CN102963930A - Method for preparing BiVO4 with photocatalytic performance under visible lights - Google Patents

Method for preparing BiVO4 with photocatalytic performance under visible lights Download PDF

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CN102963930A
CN102963930A CN2012104448747A CN201210444874A CN102963930A CN 102963930 A CN102963930 A CN 102963930A CN 2012104448747 A CN2012104448747 A CN 2012104448747A CN 201210444874 A CN201210444874 A CN 201210444874A CN 102963930 A CN102963930 A CN 102963930A
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solution
bivo
deionized water
under visible
preparation
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谈国强
张丽丽
魏莎莎
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Shaanxi University of Science and Technology
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Shaanxi University of Science and Technology
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Abstract

The invention discloses a method for preparing BiVO4 with photocatalytic performance under visible lights. The method comprises the steps that a bismuth-containing compound and a vanadium-containing compound are respectively dissolved in deionized water at first to be mixed, NaOH solution is then added so as to form precursor solution, the precursor solution is put in a polytetrafluoroethylene reactor to generate yellow precipitate, deionized water and absolute ethyl alcohol are finally used to wash, and drying is carried out to obtain BiVO4 powder. Concentrated nitric acid is not used as an inhibitor to inhibit the hydrolysis of Bi(NO3)3.5H2O when the precursor solution is prepared, but Bi(NO3)3.5H2O is directly dissolved in deionized water, so that the method has the characteristics of simplicity in operation, moderate conditions and short reaction time. The BiVO4 powders with different crystalline phases can be selectively prepared through regulating the pH value of the precursor solution, and the prepared powder has certain photocatalytic performance under visible lights.

