatus;
Step 4: by Sm (NO 3) 36H 2o joins in the mixed liquor of having regulated after the pH value, stirs 20min on magnetic stirring apparatus, is mixed with precursor liquid, and wherein the mol ratio of Sm and Bi is 4.17:100;
Step 5: precursor liquid is added in microwave hydrothermal reaction kettle, the packing ratio of controlling microwave hydrothermal reaction kettle is 55%, then the microwave hydrothermal reaction kettle sealing is placed in the microwave hydrothermal synthesizer, select the microwave temperature controlling mode, setting pressure is 1.2MPa, under the microwave power of 300W, be warming up to 100 ℃ from room temperature, at 100 ℃ of insulation 8min; Then be warming up to 150 ℃ from 100 ℃, at 150 ℃ of insulation 8min; Be warming up to 180 ℃, end reaction after 180 ℃ of insulation 40min from 150 ℃ again;
Step 6: question response is cooled to room temperature after finishing, and takes out the sediment in microwave hydrothermal reaction kettle, extremely neutral by deionized water and absolute ethanol washing, then, at 75 ℃ of lower freeze-day with constant temperature 24h, obtains Sm doping BiVO 4photochemical catalyst.
Embodiment 3:
A kind of Sm doping BiVO 4photochemical catalyst, its main component is BiVO 4, be cubic zircon phase structure, and BiVO 4lattice in contain Sm 3+, wherein the mol ratio of Sm element and Bi element is 6.38:100.
A kind of Sm doping BiVO 4the preparation method of photochemical catalyst comprises the following steps:
Step 1: by Bi (NO 3) 35H 2o is dissolved in deionized water, stirs 20min on magnetic stirring apparatus, obtains Bi (NO 3) 35H 2the bismuth salting liquid that O concentration is 0.4mol/L; By NH 4vO 3be dissolved in the deionized water of 100 ℃, add thermal agitation 20min under 95 ℃, obtain NH 4vO 3the vanadic salts solution that concentration is 0.4mol/L;
Step 2: the mol ratio by Bi and V is that 1:1 slowly is added drop-wise to vanadic salts solution in the bismuth salting liquid, stirs 15min on magnetic stirring apparatus, obtains mixed liquor;
Step 3: take the rate of addition of 0.8mL/min to dripping the NaOH solution that concentration is 5mol/L in mixed liquor, the pH that regulates mixed liquor is 8, and stirs 25min on magnetic stirring apparatus;
Step 4: by Sm (NO 3) 36H 2o joins in the mixed liquor of having regulated after the pH value, stirs 20min on magnetic stirring apparatus, is mixed with precursor liquid, and wherein the mol ratio of Sm and Bi is 6.38:100;
Step 5: precursor liquid is added in microwave hydrothermal reaction kettle, the packing ratio of controlling microwave hydrothermal reaction kettle is 55%, then the microwave hydrothermal reaction kettle sealing is placed in the microwave hydrothermal synthesizer, select the microwave temperature controlling mode, setting pressure is 1.2MPa, under the microwave power of 300W, be warming up to 100 ℃ from room temperature, at 100 ℃ of insulation 8min; Then be warming up to 150 ℃ from 100 ℃, at 150 ℃ of insulation 8min; Be warming up to 180 ℃, end reaction after 180 ℃ of insulation 40min from 150 ℃ again;
Step 6: question response is cooled to room temperature after finishing, and takes out the sediment in microwave hydrothermal reaction kettle, extremely neutral by deionized water and absolute ethanol washing, then, at 75 ℃ of lower freeze-day with constant temperature 24h, obtains Sm doping BiVO 4photochemical catalyst.
Fig. 1 is the Sm doping BiVO of embodiment 3 preparations 4the FE-SEM figure of photochemical catalyst, as can be seen from the figure its crystal morphology is the Square-edge column, cylinder is about 100nm in minor axis direction size.
Embodiment 4:
A kind of Sm doping BiVO 4photochemical catalyst, its main component is BiVO 4, be cubic zircon phase structure, and BiVO 4lattice in contain Sm 3+, wherein the mol ratio of Sm element and Bi element is 8.70:100.
A kind of Sm doping BiVO 4the preparation method of photochemical catalyst comprises the following steps:
Step 1: by Bi (NO 3) 35H 2o is dissolved in deionized water, stirs 20min on magnetic stirring apparatus, obtains Bi (NO 3) 35H 2the bismuth salting liquid that O concentration is 0.4mol/L; By NH 4vO 3be dissolved in the deionized water of 100 ℃, add thermal agitation 20min under 100 ℃, obtain NH 4vO 3the vanadic salts solution that concentration is 0.4mol/L;
