CN102309962B - Preparation method of data cake-shaped Bi2W0.5Mo0.5O6 nanometer powder - Google Patents

Preparation method of data cake-shaped Bi2W0.5Mo0.5O6 nanometer powder Download PDF

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CN102309962B
CN102309962B CN 201110187157 CN201110187157A CN102309962B CN 102309962 B CN102309962 B CN 102309962B CN 201110187157 CN201110187157 CN 201110187157 CN 201110187157 A CN201110187157 A CN 201110187157A CN 102309962 B CN102309962 B CN 102309962B
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powder
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jujube cake
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CN102309962A (en
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王秀峰
许亚琴
江红涛
鲁俊雀
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Shaanxi University of Science and Technology
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Abstract

The invention which relates to a preparation of a nanometer powder material discloses a preparation method of data cake-shaped Bi2W0.5Mo0.5O6 nanometer powder. The preparation method comprises the following steps: 1, dissolving Bi(NO)3.5H2O in a citric acid solution with the concentration of 0.01-0.05mol/L, adding Na2WO4.2H2O and NaHCO3 in a dropwise manner, and carrying out ultrasonic cleaning at a low temperature to form an uniform mixed liquid; 2, carrying out microwave heating on the mixed liquid for 1.5-3h at 200DEG C, cooling, and cleaning to obtain a sample; and 3, drying the sample in a vacuum drying box to obtain the data cake-shaped Bi2W0.5Mo0.5O6 nanometer powder. The preparation method which allows data cake-shaped Bi2WO6 microballoons with uniform morphology to be prepared without adding a surfactant has the advantages of simple preparation technology and short period, and the preparative data cake-shaped Bi2W0.5Mo0.5O6 can degrade rhodamine B under visible light.