Description

The BiVO that has photocatalysis performance under a kind of visible light 4The preparation method
Technical field
The present invention relates to a kind of BiVO that under visible light, has photocatalysis performance 4The preparation method, belong to field of functional materials.
Background technology
In recent years, utilize the research of organic pollutant in Photocatalitic Technique of Semiconductor degrading waste water and the air active, TiO 2Nontoxic with it, high chemical stability and oxidisability etc. becomes desirable photocatalyst.But TiO 2Only the UV-light that accounts for sun power 4% is had response, this has limited its application greatly.In order to utilize better the visible light that accounts for sunlight 43%, designing and developing effective visible-light photocatalyst has important science and application value.Therefore, the research worker has designed many complex metal oxidess as visible light-responded novel photocatalyst, such as BiWO 6, InVO 4, AgAlO 2, CaIn 2O 4Deng.BiVO 4Be exactly a kind of in these complex metal oxides photocatalysts, it has obtained some at aspects such as photodissociation water and degraded mineralising organic pollutants and has used, but its photocatalysis performance is subjected to the impact of its crystal formation.BiVO 4Mainly contain three kinds of crystal formations: cubic Zircon cut, monocline scheelite type structure and cubic scheelite type structure.Monocline scheelite type structure BiVO 4Energy gap narrow, under visible light, have good catalytic activity.BiVO 4The preparation method solid phase method, sol-gel method, chemical coprecipitation, hydrothermal method, liquid-phase precipitation method, microemulsion method and microwave-hydrothermal method etc. are arranged, all use concentrated nitric acid as Bi (NO in the great majority experiments precursor solution preparation process 3) 35H 2The solvent of O suppresses Bi (NO 3) 35H 2The hydrolysis of O.
Summary of the invention
The object of the present invention is to provide a kind of BiVO that under visible light, has photocatalysis performance 4The preparation method, its technical process is simple, mild condition, the reaction times is short, even particle size distribution and lower-cost.Can avoid using concentrated nitric acid as inhibitor according to processing method of the present invention, and can optionally make the BiVO of monoclinic phase, Tetragonal 4Powder, the BiVO that makes 4Powder has certain photocatalysis performance under visible light.
In order to achieve the above object, the present invention adopts following technical scheme:
A kind of BiVO that under visible light, has photocatalysis performance 4The preparation method, may further comprise the steps: bismuth salt is dissolved in the deionized water, and stirring forms the bismuth salts solution; Vanadic salts is dissolved in 100 ℃ of deionized waters, and heated and stirred evenly forms vanadic salts solution; Bismuth salts solution and vanadic salts solution are mixed according to the mole proportioning of Bi:V=1:1, after stirring, add NaOH solution, regulating pH is 1.33 ~ 9.5, and magnetic agitation forms precursor solution; Precursor solution is put into the tetrafluoroethylene reactor, 200 ℃ of microwave hydrothermal temperature of reaction, insulation reaction 40min; After reaction was finished, the yellow mercury oxide in the reactor was taken out in cooling, uses deionized water and absolute ethanol washing 3 times, at 70 ℃ of lower dry 12h, had made BiVO at last 4Powder.
The present invention further improves and is: described bismuth salt and vanadic salts are respectively Bi (NO 3) 35H 2O and NH 4VO 3
The present invention further improves and is: described NH 4VO 3The homo(io)thermism of heated and stirred at 40 ℃ ~ 45 ℃ until ammonium metavanadate solution is brown color.
The present invention further improves and is: the concentration of described NaOH solution is 1 ~ 6.5mol/L.
The present invention further improves and is: the packing ratio of microwave hydrothermal reaction is 50 ~ 60%.
A kind of BiVO that under visible light, has photocatalysis performance 4The preparation method, may further comprise the steps: step 1: with 0.01mol Bi (NO 3) 35H 2O is dissolved in the deionized water, under the room temperature, in the magnetic stirring apparatus formation solution A that stirs, with 0.01mol NH 4VO 3Be dissolved in 100 ℃ of deionized waters, heated and stirred evenly forms solution B on magnetic stirring apparatus, and the homo(io)thermism of heated and stirred is at 40 ℃ ~ 45 ℃; Step 2: after the solution A and solution B mixing with step 1 preparation, stir at magnetic stirring apparatus, then add NaOH solution, regulating the pH value is 1.33, stirs 30min at magnetic stirring apparatus, makes precursor solution; Step 3: the precursor solution that step 2 makes is put into the tetrafluoroethylene reactor, and packing ratio is 50%, then reactor is placed microwave assisted hydrothermal synthesis apparatus, and setting the microwave hydrothermal temperature of reaction is 200 ℃, and soaking time is 40min; Step 4: after question response was finished, the yellow mercury oxide in the reactor was taken out in cooling, to neutrality, uses absolute ethanol washing 3 times with deionized water wash again, at 70 ℃ of lower freeze-day with constant temperature 12h, gets BiVO at last 4Powder.
Compared with prior art, the present invention has the following advantages: the present invention is dissolved in bismuth-containing compound in the deionized water, stir 20 ~ 30min, vanadium-containing compound is dissolved in 100 ℃ the deionized water, heated and stirred 20 ~ 35min, bismuth salt and vanadic salts are mixed according to the mole proportioning of Bi:V=1:1, stir 10 ~ 20min, add the NaOH solution of different concns, magnetic agitation 30min forms precursor solution, precursor solution is put into the tetrafluoroethylene reactor, 200 ℃ of microwave hydrothermal temperature of reaction, soaking time 40min, the yellow mercury oxide that generates is taken out, with deionized water and absolute ethanol washing 3 times, at 70 ℃ of lower dry 12h, made BiVO 4Powder.The present invention suppresses Bi (NO without concentrated nitric acid as inhibitor when the preparation precursor solution 3) 35H 2The hydrolysis of O, but directly with Bi (NO 3) 35H 2O is dissolved in the deionized water, have simple to operate, mild condition, the characteristics that the reaction times is short.And the present invention can optionally make the BiVO of monoclinic phase and Tetragonal by the pH value of regulating precursor solution 4Powder, the powder that makes have certain photocatalysis performance under visible light.
Description of drawings
Fig. 1 is the BiVO of monoclinic phase of the present invention 4The XRD figure of powder (embodiment 1:pH=1.33);
Fig. 2 is the BiVO of monoclinic phase of the present invention 4The ultraviolet-visible spectrum of powder rhodamine B degradation solution under visible light is graphic representation (embodiment 1:pH=1.33) over time;
Fig. 3 is the BiVO of Tetragonal of the present invention 4The XRD figure of powder (embodiment 2:pH=2.55).
Embodiment