Step 2: the mol ratio by Bi and V is that 1:1 slowly is added drop-wise to vanadic salts solution in the bismuth salting liquid, stirs 15min on magnetic stirring apparatus, obtains mixed liquor;
Step 3: take the rate of addition of 1mL/min to dripping the NaOH solution that concentration is 5mol/L in mixed liquor, the pH that regulates mixed liquor is 8, and stirs 25min on magnetic stirring apparatus;
Step 4: by Sm (NO 3) 36H 2o joins in the mixed liquor of having regulated after the pH value, stirs 20min on magnetic stirring apparatus, is mixed with precursor liquid, and wherein the mol ratio of Sm and Bi is 8.70:100;
Step 5: precursor liquid is added in microwave hydrothermal reaction kettle, the packing ratio of controlling microwave hydrothermal reaction kettle is 55%, then the microwave hydrothermal reaction kettle sealing is placed in the microwave hydrothermal synthesizer, select the microwave temperature controlling mode, setting pressure is 1.2MPa, under the microwave power of 300W, be warming up to 100 ℃ from room temperature, at 100 ℃ of insulation 8min; Then be warming up to 150 ℃ from 100 ℃, at 150 ℃ of insulation 8min; Be warming up to 180 ℃, end reaction after 180 ℃ of insulation 40min from 150 ℃ again;
Step 6: question response is cooled to room temperature after finishing, and takes out the sediment in microwave hydrothermal reaction kettle, extremely neutral by deionized water and absolute ethanol washing, then, at 75 ℃ of lower freeze-day with constant temperature 24h, obtains Sm doping BiVO 4photochemical catalyst.
Embodiment 5:
A kind of Sm doping BiVO 4photochemical catalyst, its main component is BiVO 4, be cubic zircon phase structure, and BiVO 4lattice in contain Sm 3+, wherein the mol ratio of Sm element and Bi element is 11.11:100.
A kind of Sm doping BiVO 4the preparation method of photochemical catalyst comprises the following steps:
Step 1: by Bi (NO 3) 35H 2o is dissolved in deionized water, stirs 20min on magnetic stirring apparatus, obtains Bi (NO 3) 35H 2the bismuth salting liquid that O concentration is 0.4mol/L; By NH 4vO 3be dissolved in the deionized water of 100 ℃, add thermal agitation 20min under 98 ℃, obtain NH 4vO 3the vanadic salts solution that concentration is 0.4mol/L;
Step 2: the mol ratio by Bi and V is that 1:1 slowly is added drop-wise to vanadic salts solution in the bismuth salting liquid, stirs 15min on magnetic stirring apparatus, obtains mixed liquor;
Step 3: take the rate of addition of 0.3mL/min to dripping the NaOH solution that concentration is 5mol/L in mixed liquor, the pH that regulates mixed liquor is 8, and stirs 25min on magnetic stirring apparatus;
Step 4: by Sm (NO 3) 36H 2o joins in the mixed liquor of having regulated after the pH value, stirs 20min on magnetic stirring apparatus, is mixed with precursor liquid, and wherein the mol ratio of Sm and Bi is 11.11:100;
Step 5: precursor liquid is added in microwave hydrothermal reaction kettle, the packing ratio of controlling microwave hydrothermal reaction kettle is 55%, then the microwave hydrothermal reaction kettle sealing is placed in the microwave hydrothermal synthesizer, select the microwave temperature controlling mode, setting pressure is 1.2MPa, under the microwave power of 300W, be warming up to 100 ℃ from room temperature, at 100 ℃ of insulation 8min; Then be warming up to 150 ℃ from 100 ℃, at 150 ℃ of insulation 8min; Be warming up to 180 ℃, end reaction after 180 ℃ of insulation 40min from 150 ℃ again;
Step 6: question response is cooled to room temperature after finishing, and takes out the sediment in microwave hydrothermal reaction kettle, extremely neutral by deionized water and absolute ethanol washing, then, at 75 ℃ of lower freeze-day with constant temperature 24h, obtains Sm doping BiVO 4photochemical catalyst.
Embodiment 6:
A kind of Sm doping BiVO 4photochemical catalyst, its main component is BiVO 4, be cubic zircon phase structure, and BiVO 4lattice in contain Sm 3+, wherein the mol ratio of Sm element and Bi element is 13.64:100.
A kind of Sm doping BiVO 4the preparation method of photochemical catalyst comprises the following steps:
Step 1: by Bi (NO 3) 35H 2o is dissolved in deionized water, stirs 20min on magnetic stirring apparatus, obtains Bi (NO 3) 35H 2the bismuth salting liquid that O concentration is 0.4mol/L; By NH 4vO 3be dissolved in the deionized water of 100 ℃, add thermal agitation 20min under 96 ℃, obtain NH 4vO 3the vanadic salts solution that concentration is 0.4mol/L;
