CN114272921A - Nano-rod-shaped Bi2WO6Preparation method and application thereof - Google Patents

Nano-rod-shaped Bi2WO6Preparation method and application thereof Download PDF

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CN114272921A
CN114272921A CN202111395671.9A CN202111395671A CN114272921A CN 114272921 A CN114272921 A CN 114272921A CN 202111395671 A CN202111395671 A CN 202111395671A CN 114272921 A CN114272921 A CN 114272921A
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nanorod
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CN114272921B (en
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任家桐
王琼林
张衡
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Xian Modern Chemistry Research Institute
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Abstract

The invention discloses a nano-rod-shaped Bi2WO6A preparation method and application thereof. The method mainly comprises the steps of mixing bismuth nitrate, sodium oleate, sodium tungstate and urea according to the formula amount, then dripping nitric acid aqueous solution to obtain reaction liquid, wherein the reaction liquid is not stirred, and then reacting for at least more than 32 hours at the temperature of 150-2WO6(ii) a The molar ratio of the bismuth nitrate to the sodium oleate to the sodium tungstate to the urea to the nitric acid is 2:5:1:12.5:(20-30). The method utilizes simple one-step heating reaction, does not need to stir and mix a reaction system before the reaction, and prepares the small-size nanorod-like Bi by virtue of slow dissolution-precipitation balance of a solid-liquid interface in the reaction process2WO6The material solves the technical problem that the material is difficult to prepare. The nano rod-shaped Bi prepared by the invention2WO6The material shows excellent catalytic performance in the reaction of photodegradation of rhodamine B.

Description

Nano-rod-shaped Bi2WO6Preparation method and application thereof
Technical Field
The invention relates to Bi2WO6A preparation technology of a photocatalytic material, in particular to a nano rod-shaped Bi2WO6A preparation method and application thereof, belonging to the technical field of inorganic photocatalytic materials.
Background
Bi2WO6Is an inorganic oxide semiconductor material whose micro-crystal structure is composed of a material having a perovskite structure (WO)4)2-Layer and (Bi) having fluorite structure2O2)2+The layers are alternately stacked. Among various oxide semiconductor materials, Bi2WO6The band gap of (A) is relatively small (generally 2.8-3.0eV), and the absorption spectrum is wide, since it can absorb visible light having a wavelength of about 450 nm. Not only that, Bi2WO6Has high chemical stability and thermal stability, low toxicity and low preparation cost. Thus, Bi2WO6The material is widely applied as a photocatalytic material.
At present, Bi2WO6The nano photocatalytic material is mainly synthesized by a liquid phase reaction, and the general idea is as follows: preparing a solution containing bismuth salt and tungstate, mixing and stirring the solution containing bismuth salt and tungstate to form a solution containing Bi2WO6The precipitated suspension is reacted at high temperature again, passing through Bi2WO6The dissolution-recrystallization process of (a) gives the final product. Under the guidance of such idea, Bi can be treated by means such as adding a surfactant and adjusting the pH of the reaction solution2WO6The feature of the nano photocatalytic material is regulated and controlled, but the concept is difficult to break through, and the one-dimensional Bi with novel feature is difficult to obtain2WO6A nano photocatalytic material. If the above concept is used, the pH of the reaction solution is adjusted to 1 to 3 and a large amount of K is added2SO4As a shape regulating reagent, obtaining the flower-like Bi consisting of two-dimensional nanosheets2WO6Photocatalytic material (CN 201310047288.3). Although there are also references to the preparation of Bi by sonochemical synthesis2WO6Nanorod material, but the size distribution is very uneven and mostly straightThe diameter is large, and the effect of shortening the migration path of a photon-generated carrier and improving the photocatalytic efficiency is limited (J.Mater.Sci.,2014,49, 2085-.
Disclosure of Invention
Aiming at the defects and shortcomings in the prior art, the invention provides nano rod-shaped Bi2WO6A preparation method.
The preparation method provided by the invention comprises the following steps:
mixing bismuth nitrate, sodium oleate, sodium tungstate and urea according to the formula ratio, then dripping nitric acid aqueous solution to obtain reaction liquid, wherein the reaction liquid is not stirred, and then reacting at the temperature of 150-2WO6(ii) a The molar ratio of the bismuth nitrate to the sodium oleate to the sodium tungstate to the urea to the nitric acid is 2:5:1:12.5 (20-30).
In a further scheme, the method also comprises the steps of naturally cooling the reaction solution to room temperature after the reaction is finished, centrifuging, washing and drying the precipitate to obtain the nano rod-shaped Bi2WO6。
In some embodiments, the ratio of bismuth nitrate to reaction solution is 1mmol of bismuth nitrate: 60-90mL of reaction solution.