The present invention is dissolved in bismuth-containing compound in the deionized water first, stir 30 ~ 40min, vanadium-containing compound is dissolved in 100 ℃ the deionized water, heated and stirred 30 ~ 40min, bismuth salt and vanadic salts are mixed according to the mole proportioning of Bi:V=1:1, stir 30min, add the NaOH solution of different concns, magnetic agitation 30min forms precursor solution, and precursor solution is put into the tetrafluoroethylene reactor, 200 ℃ of microwave hydrothermal temperature of reaction, soaking time 40min takes out the yellow mercury oxide that generates, and uses deionized water and absolute ethanol washing 3 times, at 70 ℃ of lower dry 12h, made BiVO 4Powder.
The present invention adopts deionized water dissolving Bi (NO 3) 35H 2O, reaction equation is:
Bi(NO 3) 3+H 2O=2HNO 3+BiONO 3
BiONO 3+VO 3 -=BiVO 4+NO 3 -
With dissolve Bi (NO with concentrated nitric acid 3) 35H 2O compares, and the method is simple to operate, and reaction conditions is gentle, and conservation be the more important thing is the BiVO that utilizes present method can optionally prepare by regulating the pH value monoclinic phase and Tetragonal 4Powder, and the powder that makes has certain photocatalysis performance under visible light.After ionized water was replaced concentrated nitric acid, deionized water can make Bi (NO 3) 35H 2The O hydrolysis.
The present invention is described further below in conjunction with the preferred embodiment of the invention, and raw material is analytical pure.
Embodiment 1:
Step 1: with 0.01mol Bi (NO 3) 35H 2O is dissolved in the deionized water, under the room temperature, stirs 30min at magnetic stirring apparatus, with 0.01mol NH 4VO 3Be dissolved in 100 ℃ the deionized water, heated and stirred 30min on magnetic stirring apparatus, the heated and stirred homo(io)thermism is at 45 ℃.
Step 2: two kinds of solution of step 1 preparation are mixed, stir 20min at magnetic stirring apparatus, then adding 5ml concentration is the NaOH solution of 1mol/L, and measuring the pH value is 1.33, stirs 30min at magnetic stirring apparatus, makes precursor solution;
Step 3: precursor liquid is put into the tetrafluoroethylene reactor, and packing ratio is 50%, then reactor is placed microwave assisted hydrothermal synthesis apparatus, and setting the microwave hydrothermal temperature of reaction is 200 ℃, and soaking time is 40min;
Step 4: after question response was finished, the yellow mercury oxide in the reactor was taken out in cooling, to neutrality, uses absolute ethanol washing 3 times with deionized water wash again, at 70 ℃ of lower freeze-day with constant temperature 12h, obtains BiVO at last 4Powder.
Phase with the XRD determining powder forms, and as can be seen from Figure 1 adopts microwave-hydrothermal method not add the BiVO that inhibitor can be prepared monoclinic phase 4Powder.Fig. 2 is the monoclinic phase BiVO that the present invention makes under pH=1.33 4The ultraviolet-visible spectrum of powder rhodamine B degradation solution under visible light is graphic representation over time.As can be seen from the figure do not add inhibitor (concentrated nitric acid) and can prepare the BiVO that under visible light, has certain photocatalysis performance yet 4Powder.
Embodiment 2:
Step 1: with 0.01mol Bi (NO 3) 35H 2O is dissolved in the deionized water, under the room temperature, stirs 20min at magnetic stirring apparatus, with 0.01mol NH 4VO 3Be dissolved in 100 ℃ the deionized water, heated and stirred 20min on magnetic stirring apparatus, the heated and stirred homo(io)thermism is at 40 ℃.
Step 2: two kinds of solution of step 1 preparation are mixed, stir 20min at magnetic stirring apparatus, then adding 5ml concentration is the NaOH solution of 4mol/L, and measuring the pH value is 2.55, stirs 30min at magnetic stirring apparatus, makes precursor solution;
Step 3: precursor liquid is put into the tetrafluoroethylene reactor, and packing ratio is 60%, then reactor is placed microwave assisted hydrothermal synthesis apparatus, and setting the microwave hydrothermal temperature of reaction is 200 ℃, and soaking time is 40min;
Step 4: after question response was finished, the yellow mercury oxide in the reactor was taken out in cooling, to neutrality, uses absolute ethanol washing 3 times with deionized water wash again, at 70 ℃ of lower freeze-day with constant temperature 12h, obtains BiVO at last 4Powder.
Phase with the XRD determining powder forms, and as can be seen from Figure 3 adopts microwave-hydrothermal method not add the BiVO that inhibitor can be prepared Tetragonal 4Powder.
Embodiment 3:
Step 1: with 0.01mol Bi (NO 3) 35H 2O is dissolved in the deionized water, under the room temperature, stirs 30min at magnetic stirring apparatus, with 0.01mol NH 4VO 3Be dissolved in 100 ℃ of deionized waters, heated and stirred 35min on magnetic stirring apparatus, the heated and stirred homo(io)thermism is at 40 ℃.
Step 2: two kinds of solution of step 1 preparation are mixed, stir 10min at magnetic stirring apparatus, then adding 5ml concentration is the NaOH solution of 6mol/L, and measuring the pH value is 9.18, stirs 30min at magnetic stirring apparatus, makes precursor solution;
Step 3: precursor liquid is put into the tetrafluoroethylene reactor, and packing ratio is 50%, then reactor is placed microwave assisted hydrothermal synthesis apparatus, and setting the microwave hydrothermal temperature of reaction is 200 ℃, and soaking time is 40min;
Step 4: after question response was finished, the yellow mercury oxide in the reactor was taken out in cooling, to neutrality, uses absolute ethanol washing 3 times with deionized water wash again, at 70 ℃ of lower freeze-day with constant temperature 12h, obtains BiVO at last 4Powder.
This powder is the BiVO of monoclinic phase through the XRD test 4Powder.
Embodiment 4:
Step 1: with 0.01mol Bi (NO 3) 35H 2O is dissolved in the deionized water, under the room temperature, stirs 30min at magnetic stirring apparatus, with 0.01mol NH 4VO 3Be dissolved in 100 ℃ of deionized waters, heated and stirred 35min on magnetic stirring apparatus, the heated and stirred homo(io)thermism is at 40 ℃.
Step 2: two kinds of solution of step 1 preparation are mixed, stir 10min at magnetic stirring apparatus, then adding 5ml concentration is the NaOH solution of 6.5mol/L, and measuring the pH value is 9.50, stirs 30min at magnetic stirring apparatus, makes precursor solution;
Step 3: precursor liquid is put into the tetrafluoroethylene reactor, and packing ratio is 60%, then reactor is placed microwave assisted hydrothermal synthesis apparatus, and setting the microwave hydrothermal temperature of reaction is 200 ℃, and soaking time is 40min;
Step 4: after question response was finished, the yellow mercury oxide in the reactor was taken out in cooling, to neutrality, uses absolute ethanol washing 3 times with deionized water wash again, at 70 ℃ of lower freeze-day with constant temperature 12h, obtains BiVO at last 4Powder.
This powder is the BiVO of monoclinic phase through the XRD test 4Powder.
The above only is one embodiment of the present invention, it or 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 sheets of the present invention is claim of the present invention and contains.