Step 2: the mol ratio by Bi and V is that 1:1 slowly is added drop-wise to vanadic salts solution in the bismuth salting liquid, stirs 15min on magnetic stirring apparatus, obtains mixed liquor;
Step 3: take the rate of addition of 0.4mL/min to dripping the NaOH solution that concentration is 5mol/L in mixed liquor, the pH that regulates mixed liquor is 8, and stirs 25min on magnetic stirring apparatus;
Step 4: by Sm (NO 3) 36H 2o joins in the mixed liquor of having regulated after the pH value, stirs 20min on magnetic stirring apparatus, is mixed with precursor liquid, and wherein the mol ratio of Sm and Bi is 13.64:100;
Step 5: precursor liquid is added in microwave hydrothermal reaction kettle, the packing ratio of controlling microwave hydrothermal reaction kettle is 55%, then the microwave hydrothermal reaction kettle sealing is placed in the microwave hydrothermal synthesizer, select the microwave temperature controlling mode, setting pressure is 1.2MPa, under the microwave power of 300W, be warming up to 100 ℃ from room temperature, at 100 ℃ of insulation 8min; Then be warming up to 150 ℃ from 100 ℃, at 150 ℃ of insulation 8min; Be warming up to 180 ℃, end reaction after 180 ℃ of insulation 40min from 150 ℃ again;
Step 6: question response is cooled to room temperature after finishing, and takes out the sediment in microwave hydrothermal reaction kettle, extremely neutral by deionized water and absolute ethanol washing, then, at 75 ℃ of lower freeze-day with constant temperature 24h, obtains Sm doping BiVO 4photochemical catalyst.
Fig. 2 is different Sm 3+the Sm doping BiVO prepared under doping 4the XRD collection of illustrative plates of photochemical catalyst, wherein a is unadulterated BiVO 4the XRD collection of illustrative plates, unadulterated BiVO 4be according to preparation method of the present invention, Sm (NO undopes in step 4 3) 36H 2o obtains; B～g is respectively the Sm doping BiVO of embodiment 1～embodiment 6 preparations 4the XRD collection of illustrative plates of photochemical catalyst.In Fig. 2, the intensity of ordinate is relative intensity, and the 2-Theta of abscissa is angle of diffraction.As can be seen from the figure, unadulterated BiVO 4all diffraction maximums and PDF card (JCPDS NO.75-1866) coincide, and illustrate that its crystalline phase is monocline scheelite phase, the Sm BiVO that adulterates 4all diffraction maximums of photochemical catalyst are all coincide with PDF card (JCPDS NO.14-0133), illustrate that its crystalline phase is all cubic zircon phase.
Fig. 3 is different Sm 3+the Sm doping BiVO prepared under doping 4degradation rate-the time graph of the rhodamine B degradation of photochemical catalyst, the degradation curve that wherein RhB is rhodamine B self while not adding catalyst; A is unadulterated BiVO 4degradation curve, unadulterated BiVO 4be according to preparation method of the present invention, Sm (NO undopes in step 4 3) 36H 2o obtains; B～g is respectively the Sm doping BiVO of embodiment 1～embodiment 6 preparations 4the degradation curve of photochemical catalyst.The C/C of ordinate in Fig. 3 0for the concentration after certain rhodamine B degraded constantly and the ratio of its initial concentration.As can be seen from the figure Sm doping BiVO 4the degradation effect of photochemical catalyst all obviously is better than unadulterated BiVO 4degradation effect, and the Sm doping BiVO of embodiment 3 preparation 4photochemical catalyst degradation rate to rhodamine B under the irradiation of 120min reaches 96.15%, and unadulterated BiVO 4degradation rate to rhodamine B after the 120min irradiation is only 37.26%.Therefore, the Sm doping BiVO of embodiment 3 preparations 4photochemical catalyst is than unadulterated pure phase BiVO 4degradation rate after the 120min irradiation has improved 58.89%.Therefore the Sm doping BiVO that prepared by the present invention 4photochemical catalyst can be used in degradation of organic substances, and can be applied to photocatalytic degradation environmental contaminants aspect.
The foregoing is only one embodiment of the present invention, it not whole or unique embodiment, the conversion of any equivalence that those of ordinary skills take technical solution of the present invention by reading specification of the present invention, be claim of the present invention and contain.

