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    • 专利摘要:
    The present invention relates to a two-dimensional bismuth vanadate/ graphene/ carbon nitride composite material, and a preparation method and application thereof. The composite material consists of bismuth vanadate‚ graphene, and carbon nitride, wherein the bismuth vanadate and the carbon nitride are both of two-dimensional sheet structures, the two-dimensional sheet structure of the bismuth vanadate has a length of 300 to 800 nm, the two-dimensional sheet structure of the carbon nitride has a length of 400 nm to 1 um, the bismuth vanadate and the carbon nitride are both distributed on a surface of the graphene, and the main exposed crystal plane of the bismuth vanadate is a {001} crystal plane. Bismuth chloride and ammonia metavanadate are first mixed for reaction and then mixed with graphene oxide and carbon nitride for hydrothermal reaction to obtain the composite material, which constructs a Z-type photocatalytic system to improve the photocatalytic degradation rate.
    公开号:NL2026148A
    申请号:NL2026148
    申请日:2020-07-27
    公开日:2021-02-22
    发明作者:Sun Jing
    申请人:Univ Qilu Technology；
    IPC主号:
    专利说明:

    TWO-DIMENSIONAL BISMUTH VANADATE/ GRAPHENE/ CARBON NITRIDE COMPOSITE MATERIAL, AND PREPARATION METHOD AND
    APPLICATION THEREOF Field of the Invention The present invention belongs to the technical field of nanomaterial preparation, and specifically relates to a two-dimensional BiVOy/ graphene/ carbon nitride composite material, and a preparation method and application thereof.
    Background of the Invention The information disclosed in the background of the invention is merely intended to increase the understanding of the general background of the invention, and should not be construed as acknowledgment or hint in any form that the information constitutes the prior art known by those skilled in the art.
    Solar driven semiconductor photocatalysis technology has attracted people's attention because of its excellent performances in energy conversion and environmental remediation. Studies have shown that bismuth vanadate (BiVO:) with a band gap of 2.4 eV is an ideal photocatalyst, has the characteristics of low preparation cost, environment friendliness, high stability, etc., and thus has been widely used. The inventors found that single BiVO, has certain inherent defects, such as low visible light utilization efficiency, high photogenerated charge recombination rate, low quantum yield and poor adsorption capacity, which limit its further application in practical fields.
    Summary of the Invention In view of the above problems in the prior art, the objective of the present invention is to provide a two-dimensional bismuth vanadate/ graphene/ carbon nitride composite material, and a preparation method and application thereof.
    In order to solve the above technical problems, the technical solution of the present invention Is:
    In a first aspect, a two-dimensional BiVO,/ graphene/ carbon nitride composite material consists of bismuth vanadate, reduced graphene oxide, and carbon nitride (g-CsNy), wherein the bismuth vanadate and the carbon nitride are both of two-dimensional sheet structures, the two-dimensional sheet structure of the bismuth vanadate has a length of 300 to 800 nm, the two-dimensional sheet structure of the carbon nitride has a length of 400 nm to 1 um, the bismuth vanadate and the carbon nitride are both distributed on a surface of the reduced graphene oxide, and the main exposed crystal plane of the bismuth vanadate is a {001} crystal plane.
    XRD spectra show that the bismuth vanadate is dominated by a 004 diffraction peak, indicating that the bismuth vanadate has a dominant orientation along the {001} plane, so it is inferred that the main exposed crystal plane of the bismuth vanadate is the {001} crystal plane.
    The present invention relates to a two-dimensional BiVO/ graphene/ carbon nitride composite material, which is an artificial Z-type photocatalytic system. The construction of the Z-type photocatalytic system can not only improve the separation and migration efficiency of photogenerated carriers, but also maintain the oxidizing ability of photogenerated holes. Therefore, the interface characteristics of the artificial Z-type photocatalytic system play a key role in the photocatalytic performance of a nanomaterial.
    The inventors believe that the Z-type photocatalytic system constructed by photosystems I and II with different morphologies and structures has an important impact on the photocatalytic performance of the system because it will affect the electron transfer path between the interfaces. In the present invention, carbon nitride is used as the photosystem I, BiVO, is used as the photosystem II, and reduced graphene oxide is used as an electron transfer chain. In the two-dimensional sheet structures of bismuth vanadate and carbon nitride synthesized by the present invention, the reduced graphene oxide is connected to the bismuth vanadate and the carbon nitride, which increases the number of intermediates and electrons in the photocatalytic process within the same time, thereby improving the photocatalytic efficiency. Effective application of the BiVO: composite photocatalytic system in photocatalytic degradation of pollutants is achieved.