Description

A kind of jujube cake shape Bi 2W 0.5Mo 0.5O 6The preparation method of nano-powder
Technical field
The present invention relates to the preparation of nano-powder material, be specifically related to a kind of jujube cake shape Bi 2W 0.5Mo 0.5O 6The preparation method of nano-powder.
Background technology
Bismuth tungstate (Bi 2WO 6) be a kind of perofskite type oxide that typically has stratiform, the perofskite type oxide general formula is Bi 2A N-1BnO 3n+3(A=Ca, Sr, Ba, Pb, Na, K; B=Ti, Nb, Ta, Mo, W, Fe; N depends on (A N-1B nO 3n+3) 2-Number), intersect by Ca-Ti ore type unit and fluorite type unit on the structure and constitute.Bi 2WO 6Be by O 2-And Bi 2+It is cube tightly packed that mutual group becomes, W 6+The ion filling in 1/4 octahedral interstices, in addition because Bi 2WO 6Good physics, chemical property are arranged itself, have good photocatalysis performance, and can be used as solar energy materials, thereby enjoy people to favor.Bi 2WO 6Performance with use with its pattern closely related.Bi 2WO 6The control of pattern still has very big development space, and therefore the preparation method of new controllable appearance causes numerous scholars' extensive concern.At present synthetic Bi 2WO 6Method mainly contain solid state process, hydro-thermal method, ultrasonic method etc., and synthesized the nanostructured of different-shape, for example nanometer sheet, microballoon, tire-helical form, flower-shaped, nano particle.But microwave-hydrothermal method is compared with it, and microwave-hydrothermal method has the not available advantage of additive method.
Because microwave (MW) be frequency greatly about 300MHz～300GHz, i.e. the electromagnetic wave of wavelength in 1m～1mm scope.Microwave technology is because its reaction speed is fast, the efficient height, saves cost, pollution-free, advantage such as save time, and has been widely used in the preparation of sample, organic synthesis, and water purifies, every field such as inducing catalysis.Microwave has unique advantage as the thermal source of chemical reaction: at first the penetration power of microwave is extremely strong, to sample is inside and outside heating together, thereby object is evenly heated up fast, and have only those materials that under the extra electric field effect, can produce polarization just can absorb microwave and heat up, make heating using microwave have selectivity and controllability; Interaction between microwave and the material also has unique " non-thermal effect ", thereby has reduced reaction temperature.Process for solid-phase microwave synthesis have reaction fast, need not post processing, applied range, productive rate advantages of higher.
In order further to improve Bi 2WO 6Photocatalysis performance, this paper has studied Bi 2Mo 0.5W 0.5O 6The preparation of solid solution is to reduce Bi 2WO 6Energy gap, improve Bi 2WO 6Photocatalysis performance.In this experiment, under the situation of not adding surfactant, utilize microwave-hydrothermal method to prepare to have the jujube cake shape Bi of uniform morphology 2WO 6Microballoon, and carry out sign and Analysis on Mechanism thereof such as pattern and structure, simultaneously also to jujube cake shape Bi 2WO 6Microballoon is studied by the rhodamine B of degrading under visible light radiation.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of jujube cake shape Bi 2W 0.5Mo 0.5O 6The preparation method of nano-powder can prepare the jujube cake shape Bi with uniform morphology need not to add under the situation of surfactant 2WO 6Microballoon, and preparation technology is simple, and the cycle is short, the jujube cake shape Bi that makes 2W 0.5Mo 0.5O 6The rhodamine B of can under visible light, degrading.