Claims (10)

1. Sm doping BiVO 4photochemical catalyst is characterized in that: its main component is BiVO 4, be cubic zircon phase structure, and BiVO 4lattice in contain Sm 3+, wherein the mol ratio of Sm element and Bi element is (2.04～13.64): 100.
2. Sm according to claim 1 doping BiVO 4photochemical catalyst is characterized in that: its pattern is the Square-edge column.
3. Sm doping BiVO 4the preparation method of photochemical catalyst, is characterized in that, comprises the following steps:
Step 1: by Bi (NO 3) 35H 2o is soluble in water, stirs, and obtains the bismuth salting liquid; By NH 4vO 3be dissolved in the water of 100 ℃, heating stirs, and obtains vanadic salts solution;
Step 2: the mol ratio by Bi and V is that 1:1 is added to vanadic salts solution in the bismuth salting liquid, stirs, and obtains mixed liquor;
Step 3: the pH value of regulating mixed liquor is 8, stirs;
Step 4: by Sm (NO 3) 36H 2o joins in the mixed liquor of having regulated after the pH value, stirs, and obtains precursor liquid, and wherein the mol ratio of Sm and Bi is (2.04～13.64): 100;
Step 5: precursor liquid is added in microwave hydrothermal reaction kettle, the microwave hydrothermal reaction kettle sealing is placed in microwave assisted hydrothermal synthesis apparatus, setting pressure is 1.2MPa, under the microwave power of 300W, from room temperature, is warming up to 100 ℃, at 100 ℃ of insulation 8min; Then be warming up to 150 ℃ from 100 ℃, at 150 ℃ of insulation 8min; Be warming up to 180 ℃, end reaction after 180 ℃ of insulation 40min from 150 ℃ again;
Step 6: question response is cooled to room temperature after finishing, and takes out the sediment in microwave hydrothermal reaction kettle, washing, and drying, obtain Sm doping BiVO 4photochemical catalyst.
4. Sm according to claim 3 doping BiVO 4the preparation method of photochemical catalyst is characterized in that: 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.
5. according to the described Sm doping of claim 3 or 4 BiVO 4the preparation method of photochemical catalyst is characterized in that: in described step 1 by Bi (NO 3) 35H 2o stirring soluble in water 20min; By NH 4vO 3be dissolved in the water of 100 ℃, add thermal agitation 20min under 90-100 ℃; Stirring in described step 2 is to stir 15min on magnetic stirring apparatus.
6. Sm according to claim 3 doping BiVO 4the preparation method of photochemical catalyst is characterized in that: the NaOH solution that is 5mol/L by concentration in described step 3 is regulated the pH value of mixed liquor, and the rate of addition of NaOH solution is less than or equal to 1mL/min.
7. according to the described Sm doping of claim 3 or 6 BiVO 4the preparation method of photochemical catalyst is characterized in that: stirring in described step 3 is to stir 25min on magnetic stirring apparatus; Stirring in described step 4 is to stir 20min on magnetic stirring apparatus.
8. Sm according to claim 3 doping BiVO 4the preparation method of photochemical catalyst is characterized in that: in described step 5, the packing ratio of microwave hydrothermal reaction kettle is 55%.
9. Sm according to claim 3 doping BiVO 4the preparation method of photochemical catalyst is characterized in that: the washing in described step 6 is extremely neutral by deionized water and absolute ethanol washing sediment; Described drying is at 75 ℃ of lower freeze-day with constant temperature 24h.
10. Sm according to claim 1 doping BiVO 4the application of photochemical catalyst aspect the photocatalytic degradation environmental contaminants.
CN201310356837.5A 2013-08-15 2013-08-15 A kind of Sm doping BiVO 4photochemical catalyst and its preparation method and application Active CN103433019B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201310356837.5A CN103433019B (en) 2013-08-15 2013-08-15 A kind of Sm doping BiVO 4photochemical catalyst and its preparation method and application