    In a second aspect, a preparation method of the two-dimensional BiVO./ graphene/ carbon nitride composite material includes dissolving bismuth chloride (BiCl3) into water, adding ammonia metavanadate (NH; VO:;) for mixed reaction, and then adding an ethanolamine solution, graphene oxide, and carbon nitride (g-C;Ny) for hydrothermal reaction to obtain the two-dimensional BiVO:/ graphene/ carbon nitride composite material.
    Bismuth chloride and ammonia metavanadate are first uniformly mixed for reaction, and then mixed with graphene oxide, carbon nitride and ethanolamine solution for hydrothermal reaction, and BiVO, of a two-dimensional sheet structure is gradually generated during the hydrothermal reaction.
    The benefit of the hydrothermal reaction after the three are mixed is: the combination and simultaneous growth of the three can be achieved.
    During the hydrothermal reaction, the graphene oxide is reduced to reduced graphene oxide of a two-dimensional sheet structure, BiVOys and carbon nitride are grown on the surface of graphene oxide and are of sheet structures.
    BiVO, and carbon nitride perform light conversion on the surface of graphene oxide for connecting BiVO, and carbon nitride, and the graphene oxide transfers electrons.
    In some embodiments, a preparation method of the carbon nitride is: calcining urea as a raw material to obtain the carbon nitride.
    Preferably, the temperature of calcination is 500 to 600°C and the time of calcination is 3 to 6 h, preferably 500 to 550°C and 4 to 5 h.
    In some embodiments, the reaction time of bismuth chloride and ammonia metavanadate is 20 to 40 min.
    In some embodiments, the concentration of an aqueous solution of bismuth chloride is 3 to 3.5 mg'mL™. The reason why bismuth chloride is selected as a raw material in the present invention is: the inventors found that the reaction of bismuth chloride and ammonia metavanadate can fully expose the {001} crystal plane of bismuth vanadate, while the bismuth vanadate obtained by reaction of bismuth nitrate and metavanadium in the prior art mostly exposes a {040} crystal plane.
    The inventors found that the {001} crystal plane has better reactivity.
    A two-dimensional sheet structure mainly containing the {001} crystal plane is formed through hydrothermal reaction, which improves the photocatalytic rate.
    In some embodiments, the mass ratio of bismuth chloride, ammonia metavanadate, graphene oxide, and g-C;N4 is (2.4-2.8): (0.7-1.1): (0.047-0.055): (0.9-1.4), preferably (2.45-2.7): (0.8-1): (0.049-0.052): (1-1.2). In some embodiments, the concentration of the graphene oxide is 0.8 to 1.2 g L'!, and the concentration of the ethanolamine solution is 0.8 to 1.2 mol-L"!. In some embodiments, the volume of the ethanolamine solution corresponding to 1 g of bismuth chloride is 1.8 to 3.8 mL.
    The amount of ethanolamine solution added can control the morphology of bismuth vanadate formed, when the volume of ethanolamine solution corresponding to 1 g of bismuth chloride 1s about 1.8-3.8 mL, bismuth vanadate nanosheets are formed, and when the volume of ethanolamine solution corresponding to 1 g of bismuth chloride 1s about 12 mL, bismuth vanadate nanotubes are formed.
    In some embodiments, the temperature of hydrothermal reaction is 160 to 180°C and the time of hydrothermal reaction is 8 to 16 h, preferably 160 to 170°C and 10 to 14 h.
    The temperature and time of the hydrothermal reaction affect the stability of the formed sheet structure.
    If the temperature of the hydrothermal reaction is higher and the time is longer, the sheet structure of the obtained composite material become large, and then the sheet structure cannot be formed.
    In a third aspect, an application of the two-dimensional BiVO:/ graphene/ carbon nitride composite material in the field of photocatalysis is provided, preferably an application in photocatalytic degradation of organic pollutants in water.
    In the Z-type composite photocatalytic system of the composite material of the present invention, carbon nitride is used as a photosystem I, BiVO, is used as a photosystem II, and reduced graphene oxide is used as an electron transfer chain, which is beneficial to reducing the disadvantage of easy recombination of simple photocatalyst photogenerated electrons and holes, and conducting the photogenerated electrons out in time through the graphene, such that oxidation-reduction reaction occurs on the surfaces of bismuth vanadate and carbon nitride respectively.
    A photocatalyst includes the two-dimensional BiVO4/ graphene/ carbon nitride composite material.