In some embodiments, the reaction time is 40 to 50 hours.
In a further aspect, the nanorod-shaped Bi2WO6The microscopic appearance of the material is a nano rod-shaped structure which is mutually staggered.
In a further scheme, the diameter of the nanorod is 3-13nm, and the length of the nanorod is 40-250 nm.
The invention has the beneficial technical effects that:
1. the invention does not need to stir and mix the reaction system before the reaction, and can obtain the one-dimensional Bi by utilizing a simple one-step heating reaction2WO6The nanorod photocatalytic material is simple in reaction process, can be prepared by using simple equipment, and has a prospect of being popularized to large-scale production;
2. since Bi2WO6Characteristic of its own two-dimensional layered structure, existing Bi2WO6The nano photocatalytic material is mostly in two-dimensional shapes (such as nano-sheets)Nano disc) or Bi with three-dimensional appearance (such as nano flower and multi-level structure nanosphere) formed by two-dimensional stacking, and one-dimensional appearance (such as nano rod and nano wire)2WO6Few reports have been made on nano photocatalytic materials. The one-dimensional Bi with novel appearance is prepared by means of slow dissolution-precipitation balance between solid-liquid interfaces of the solid raw material and the solvent in the reaction process2WO6The nano rod photocatalysis material solves the problem of one-dimensional Bi2WO6The photocatalytic material is difficult to prepare;
3. bi prepared by the invention2WO6The nanorod photocatalytic material has the diameter smaller than 10nm, so that the migration distance of a photon-generated carrier can be effectively shortened, and the photocatalytic efficiency is improved;
4. bi prepared by the invention2WO6The nano-rod photocatalytic material is far superior to commercial Bi in the reaction of photodegradation of rhodamine B2WO6Material and Bi2WO6The catalytic performance of the nanosheet photocatalytic material is a high-efficiency photodegradation rhodamine B reaction catalyst.
Drawings
FIG. 1 shows Bi prepared in example 12WO6TEM images of the nanorod photocatalytic material.
FIG. 2 shows Bi prepared in example 12WO6TEM image of the nano rod photocatalytic material at magnification.
FIG. 3 shows Bi prepared in example 12WO6XRD spectrogram of nanorod photocatalytic material, in which o-Bi is in pattern2WO6Quadrature phase Bi corresponding to spectral line2WO6Standard XRD spectrum of (1).
FIG. 4 shows Bi prepared in comparative example 12WO6TEM images of nano-photocatalytic materials.
FIG. 5 shows Bi prepared in example 12WO6And testing the result of the photodegradation rhodamine B reaction of the nanorod photocatalytic material.
FIG. 6 shows Bi prepared in comparative example 22WO6TEM images of nano-photocatalytic materials.
FIG. 7 is a drawing showingBi prepared in comparative example 32WO6TEM images of nano-photocatalytic materials.
FIG. 8 shows Bi prepared in comparative examples 2 and 32WO6XRD spectrogram of nano photocatalytic material, in the figure, o-Bi2WO6Quadrature phase Bi corresponding to spectral line2WO6Standard XRD spectrum of (1).
FIG. 9 shows Bi prepared in comparative example 42WO6TEM images of nano-photocatalytic materials.
FIG. 10 shows Bi prepared in comparative example 52WO6TEM images of nano-photocatalytic materials.
FIG. 11 shows Bi prepared in comparative example 62WO6TEM images of nano-photocatalytic materials.
FIG. 12 shows Bi prepared in comparative example 72WO6TEM images of nano-photocatalytic materials.
FIG. 13 shows Bi prepared in comparative examples 5 to 72WO6XRD spectrogram of nano photocatalytic material, in the figure, o-Bi2WO6Quadrature phase Bi corresponding to spectral line2WO6Standard XRD spectrum of (1).
FIG. 14 shows Bi prepared in comparative example 82WO6TEM images of nano-photocatalytic materials.
The technical solution of the present invention is further illustrated by the following examples.
Detailed Description
Unless otherwise specified, the terms or methods herein are understood or implemented using known related methods as would be recognized by one of ordinary skill in the relevant art.
The photodegradation rhodamine B reaction can be realized by adopting the existing method, such as rare earth Ce in the literature3+Doping with Bi2WO6A method disclosed in the environmental science of China (2015), Wangchuning et al.
The present invention is not limited to the following embodiments, and all equivalent changes based on the technical solutions of the present invention fall within the protection scope of the present invention.