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201310356837.5A CN103433019B (en) 2013-08-15 2013-08-15 A kind of Sm doping BiVO 4photochemical catalyst and its preparation method and application

Publications (2)

Publication Number Publication Date
CN103433019A true CN103433019A (en) 2013-12-11
CN103433019B CN103433019B (en) 2015-08-12

Family

ID=49686788

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201310356837.5A Active CN103433019B (en) 2013-08-15 2013-08-15 A kind of Sm doping BiVO 4photochemical catalyst and its preparation method and application

Country Status (1)

Country Link
CN (1) CN103433019B (en)

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107159197A (en) * 2017-05-25 2017-09-15 上海交通大学 Mischcrystal photocatalyst with dodecahedron pattern and preparation method thereof
CN107469807A (en) * 2017-09-08 2017-12-15 郑州轻工业学院 A kind of monoclinic phase BiVO4：The high pressure method for preparing of Re catalysis materials
CN111992201A (en) * 2020-08-21 2020-11-27 重庆交通大学 One-step synthesis of BiVO by microwave hydrothermal method4/InVO4Method and application of photocatalyst
CN112058257A (en) * 2020-09-30 2020-12-11 攀枝花学院 Rare earth Tb doped bismuth vanadate photocatalyst and preparation method thereof
CN114602516A (en) * 2022-04-13 2022-06-10 华北理工大学 Fe-doped BiOBr photo-Fenton catalytic material rich in oxygen vacancies and preparation method thereof
CN115155560A (en) * 2022-08-10 2022-10-11 中国科学院城市环境研究所 Rare earth modified vanadate catalyst, preparation method and application thereof
JP7502581B2 (en) 2020-03-13 2024-06-19 国立研究開発法人産業技術総合研究所 Photoelectrode, hydrogen peroxide production device, and method for producing hydrogen peroxide

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000016899A1 (en) * 1998-09-21 2000-03-30 The University Of Queensland Catalysts and process for reforming of hydrocarbons
CN103011288A (en) * 2012-12-24 2013-04-03 陕西科技大学 Preparation method for BiVO4 provided with visible light photocatalysis performance

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2000016899A1 (en) * 1998-09-21 2000-03-30 The University Of Queensland Catalysts and process for reforming of hydrocarbons
CN103011288A (en) * 2012-12-24 2013-04-03 陕西科技大学 Preparation method for BiVO4 provided with visible light photocatalysis performance

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
AIPING ZHANG等: ""Effects of europium doping on the photocatalytic behavior of BiVO4"", 《JOURNAL OF HAZARDOUS MATERIALS》, vol. 173, 25 August 2009 (2009-08-25) *
王其召: ""Bi1-xLnxVO4（Ln=La,Sm,Nd,Gd,Eu,Dy,Y）的制备、表征及光催化分解水性质"", 《中国博士学位论文全文数据库工程科技Ⅰ辑》, no. 4, 15 April 2013 (2013-04-15) *

Cited By (9)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN107159197A (en) * 2017-05-25 2017-09-15 上海交通大学 Mischcrystal photocatalyst with dodecahedron pattern and preparation method thereof
CN107469807A (en) * 2017-09-08 2017-12-15 郑州轻工业学院 A kind of monoclinic phase BiVO4：The high pressure method for preparing of Re catalysis materials
CN107469807B (en) * 2017-09-08 2019-10-18 郑州轻工业学院 A kind of monoclinic phase BiVO4: the high pressure method for preparing of Re catalysis material
JP7502581B2 (en) 2020-03-13 2024-06-19 国立研究開発法人産業技術総合研究所 Photoelectrode, hydrogen peroxide production device, and method for producing hydrogen peroxide
CN111992201A (en) * 2020-08-21 2020-11-27 重庆交通大学 One-step synthesis of BiVO by microwave hydrothermal method4/InVO4Method and application of photocatalyst
CN112058257A (en) * 2020-09-30 2020-12-11 攀枝花学院 Rare earth Tb doped bismuth vanadate photocatalyst and preparation method thereof
CN114602516A (en) * 2022-04-13 2022-06-10 华北理工大学 Fe-doped BiOBr photo-Fenton catalytic material rich in oxygen vacancies and preparation method thereof
CN115155560A (en) * 2022-08-10 2022-10-11 中国科学院城市环境研究所 Rare earth modified vanadate catalyst, preparation method and application thereof
CN115155560B (en) * 2022-08-10 2024-04-23 中国科学院城市环境研究所 Rare earth modified vanadate catalyst and preparation method and application thereof