    Beneficial effects of the invention: The preparation method provided by the present invention is simple and easy to control. In the synthesized BiVO,/ graphene/ carbon nitride Z-type photocatalytic 5 system, carbon nitride is used as a photosystem I, BiVO: is used as a photosystem II, and reduced graphene oxide is used as an electron transfer chain, such that the conductivity of electrons between interfaces is improved, and the photosystem II has a higher oxidation potential, which greatly improves its catalytic ability under visible light. The preparation method is beneficial to its practical application in the remediation of pollutants.
    Brief Description of the Drawings The accompanying drawings constituting a part of the present invention are used for providing a further understanding of the present application, and the schematic embodiments of the present invention and the descriptions thereof are used for interpreting the present invention, rather than constituting improper limitations to the present invention.
    FIG. 1 illustrates scanning electron microscopy images of a BiVO,/ graphene/ carbon nitride composite photocatalytic system of the present invention; a: a scanning electron microscopy image of carbon nitride in Example 1; b: a scanning electron microscopy image of BiVO, in Comparative Example 1; c: a BiVOy/ graphene/ carbon nitride scanning electron microscopy image after hydrothermal reaction for 12 h in Example 2; FIG. 2 illustrates XRD spectra of BiVO; in Comparative Example 1, BiVOy/ graphene (BiVO4/RGO) in Comparative Example 2, and BiVOy/ graphene/ carbon nitride composite photocatalyst (BiVO4/RGO/g-C3sNy) in Example 2.
    FIG. 3 illustrates the efficiencies of catalytic degradation of methylene blue under visible light by BiVO; in Comparative Example 1, carbon nitride (g-C3N4) in Example 1, BiVO,/ graphene (BiVO4/RGO) in Comparative Example 2, and BiVO:/ graphene/ carbon nitride composite photocatalyst (BiVO4/RGO/g-CsNy) in Example
    2.
    Detailed Description of the Embodiments It should be pointed out that the following detailed descriptions are all exemplary and aim to further illustrate the present invention. Unless otherwise specified, all technical and scientific terms used in the descriptions have the same meanings generally understood by those of ordinary skill in the art of the present invention.
    It should be noted that terms used herein are intended to describe specific embodiments only, instead of limiting the exemplary embodiments according to the present application. As used herein, the singular form is also intended to comprise the plural form unless otherwise indicated in the context. In addition, it should be understood that when the terms “contain” and/or “comprise” are used in the description, they are intended to indicate the presence of features, steps, operations, devices, components and/or combinations thereof.
    The present invention will be further illustrated below in conjunction with embodiments.
    Example 1 g of urea was weighed and put into a semi-closed crucible, and the crucible was placed in a muffle furnace. The urea was heated to 550°C at a rate of 5°C/min and maintained for 4 h to finally obtain light yellow g-C3N4 powder. 0.15 g of this 20 sample was added to 150 mL of 10 mg-L™ methylene blue solution, followed by ultrasonic treatment and stirring in the dark for 30 min to reach an adsorption equilibrium. The solution was irradiated under a 300 W xenon light source, and the degradation efficiency of the sample was calculated.
    Example 2 158 mg of BiCl; was weighed, added into 50 mL of deionized water, and stirred to form a white suspension. 59 mg of NH; VO; powder was weighed and slowly added to the solution, the solution turned from white to yellow, and the solution was continuously stirred for 30 min. Later, 0.3 mL of 1 M ethanolamine solution, 3.16 mL of 1 gL" aqueous GO solution, and 0.064 g of g-C:Ny solid obtained in Example 1 were added, followed by ultrasonic treatment for 30 min and uniform mixing. The solution was poured into a 100 mL polytetrafluoroethylene-lined autoclave and hydrothermally reacted at 160°C for 12 h. The reaction product was centrifuged and washed with absolute ethanol and deionized water, and a solid was collected by drying. 0.15 g of this sample was added to 150 mL of 10 mg L* methylene blue solution, followed by ultrasonic treatment and stirring in the dark for 30 min to reach an adsorption equilibrium. The solution was irradiated under a 300 W xenon light source, and the degradation efficiency of the sample was calculated. Example 3