To achieve these goals, the technical solution used in the present invention is:
A kind of jujube cake shape Bi 2W 0.5Mo 0.5O 6The preparation method of nano-powder may further comprise the steps:
The first step is with the Bi (NO) of 1～4mmol 35H 2O is dissolved in the citric acid solution that 50～100mL concentration is 0.01～0.05mol/L, gets bismuth-containing solution;
Second step is with the Na of 0.25～1mmol 2WO 42H 2(the NH of O, 0.25～1mmol 4) 6Mo 7O 24H 2The NaHCO of O and 1～4mmol 3Be added drop-wise in the above-mentioned bismuth-containing solution, put into ultrasonic instrument behind the stirring 10min,, form uniform mixed liquor in 20～30 ℃ of following ultrasonic cleaning 10～20min;
The 3rd step, with the mixed liquor that obtains in reactor at 200 ℃ of microwave hydrothermal 1.5～3h, be cooled to normal temperature, clean, obtain sample;
In the 4th step, sample 60～80 ℃ of drying 20～25h in vacuum drying chamber with obtaining obtain jujube cake shape Bi 2W 0.5Mo 0.5O 6Nano-powder.
Wherein, the dropping time of NaHCO3 is 1～20min in described second step, and the cleaning in described the 3rd step is meant respectively washs cooled product 3 times with deionized water and absolute ethyl alcohol, and microwave hydrothermal utilizes the microwave hydrothermal instrument to finish.
Compared with prior art, advantage of the present invention is:
(1) method is easy, easy operating, reaction condition gentleness;
(2) manufacturing cycle is short, can make sample in 1～3 day;
(3) Bi that makes 2W 0.5Mo 0.5O 6The rhodamine B of can under visible light, degrading.
Description of drawings
Fig. 1 is the jujube cake shape Bi of the embodiment of the invention one preparation 2W 0.5Mo 0.5O 6The XRD figure of nano-powder.
Fig. 2 is the jujube cake shape Bi of the embodiment of the invention one preparation 2W 0.5Mo 0.5O 6The SEM figure of nano-powder, 5000 times of multiplication factors.
Fig. 3 is the jujube cake shape Bi of the embodiment of the invention one preparation 2W 0.5Mo 0.5O 6The SEM figure of nano-powder, 30000 times of multiplication factors.
The specific embodiment
Below in conjunction with drawings and Examples the present invention is described in further details.
Embodiment one
A kind of jujube cake shape Bi 2W 0.5Mo 0.5O 6The preparation method of nano-powder may further comprise the steps:
The first step is with the Bi (NO) of 1mmol 35H 2O is dissolved in the citric acid solution that 60mL concentration is 0.017mol/L, gets bismuth-containing solution;
Second step is with the Na of 0.25mmol 2WO 42H 2(the NH of O, 0.25mmol 4) 6Mo 7O 24H 2The NaHCO of O and 1mmol 3Be added drop-wise in the above-mentioned bismuth-containing solution, put into ultrasonic instrument behind the stirring 10min,, form uniform mixed liquor in 20 ℃ of following ultrasonic cleaning 10min;
The 3rd step, with the mixed liquor that obtains in reactor at 200 ℃ of microwave hydrothermal 1.5h, be cooled to normal temperature, clean, obtain sample;
In the 4th step, the sample 60 ℃ of dry 20h in vacuum drying chamber with obtaining obtain jujube cake shape Bi 2W 0.5Mo 0.5O 6Nano-powder.
As shown in Figure 1, the jujube cake shape Bi for preparing for present embodiment 2W 0.5Mo 0.5O 6The XRD figure of nano-powder, its purity is higher as can be seen.