Also Published As

Publication number Publication date
CN103433019B (en) 2015-08-12

Similar Documents

Publication Publication Date Title
CN103433019B (en) A kind of Sm doping BiVO 4photochemical catalyst and its preparation method and application
CN103263910B (en) A kind of pucherite-graphene composite photocatalyst and Synthesis and applications thereof
CN102616849B (en) Method for directly synthesizing M-phase vanadium dioxide nano particles by liquid phase method
CN102963930A (en) Method for preparing BiVO4 with photocatalytic performance under visible lights
CN102249305A (en) Method for synthesizing monoclinic phase and tetragonal phase mixed high-catalytic-activity bismuth vanadate powder by microwave hydrothermal process
CN102275988B (en) Microwave hydrothermal method for synthesizing monoclinic-phase bismuth vanadate photocatalyst powder
CN103240073B (en) Zn&lt;2+&gt;-doped BiVO4 visible-light-driven photocatalyst and preparation method thereof
CN102580721A (en) Method for preparing TiO2/BiVO4 composite photocatalyst by MH method
CN102343260A (en) Method for preparing boron-doped titanium dioxide crystal containing specific crystal plane
CN102553604A (en) Method for implementing Cu&lt;2+&gt; doping modification on BiVO4 photocatalyst by using microwave hydrothermal method
CN105195198A (en) Mpg-C3N4/Bi0.9Nd0.1VO4 composite photocatalyst and preparation method and application thereof
CN105289661A (en) Preparation method of bismuth oxychloride composite magnetic photocatalyst
Luévano-Hipólito et al. Synthesis, characterization, and photocatalytic properties of γ-Bi2MoO6 prepared by co-precipitation assisted with ultrasound irradiation
CN103433023B (en) A kind of Gd doping BiVO4photocatalyst and its preparation method and application
CN103464138B (en) Ytterbium doped bismuth vanadate visible light photocatalyst, and preparation method and application thereof
CN103464137B (en) Multi-morphologic Ho/BiVO4 composite photocatalyst, and preparation method and application thereof
CN103464136B (en) Y/BiVO4 composite photocatalyst, and preparation method and application thereof
CN102557133B (en) Method for preparing fishbone-shaped and firewood-shaped BiVO4 powder by microwave hydrothermal method
CN104549222A (en) Preparation method and application of visible-light-induced photocatalyst chromium chromate
CN105032394A (en) Pucherite visible-light-driven photocatalyst, preparing method and application
CN103433020B (en) A kind of Eu/BiVO 4photochemical catalyst and its preparation method and application
CN103447025B (en) Dy/BiVO4 photocatalyst as well as preparation method and application thereof
CN103433022B (en) A kind of visible-light response type Tb/BiVO4catalyst and its preparation method and application
Phuruangrat et al. Hydrothermal synthesis, characterization and photocatalytic properties of Au-doped Bi2MoO6 nanoplates
Torres-Martínez et al. Sol–gel synthesis of Sm 2 InTaO 7 and its photocatalytic activity on degradation of crystal violet dye and reduction of Cr (VI) ions

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
TR01 Transfer of patent right
TR01 Transfer of patent right

Effective date of registration: 20201224

Address after: 518000 No.6 Qinglong Road, Qinglong Road, Qinghua community, Longhua street, Longhua District, Shenzhen City, Guangdong Province

Patentee after: Shenzhen Pengbo Information Technology Co.,Ltd.

Address before: No. 1, Weiyang District university garden, Xi'an, Shaanxi Province, Shaanxi

Patentee before: SHAANXI University OF SCIENCE & TECHNOLOGY

Effective date of registration: 20201224

Address after: 224000 Qingyang Road (within Qingdun Office), Nanyang Town, Tinghu District, Yancheng City, Jiangsu Province (8)

Patentee after: Yancheng Qinglong Jinbang water Co.,Ltd.

Address before: 518000 No.6 Qinglong Road, Qinglong Road, Qinghua community, Longhua street, Longhua District, Shenzhen City, Guangdong Province

Patentee before: Shenzhen Pengbo Information Technology Co.,Ltd.

CI03 Correction of invention patent
CI03 Correction of invention patent

Correction item: Patentee|Address

Correct: Yancheng Qingdun Jinbang Water Co., Ltd.|224000 Qingyang Road, Nanyang Town, Tinghu District, Yancheng City, Jiangsu Province (in Qingdun Office) (8)

False: Yancheng Qingyi Jinbang Water Affairs Co., Ltd.|224000 Qingyang Road, Nanyang Town, Tinghu District, Yancheng City, Jiangsu Province (in Qingdun Office) (8)

Number: 02-01

Volume: 37