    166.4 mg of BiCl; was weighed, added into 55 mL of deionized water, and stirred to form a white suspension. 61 mg of NH;VO; powder was weighed and slowly added to the solution, the solution turned from white to yellow, and the solution was continuously stirred for 25 min. Later, 0.3 mL of 1 M ethanolamine solution, 3.16 mL of 1.1 g'L” aqueous GO solution, and 0.064 g of g-C3N; solid obtained in Example 1 were added, followed by ultrasonic treatment for 30 min and uniform mixing. The solution was poured into a 100 mL polytetrafluoroethylene-lined autoclave and hydrothermally reacted at 170°C for 14 h. The reaction product was centrifuged and washed with absolute ethanol and deionized water, and a solid was collected by drying. 0.15 g of this sample was added to 150 mL of 10 mg-L” methylene blue solution, followed by ultrasonic treatment and stirring in the dark for 30 min to reach an adsorption equilibrium. Example 4
    153.4 mg of BiCl; was weighed, added into 50 mL of deionized water, and stirred to form a white suspension. 59 mg of NH; VO; powder was weighed and slowly added to the solution, the solution turned from white to yellow, and the solution was continuously stirred for 35 min. Later, 0.3 mL of 1 M ethanolamine solution, 3.16 mL of 0.9 g'L" aqueous GO solution, and 0.064 g of g-C3N,4 solid obtained in Example 1 were added, followed by ultrasonic treatment for 30 min and uniform mixing. The solution was poured into a 100 mL polytetrafluoroethylene-lined autoclave and hydrothermally reacted at 175°C for 13 h. The reaction product was centrifuged and washed with absolute ethanol and deionized water, and a solid was collected by drying. 0.15 g of this sample was added to 150 mL of 10 mg-L" methylene blue solution, followed by ultrasonic treatment and stirring in the dark for 30 min to reach an adsorption equilibrium. Comparative Example 1 158 mg of BiCl; was weighed, added into 50 mL of deionized water, and stirred to form a white suspension. 59 mg of NH; VO; powder was weighed and slowly added to the solution, the solution turned from white to yellow, and the solution was continuously stirred for 30 min. Later, 0.3 mL of 1 M ethanolamine solution was added, followed by ultrasonic treatment for 30 min and uniform mixing. The solution was poured into a 100 mL polytetrafluoroethylene-lined autoclave and hydrothermally reacted at 160°C for 12 h. The reaction product was centrifuged and washed with absolute ethanol and deionized water, and a solid was collected by drying. 0.15 g of this sample was added to 150 mL of 10 mg L” methylene blue solution, followed by ultrasonic treatment and stirring in the dark for 30 min to reach an adsorption equilibrium. The solution was irradiated under a 300 W xenon light source, and the degradation efficiency of the sample was calculated. Comparative Example 2 158 mg of BiCl; was weighed, added into 50 mL of deionized water, and stirred to form a white suspension. 59 mg of NHsVO; powder was weighed and slowly added to the solution, the solution turned from white to yellow, and the solution was continuously stirred for 30 min. Later, 0.3 mL of 1 M ethanolamine solution and
    3.16 mL of 1 gL" aqueous GO solution were added, followed by ultrasonic treatment for 30 min and uniform mixing. The solution was poured into a 100 mL polytetrafluoroethylene-lined autoclave and hydrothermally reacted at 160°C for 12 h. The reaction product was centrifuged and washed with absolute ethanol and deionized water, and a solid was collected by drying. 0.15 g of this sample was added to 150 mL of 10 mg L* methylene blue solution, followed by ultrasonic treatment and stirring in the dark for 30 min to reach an adsorption equilibrium. Comparative Example 3 158 mg of BiCl; was weighed, added into 50 mL of deionized water, and stirred to form a white suspension. 59 mg of NHsVO; powder was weighed and slowly added to the solution, the solution turned from white to yellow, and the solution was continuously stirred for 30 min. Later, 0.3 mL of | M ethanolamine solution and
    3.16 mL of 1 gL" aqueous GO solution were added, followed by ultrasonic treatment for 30 min and uniform mixing. The solution was poured into a 100 mL polytetrafluoroethylene-lined autoclave and hydrothermally reacted at 160°C for 12 h. The reaction product was centrifuged and washed with absolute ethanol and deionized water, and a solid was collected by drying. The obtained solid was mixed with 0.064 g of g-C3N4 solid obtained in Example 1 to obtain a sample by ultrasonic reaction. 0.15 g of this sample was added to 150 mL of 10 mg-L™ methylene blue solution, followed by ultrasonic treatment and stirring in the dark for 30 min to reach an adsorption equilibrium. The solution was irradiated under a 300 W xenon light source, and the degradation efficiency of the sample was calculated. In Comparative Example 2, bismuth vanadate and graphene oxide were compounded to obtain a composite material, and the degradation efficiency at 90 minutes was 81%, which was lower than that of the Z system. It showed that the growth of single bismuth vanadate in graphene oxide cannot form a good Z-type photocatalytic system, so the degradation efficiency was low.