Claims (6)

1. BiVO who under visible light, has photocatalysis performance 4The preparation method, it is characterized in that, may further comprise the steps:
Bismuth salt is dissolved in the deionized water, and stirring forms the bismuth salts solution; Vanadic salts is dissolved in 100 ℃ of deionized waters, and heated and stirred evenly forms vanadic salts solution; With bismuth salts solution and vanadic salts solution according to Bi:V=1: 1 mole proportioning is mixed, and after stirring, adds NaOH solution, and regulating pH is 1.33 ~ 9.5, and magnetic agitation forms precursor solution; Precursor solution is put into the tetrafluoroethylene reactor, 200 ℃ of microwave hydrothermal temperature of reaction, insulation reaction 40min; After reaction was finished, the yellow mercury oxide in the reactor was taken out in cooling, uses deionized water and absolute ethanol washing 3 times, at 70 ℃ of lower dry 12h, had made BiVO at last 4Powder.
2. a kind of BiVO that under visible light, has photocatalysis performance as claimed in claim 1 4The preparation method, it is characterized in that described bismuth salt and vanadic salts are respectively Bi (NO 3) 35H 2O and NH 4VO 3
3. a kind of BiVO that under visible light, has photocatalysis performance as claimed in claim 1 4The preparation method, it is characterized in that described NH 4VO 3The homo(io)thermism of heated and stirred at 40 ℃ ~ 45 ℃ until ammonium metavanadate solution is brown color.
4. a kind of BiVO that under visible light, has photocatalysis performance as claimed in claim 1 4The preparation method, it is characterized in that the concentration of described NaOH solution is 1 ~ 6.5mol/L.
5. a kind of BiVO that under visible light, has photocatalysis performance as claimed in claim 1 4The preparation method, it is characterized in that the packing ratio of microwave hydrothermal reaction is 50 ~ 60%.
6. BiVO who under visible light, has photocatalysis performance 4The preparation method, it is characterized in that, may further comprise the steps:
Step 1: with 0.01mol Bi (NO 3) 35H 2O is dissolved in the deionized water, under the room temperature, in the magnetic stirring apparatus formation solution A that stirs, with 0.01mol NH 4VO 3Be dissolved in 100 ℃ of deionized waters, heated and stirred evenly forms solution B on magnetic stirring apparatus, and the homo(io)thermism of heated and stirred is at 40 ℃ ~ 45 ℃;
Step 2: after the solution A and solution B mixing with step 1 preparation, stir at magnetic stirring apparatus, then add NaOH solution, regulating the pH value is 1.33, stirs 30min at magnetic stirring apparatus, makes precursor solution;
Step 3: the precursor solution that step 2 makes is put into the tetrafluoroethylene reactor, and packing ratio is 50%, then reactor is placed microwave assisted hydrothermal synthesis apparatus, and setting the microwave hydrothermal temperature of reaction is 200 ℃, and soaking time is 40min;
Step 4: after question response was finished, the yellow mercury oxide in the reactor was taken out in cooling, to neutrality, uses absolute ethanol washing 3 times with deionized water wash again, at 70 ℃ of lower freeze-day with constant temperature 12h, gets BiVO at last 4Powder.
CN2012104448747A 2012-11-09 2012-11-09 Method for preparing BiVO4 with photocatalytic performance under visible lights Pending CN102963930A (en)