The 300W xenon lamp used in the following examples was available from Beijing Pofely technologies, Inc. (China), under the model of Microsalar 300; UV-visible absorption Spectroscopy test UV-3600Plus UV-visible-near Infrared Spectrophotometer available from Shimadzu corporation (Japan); commercial Bi2WO6The photocatalytic material has a CAS number of 13595-87-4, a product number of B914972-1g, and a specification of 1g, and is purchased from Shanghai Michelin Biochemical technology Co., Ltd (China).
Example 1:
this example shows Bi2WO6The preparation method of the nanorod photocatalytic material specifically comprises the following steps:
0.2mmol of Bi (NO) are added in turn3)3·5H2O, 0.5mmol of sodium oleate, 0.1mmol of Na2WO4·2H2O and 1.25mmol urea are added into a reaction vessel, and 2.5mL of urea with the concentration of 1 mol.L is slowly dropped-1Finally diluting with 12.5mL of deionized water to obtain a reaction solution; transferring the reaction solution to an oven stabilized at 160 ℃ in advance without stirring for reaction for 48 hours;
taking out the reaction container after the reaction is finished, naturally cooling to room temperature, centrifuging the obtained precipitate, washing with anhydrous ethanol and deionized water for multiple times, and collecting the product by centrifugation (the centrifugation speed is 9000r min)-1Centrifugation time 10min), and finally drying the product at 70 ℃ to obtain Bi2WO6A nanorod photocatalytic material.
FIG. 1 shows Bi prepared in example 12WO6TEM image of nanorod photocatalytic material, it can be seen that Bi obtained in example 12WO6The nanorod photocatalytic material is in the shape of mutually staggered nanorods, and the length of the nanorods is about 40-240 nm.
FIG. 2 shows Bi prepared in example 12WO6TEM image of magnification of nanorod photocatalytic material, it can be seen that Bi obtained in example 12WO6The nanorods have a diameter of between about 4-12 nm.
FIG. 3 shows a schematic view of a liquid crystal display device of example 1Prepared Bi2WO6XRD spectrogram of nanorod photocatalytic material, in which o-Bi is in pattern2WO6Quadrature phase Bi corresponding to spectral line2WO6Standard XRD spectrum of (1). It can be seen that Bi prepared in example 12WO6The nano-rod photocatalytic material is orthorhombic phase Bi2WO6No obvious diffraction peak of other impurities, good crystallinity and high phase purity.
Comparative example 1:
this comparative example differs from example 1 in that the reaction vessel was stirred for 30min before being transferred to the reaction temperature conditions (i.e. oven).
The morphology of the obtained material is shown in FIG. 4, which shows that Bi obtained in comparative example 12WO6The material is in a nano-sheet stacking shape. This means that the reaction system was stirred before the heating reaction to form a Bi-containing solution in which each solid raw material was uniformly dissolved or dispersed2WO6The precipitated suspension cannot react to obtain Bi with one-dimensional morphology2WO6A nano photocatalytic material.
Example 2:
this example shows Bi obtained in example 12WO6The application of the nanorod photocatalytic material as a reaction catalyst for photodegradation of rhodamine B comprises the following specific steps:
step one, 30mg Bi2WO6The photocatalytic material is ultrasonically dispersed in 80mL solution with the concentration of 10 mg.L-1Obtaining reaction liquid from the rhodamine B water solution, controlling the temperature of the reaction liquid to be 20 ℃ by using condensed water, and stirring for 30min in a dark place to ensure that the reaction liquid reaches adsorption balance;
step two, sucking 1.5mL of reaction solution as a first sampling point, continuing to react for 20min in a dark place, and taking a second sample to measure the degradation reaction degree under the condition without light;
step three, turning on a 300W xenon lamp at 200W cm-2Irradiating the reaction solution with the illumination intensity to initiate photodegradation reaction, sampling once every 20min (1.5 mL for each sampling), taking 5 times in total, centrifuging the sample immediately after each sampling, taking supernatant, and testing by ultraviolet-visible absorption spectrum to obtain the final productUntil the light absorption intensity of the supernatant liquid at 550nm, the concentration of rhodamine B in the reaction liquid at this time is calculated by using the light absorption intensity-concentration curve of the rhodamine B standard solution.
In this example, commercial Bi was used without using a photocatalytic material as the control 12WO6Photocatalytic Material As control 2, Bi in comparative example 1 was used2WO6The nanoplatelet photocatalytic material served as control group 3.