As shown in Figure 2, the jujube cake shape Bi for preparing for present embodiment 2W 0.5Mo 0.5O 6The SEM figure of nano-powder, 5000 times of multiplication factors;
As shown in Figure 3, the jujube cake shape Bi for preparing for present embodiment 2W 0.5Mo 0.5O 6The SEM figure of nano-powder, 30000 times of multiplication factors.
The Bi of present embodiment preparation as can be seen 2W 0.5Mo 0.5O 6Nano-powder is tangible jujube cake shape.
Embodiment two
A kind of jujube cake shape Bi 2W 0.5Mo 0.5O 6The preparation method of nano-powder may further comprise the steps:
The first step is with 4mmol Bi (NO) 35H 2O is dissolved in the citric acid solution that 100mL concentration is 0.05mol/L, gets bismuth-containing solution;
Second step is with the Na of 1mmol 2WO 42H 2(the NH of O, 1mmol 4) 6Mo 7O 24H 2The NaHCO of O and 4mmol 3Be added drop-wise in the above-mentioned bismuth-containing solution, put into ultrasonic instrument behind the stirring 10min,, form uniform mixed liquor in 30 ℃ of following ultrasonic cleaning 20min;
The 3rd step, with the mixed liquor that obtains in reactor at 200 ℃ of microwave hydrothermal 3h, be cooled to normal temperature, clean, obtain sample;
In the 4th step, the sample 62 ℃ of dry 25h in vacuum drying chamber with obtaining obtain jujube cake shape Bi 2W 0.5Mo 0.5O 6Nano-powder.
Embodiment three
A kind of jujube cake shape Bi 2W 0.5Mo 0.5O 6The preparation method of nano-powder may further comprise the steps:
The first step is with the Bi (NO) of 1.5mmol 35H 2O is dissolved in the citric acid solution that 60mL concentration is 0.025mol/L, gets bismuth-containing solution;
Second step is with the Na of 0.4mmol 2WO 42H 2(the NH of O, 0.4mmol 4) 6Mo 7O 24H 2The NaHCO of O and 1.5mmol 3Be added drop-wise in the above-mentioned bismuth-containing solution, put into ultrasonic instrument behind the stirring 10min,, form uniform mixed liquor in 25 ℃ of following ultrasonic cleaning 15min;
The 3rd step, with the mixed liquor that obtains in reactor at 200 ℃ of microwave hydrothermal 1.5h, be cooled to normal temperature, clean, obtain sample;
In the 4th step, the sample 80 ℃ of dry 20h in vacuum drying chamber with obtaining obtain jujube cake shape Bi 2W 0.5Mo 0.5O 6Nano-powder.
Embodiment four
A kind of jujube cake shape Bi 2W 0.5Mo 0.5O 6The preparation method of nano-powder may further comprise the steps:
The first step is with the Bi (NO) of 3mmol 35H 2O is dissolved in the citric acid solution that 85mL concentration is 0.02mol/L, gets bismuth-containing solution;
Second step is with the Na of 0.75mmol 2WO 42H 2(the NH of O, 0.75mmol 4) 6Mo 7O 24H 2The NaHCO of O and 3mmol 3Be added drop-wise in the above-mentioned bismuth-containing solution, put into ultrasonic instrument behind the stirring 10min,, form uniform mixed liquor in 25 ℃ of following ultrasonic cleaning 15min;
The 3rd step, with the mixed liquor that obtains in reactor at 200 ℃ of microwave hydrothermal 2h, be cooled to normal temperature, clean, obtain sample;
In the 4th step, the sample 70 ℃ of dry 20h in vacuum drying chamber with obtaining obtain jujube cake shape Bi 2W 0.5Mo 0.5O 6Nano-powder.
More than among each embodiment, microwave hydrothermal is all finished by the microwave hydrothermal instrument, the present application of microwave hydrothermal instrument is very extensive.Simultaneously, in order to obtain better preparation effect, in the 3rd step separately, cooled product is respectively washed 3 times with deionized water and absolute ethyl alcohol.