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CN105063740A (en) * 2015-07-30 2015-11-18 陕西科技大学 Quadrangular frustum lamellar Bi2O3 nano-single crystal and preparation method thereof
CN109433185A (en) * 2018-12-10 2019-03-08 北华大学 One step hydro thermal method prepares vanadic acid indium/isomerism knot composite bismuth vanadium photocatalyst
JP2020111476A (en) * 2019-01-09 2020-07-27 学校法人 龍谷大学 Method for producing visible light-responsive bismuth vanadate
CN111790372A (en) * 2020-07-29 2020-10-20 上海第二工业大学 Visible light response peanut-shaped bismuth vanadate and preparation method thereof
CN113896243A (en) * 2021-09-29 2022-01-07 陕西科技大学 BiVO4Nanosheet and preparation method and application thereof
CN114031114A (en) * 2021-11-12 2022-02-11 成都先进金属材料产业技术研究院股份有限公司 Method for preparing bismuth vanadate powder by using failure electrolyte of vanadium battery
CN114632508A (en) * 2022-02-15 2022-06-17 江苏大学 Mulberry-shaped BiVO4Preparation method of micron rod-shaped material and application of micron rod-shaped material in photocatalytic degradation of pollutants
CN115536065A (en) * 2022-09-14 2022-12-30 哈尔滨理工大学 Preparation method of bismuth vanadate

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Cited By (12)

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Publication number Priority date Publication date Assignee Title
CN103240107A (en) * 2013-04-27 2013-08-14 天津大学 Silver phosphate-bismuth vanadate multiplex photocatalyst and preparation method thereof
CN105063740A (en) * 2015-07-30 2015-11-18 陕西科技大学 Quadrangular frustum lamellar Bi2O3 nano-single crystal and preparation method thereof
CN105063740B (en) * 2015-07-30 2017-10-24 陕西科技大学 A kind of truncated rectangular pyramids flake Bi2O3Nano crystal and preparation method thereof
CN109433185A (en) * 2018-12-10 2019-03-08 北华大学 One step hydro thermal method prepares vanadic acid indium/isomerism knot composite bismuth vanadium photocatalyst
JP2020111476A (en) * 2019-01-09 2020-07-27 学校法人 龍谷大学 Method for producing visible light-responsive bismuth vanadate
JP7292703B2 (en) 2019-01-09 2023-06-19 学校法人 龍谷大学 Method for producing visible-light-responsive bismuth vanadate
CN111790372A (en) * 2020-07-29 2020-10-20 上海第二工业大学 Visible light response peanut-shaped bismuth vanadate and preparation method thereof
CN113896243A (en) * 2021-09-29 2022-01-07 陕西科技大学 BiVO4Nanosheet and preparation method and application thereof
CN113896243B (en) * 2021-09-29 2023-08-18 陕西科技大学 BiVO (binary organic acid) 4 Nanosheets, preparation method and application thereof
CN114031114A (en) * 2021-11-12 2022-02-11 成都先进金属材料产业技术研究院股份有限公司 Method for preparing bismuth vanadate powder by using failure electrolyte of vanadium battery
CN114632508A (en) * 2022-02-15 2022-06-17 江苏大学 Mulberry-shaped BiVO4Preparation method of micron rod-shaped material and application of micron rod-shaped material in photocatalytic degradation of pollutants
CN115536065A (en) * 2022-09-14 2022-12-30 哈尔滨理工大学 Preparation method of bismuth vanadate

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Application publication date: 20130313