FIG. 5 shows Bi prepared in example 12WO6The reaction test result of the photodegradation rhodamine B of the nanorod photocatalytic material is obtained; bi prepared in example 1 in the photodegradation of rhodamine B2WO6The concentration of rhodamine B is reduced to 17.9 percent of the initial concentration by the nanorod photocatalytic material after 20min dark reaction and 100min illumination reaction. As a control, when the photocatalytic material was not used, the concentration of rhodamine B was reduced to 94.4% of the initial concentration after 20min dark reaction and 100min light reaction; commercial Bi2WO6The concentration of the rhodamine B is reduced to 54.4 percent of the initial concentration by the photocatalytic material after 20min dark reaction and 100min illumination reaction; bi in comparative example 12WO6The nano-sheet photocatalytic material reduces the concentration of rhodamine B to 39.1 percent of the initial concentration after 20min dark reaction and 100min illumination reaction. It can be seen that Bi prepared by the invention2WO6The catalytic performance of the nanorod photocatalytic material for photodegradation of rhodamine B is far superior to that of commercial Bi2WO6Photocatalytic material and Bi2WO6The nanosheet photocatalytic material can be used as a high-efficiency reaction catalyst for photodegradation of rhodamine B.
Comparative example 2:
this comparative example differs from example 1 in that the reaction temperature is 140 ℃. The morphology of the obtained material is shown in FIG. 6, which shows that Bi obtained in comparative example 22WO6The material is in the shape of a nano-sheet. This indicates that if the reaction temperature is too low, Bi with one-dimensional morphology cannot be obtained2WO6A nano photocatalytic material.
Comparative example 3:
this comparative example differs from example 1 in that the reaction temperature is 180 ℃. The morphology of the obtained material is shown in FIG. 7, canSee Bi obtained in this comparative example2WO6The material is in the shape of coexisting nano-sheets and nano-rods, which indicates that pure one-dimensional Bi cannot be obtained at an excessively high reaction temperature2WO6A nano photocatalytic material.
FIG. 8 shows Bi prepared in comparative examples 2 and 32WO6XRD spectrogram of the nano photocatalytic material; in the figure, o-Bi2WO6Quadrature phase Bi corresponding to spectral line2WO6Standard XRD spectrum of (1). It can be seen that Bi prepared in comparative example 22WO6The nano photocatalytic material is not only present corresponding to the orthorhombic phase Bi2WO6The diffraction peak of (2) also has obvious diffraction peaks of other impurities, and the phase purity is not high; bi prepared in comparative example 32WO6The nano-photocatalytic material is orthorhombic phase Bi2WO6No obvious diffraction peak of other impurities, good crystallinity and high phase purity.
Comparative example 4:
this comparative example differs from example 1 in that no sodium oleate is added. The morphology of the obtained material is shown in FIG. 9, which shows that Bi obtained in comparative example 42WO6The material is in the shape of a nano-sheet. This indicates that sodium oleate is present in Bi2WO6The shape control of the nano photocatalytic material is indispensable, and the Bi with one-dimensional shape can not be obtained without adding sodium oleate2WO6A nano photocatalytic material.
Comparative example 5:
this comparative example differs from example 1 in that the reaction time is 8 h. The morphology of the obtained material is shown in FIG. 10, which shows that Bi obtained in comparative example 52WO6The material is in the shape of coexistence of the nano-sheets and the nano-particles. This indicates that when the reaction time is too short, Bi having a one-dimensional morphology cannot be obtained2WO6A nano photocatalytic material.
Comparative example 6:
this comparative example differs from example 1 in that the reaction time is 16 h. The morphology of the obtained material is shown in FIG. 11, which shows that Bi obtained in comparative example 62WO6The material is in the shape of a nano-sheet. This indicates that when the reaction time is too short, a one-dimensional form cannot be obtainedBismuth (Bi) of morphology2WO6A nano photocatalytic material.
Comparative example 7:
this comparative example differs from example 1 in that the reaction time is 32 h. The morphology of the obtained material is shown in FIG. 12, which shows that Bi obtained in comparative example 72WO6The material is in the shape of coexisting nano-sheets, nano-rods and nano-particles. This indicates that when the reaction time is too short, pure one-dimensional Bi can not be obtained2WO6A nano photocatalytic material.
FIG. 13 shows Bi prepared in comparative examples 5 to 72WO6XRD spectrogram of the nano photocatalytic material; in the figure, o-Bi2WO6Quadrature phase Bi corresponding to spectral line2WO6Standard XRD spectrum of (1). It can be seen that Bi prepared in comparative examples 5 to 72WO6The nano photocatalytic materials are all orthorhombic phase Bi2WO6No obvious diffraction peak of other impurities, good crystallinity and high phase purity.