Claims (8)

1. jujube cake shape Bi 2W 0.5Mo 0.5O 6The preparation method of nano-powder is characterized in that, may further comprise the steps:
The first step is with the Bi(NO of 1～4mmol 3) 35H 2O is dissolved in the citric acid solution that 50～100mL concentration is 0.01～0.05mol/L, gets bismuth-containing solution;
Second step is with the Na of 0.25～1mmol 2WO 42H 2(the NH of O, 0.25～1mmol 4) 6Mo 7O 24H 2The NaHCO of O and 1～4mmol 3Be added drop-wise in the above-mentioned bismuth-containing solution, put into ultrasonic instrument behind the stirring 10min,, form uniform mixed liquor in 20～30 ℃ of following ultrasonic cleaning 10～20min;
The 3rd step, with the mixed liquor that obtains in reactor at 200 ℃ of microwave hydrothermal 1.5～3h, be cooled to normal temperature, clean, obtain sample;
In the 4th step, sample 60～80 ℃ of drying 20～25h in vacuum drying chamber with obtaining obtain jujube cake shape Bi 2W 0.5Mo 0.5O 6Nano-powder.
2. jujube cake shape Bi 2W 0.5Mo 0.5O 6The preparation method of nano-powder is characterized in that, may further comprise the steps:
The first step is with the Bi(NO of 1mmol 3) 35H 2O is dissolved in the citric acid solution that 60mL concentration is 0.017mol/L, gets bismuth-containing solution;
Second step is with the Na of 0.25mmol 2WO 42H 2(the NH of O, 0.25mmol 4) 6Mo 7O 24H 2The NaHCO of O and 1mmol 3Be added drop-wise in the above-mentioned bismuth-containing solution, put into ultrasonic instrument behind the stirring 10min,, form uniform mixed liquor in 20 ℃ of following ultrasonic cleaning 10min;
The 3rd step, with the mixed liquor that obtains in reactor at 200 ℃ of microwave hydrothermal 1.5h, be cooled to normal temperature, clean, obtain sample;
In the 4th step, the sample 60 ℃ of dry 20h in vacuum drying chamber with obtaining obtain jujube cake shape Bi 2W 0.5Mo 0.5O 6Nano-powder.
3. jujube cake shape Bi 2W 0.5Mo 0.5O 6The preparation method of nano-powder is characterized in that, may further comprise the steps:
The first step is with 4mmol Bi(NO 3) 35H 2O is dissolved in the citric acid solution that 100mL concentration is 0.05mol/L, gets bismuth-containing solution;
Second step is with the Na of 1mmol 2WO 42H 2(the NH of O, 1mmol 4) 6Mo 7O 24H 2The NaHCO of O and 4mmol 3Be added drop-wise in the above-mentioned bismuth-containing solution, put into ultrasonic instrument behind the stirring 10min,, form uniform mixed liquor in 30 ℃ of following ultrasonic cleaning 20min;
The 3rd step, with the mixed liquor that obtains in reactor at 200 ℃ of microwave hydrothermal 3h, be cooled to normal temperature, clean, obtain sample;
In the 4th step, the sample 62 ℃ of dry 25h in vacuum drying chamber with obtaining obtain jujube cake shape Bi 2W 0.5Mo 0.5O 6Nano-powder.
4. jujube cake shape Bi 2W 0.5Mo 0.5O 6The preparation method of nano-powder is characterized in that, may further comprise the steps:
The first step is with the Bi(NO of 1.5mmol 3) 35H 2O is dissolved in the citric acid solution that 60mL concentration is 0.025mol/L, gets bismuth-containing solution;
Second step is with the Na of 0.4mmol 2WO 42H 2(the NH of O, 0.4mmol 4) 6Mo 7O 24H 2The NaHCO of O and 1.5mmol 3Be added drop-wise in the above-mentioned bismuth-containing solution, put into ultrasonic instrument behind the stirring 10min,, form uniform mixed liquor in 25 ℃ of following ultrasonic cleaning 15min;
The 3rd step, with the mixed liquor that obtains in reactor at 200 ℃ of microwave hydrothermal 1.5h, be cooled to normal temperature, clean, obtain sample;
In the 4th step, the sample 80 ℃ of dry 20h in vacuum drying chamber with obtaining obtain jujube cake shape Bi 2W 0.5Mo 0.5O 6Nano-powder.
5. jujube cake shape Bi 2W 0.5Mo 0.5O 6The preparation method of nano-powder is characterized in that, may further comprise the steps:
The first step is with the Bi(NO of 3mmol 3) 35H 2O is dissolved in the citric acid solution that 85mL concentration is 0.02mol/L, gets bismuth-containing solution;
Second step is with the Na of 0.75mmol 2WO 42H 2(the NH of O, 0.75mmol 4) 6Mo 7O 24H 2The NaHCO of O and 3mmol 3Be added drop-wise in the above-mentioned bismuth-containing solution, put into ultrasonic instrument behind the stirring 10min,, form uniform mixed liquor in 25 ℃ of following ultrasonic cleaning 15min;
The 3rd step, with the mixed liquor that obtains in reactor at 200 ℃ of microwave hydrothermal 2h, be cooled to normal temperature, clean, obtain sample;
In the 4th step, the sample 70 ℃ of dry 20h in vacuum drying chamber with obtaining obtain jujube cake shape Bi 2W 0.5Mo 0.5O 6Nano-powder.
6. jujube cake shape Bi according to claim 1 2W 0.5Mo 0.5O 6The preparation method of nano-powder is characterized in that, NaHCO in described second step 3The dropping time be 1～20min.
7. jujube cake shape Bi according to claim 1 2W 0.5Mo 0.5O 6The preparation method of nano-powder is characterized in that, the cleaning in described the 3rd step is meant respectively washs cooled product 3 times with deionized water and absolute ethyl alcohol.
8. jujube cake shape Bi according to claim 1 2W 0.5Mo 0.5O 6The preparation method of nano-powder is characterized in that, the microwave hydrothermal in described the 3rd step utilizes the microwave hydrothermal instrument to finish.
CN 201110187157 2011-07-06 2011-07-06 Preparation method of data cake-shaped Bi2W0.5Mo0.5O6 nanometer powder Expired - Fee Related CN102309962B (en)

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CN105148903B (en) * 2015-08-14 2017-12-29 南昌航空大学 A kind of Bi2WxMo1‑XO6Solid solution catalysis material photo catalytic reduction CO under visible light conditions2The method for preparing methanol and ethanol
CN105797712B (en) * 2016-04-07 2018-01-02 常州大学 The preparation method of molybdenum doping bismuth tungstate/montmorillonite composite material and its application in photocatalysis desulfurization
CN106799223A (en) * 2016-12-29 2017-06-06 广州凯耀资产管理有限公司 A kind of synthetic method of Bi systems compound semiconductor photocatalytic material

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