Example 3:
this example is different from example 1 in that 2mL of the solution was dropped at a concentration of 1 mol. L-1The aqueous solution of nitric acid was diluted with 13mL of deionized water to obtain a reaction solution, and finally a product having the same microstructure as the material prepared in example 1 was obtained.
Example 4:
this example is different from example 1 in that 3mL of 1 mol. L was added dropwise-1The aqueous solution of nitric acid was diluted with 12mL of deionized water to obtain a reaction solution, and finally a product having the same microstructure as the material prepared in example 1 was obtained.
Comparative example 8:
this comparative example differs from example 1 in that 5mL of 1 mol. L was added dropwise-1The aqueous nitric acid solution was diluted with 10mL of deionized water to obtain a reaction solution. The morphology of the obtained material is shown in FIG. 14, which shows that Bi obtained in comparative example 82WO6The material is in the shape of coexistence of the nano-sheets and the nano-rods. This shows that the amount of nitric acid added to the reaction solution is equal to Bi2WO6The shape control of the nano photocatalytic material is very important, and when the addition amount of the nitric acid is excessive, a pure one-dimensional shape can not be obtainedBi2WO6A nano photocatalytic material.

Claims (7)

1. Nano-rod-shaped Bi2WO6The preparation method is characterized by comprising the following steps:
mixing bismuth nitrate, sodium oleate, sodium tungstate and urea according to the formula ratio, then dripping nitric acid aqueous solution to obtain reaction liquid, wherein the reaction liquid is not stirred, and then reacting at the temperature of 150-2WO6(ii) a The molar ratio of the bismuth nitrate to the sodium oleate to the sodium tungstate to the urea to the nitric acid is 2:5:1:12.5 (20-30).
2. The nanorod shaped Bi of claim 12WO6The preparation method is characterized by further comprising the steps of naturally cooling the reaction solution to room temperature after the reaction is finished, centrifuging, washing and drying the precipitate to obtain the nano rod-shaped Bi2WO6。
3. The nanorod shaped Bi of claim 12WO6The preparation method is characterized in that the ratio of the bismuth nitrate to the reaction liquid is 1mmol of bismuth nitrate: 60-90mL of reaction solution.
4. The nanorod shaped Bi of claim 12WO6The preparation method is characterized in that the reaction time is 40-50 h.
5. The nanorod shaped Bi of claim 12WO6The preparation method is characterized in that the nano-rod-shaped Bi2WO6The microscopic appearance of the material is a nano rod-shaped structure which is mutually staggered.
6. The nanorod Bi of claim 1 or 52WO6The preparation method is characterized in that the diameter of the nanorod is 3-13nm, and the length of the nanorod is 40-250 nm.
7. RightsNanorod-shaped Bi prepared by the method of claim 12WO6The application of the compound serving as a catalyst in a photodegradation rhodamine B reaction.
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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1951557A (en) * 2006-11-03 2007-04-25 中国科学院上海硅酸盐研究所 Hydrothermal method for preparing superstructure visible light responsive Bi2WO6 photcatalyst
CN101612565A (en) * 2009-07-21 2009-12-30 中国科学院上海硅酸盐研究所 A kind of Bi 2WO 6Nano-fiber cloth, preparation method and application
CN104014326A (en) * 2014-06-25 2014-09-03 上海交通大学 Efficient photocatalyst for bismuth vanadate nanorod and preparation method of catalyst
CN105170137A (en) * 2015-06-03 2015-12-23 河南师范大学 Preparation method of a Bi2WO6 photocatalyst with cubic structure
US20190127883A1 (en) * 2017-10-26 2019-05-02 Soochow University Iodine doped bismuthyl carbonate nanosheet and molybdenum disulfide modified carbon nanofiber composites, preparation method and application thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1951557A (en) * 2006-11-03 2007-04-25 中国科学院上海硅酸盐研究所 Hydrothermal method for preparing superstructure visible light responsive Bi2WO6 photcatalyst
CN101612565A (en) * 2009-07-21 2009-12-30 中国科学院上海硅酸盐研究所 A kind of Bi 2WO 6Nano-fiber cloth, preparation method and application
CN104014326A (en) * 2014-06-25 2014-09-03 上海交通大学 Efficient photocatalyst for bismuth vanadate nanorod and preparation method of catalyst
CN105170137A (en) * 2015-06-03 2015-12-23 河南师范大学 Preparation method of a Bi2WO6 photocatalyst with cubic structure
US20190127883A1 (en) * 2017-10-26 2019-05-02 Soochow University Iodine doped bismuthyl carbonate nanosheet and molybdenum disulfide modified carbon nanofiber composites, preparation method and application thereof

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