    In Comparative Example 3, the combination of carbon nitride, graphene, and bismuth vanadate was only loaded by ultrasound, and the resulting sample did not form a Z-type photocatalytic system, so the degradation efficiency was low.
    As shown in FIG. 1, the g-CsNy (FIG. la) prepared in Example 1 is of a thin two-dimensional sheet structure. The BiVO: (FIG. 1b) prepared in Comparative Example 1 is of a thick two-dimensional sheet having a length of about 300 to 800 nm. Two-dimensional sheet BiVOy, graphene and g-C:N,4 can be observed from the BiVO:/ graphene/ carbon nitride (FIG. lc) prepared in Example 2, and the three systems are all intact. In FIG. lc, the two-dimensional sheet BiVOy has a length of 200 to 800 nm, the two-dimensional sheet BiVO; and g-C;Ny are distributed on the surface of the reduced graphene oxide, and the reduced graphene oxide forms a substrate having a certain thickness.
    FIG. 3 illustrates photocatalytic degradation efficiencies of methylene blue. After the graphene was added, the catalytic effect of the BiVO./ graphene sample in Comparative Example 2 was superior to that of the single BiVO; (Comparative Example 1). After compounded with the g-CsNy4 in Example 1, the BiVO:/ graphene/ carbon nitride photocatalytic system prepared in Example 2 had the highest degradation efficiency. From FIG. 2, it can be seen that the main exposed crystal plane of bismuth vanadate is {001} crystal plane.
    Described above are merely preferred embodiments of the present invention, and the present invention is not limited thereto. Various modifications and variations may be made to the present invention for those skilled in the art. Any modification, equivalent substitution or improvement made within the spirit and principle of the present invention shall fall into the protection scope of the present invention.
    权利要求:
    Claims (14)
    [1]
    1. Two-dimensional BiVO./ graphene / carbon nitride composite material, consisting of bismuth vanadate, graphene, and carbon nitride, wherein the bismuth vanadate and the carbon nitride are both two-dimensional sheet structures, the two-dimensional sheet structure of the bismuth vanadate has a length of 300 to 800 nm, the two-dimensional plate structure of the carbon nitride has a length of 400 nm to 1 µm, the bismuth vanadate and the carbon nitride are both distributed on a surface of the graphene, and the main exposed crystal face of the bismuth vanadate has a {001} crystal face is.
    [2]
    A method for preparing the two-dimensional BiVO: / graphene / carbon nitride composite material according to claim 1 comprising: dissolving bismuth chloride in water, adding ammonium metavanadate for a mixed reaction, and then adding an ethanolamine solution, graphene oxide and carbon nitride for a hydrothermal reaction to obtain the two-dimensional BiVO, / graphene / carbon nitride composite material
    [3]
    The method for preparing the two-dimensional BiVO: / graphene / carbon nitride composite material according to claim 2, wherein a preparation method for the carbon nitride is: calcining urea as a raw material to obtain carbon nitride.
    [4]
    The method of preparing the two-dimensional BiVQy / graphene / carbon nitride composite material according to claim 3, wherein the calcination temperature is 500 to 600 ° C and the calcination time is 3 to 6 hours.
    [5]
    The method of preparing the two-dimensional BiVO: / graphene / carbon nitride composite material according to claim 4, wherein the calcination temperature is 500 to 550 ° C and the calcination time is 4 to 5 hours.
    [6]
    The method of preparing the two-dimensional BiVO, / graphene / carbon nitride composite material according to any one of claims 2 to 5, wherein the reaction time of the bismuth chloride and the ammonium metavanadate is 20 to 40 minutes.
    [7]
    The method for preparing the two-dimensional BiVO, / graphene / carbon nitride composite material according to any one of claims 2 to 6, wherein the concentration of an aqueous solution of bismuth chloride is 3 to 3.5 mg mL.
    [8]
    The method for preparing the two-dimensional BiVO./ graphene / carbon nitride composite material according to any one of claims 2 to 7, wherein the mass ratio of bismuth chloride, ammonium metavanadate, graphene oxide, and gCsN4 (2.4-2.8 ): (0.7-1.1): (0.047-0.055): (0.9-1.4).
    [9]
    The method of preparing the two-dimensional BiVO, / graphene / carbon nitride composite material according to claim 8, wherein the mass ratio of bismuth chloride, ammonium metavanadate, graphene oxide, and g-C3N4 (2.45-2.7): (0 , 8-1): (0.049-0.052): (1-1.2).
    [10]
    The method of preparing the two-dimensional BiVO./ graphene / carbon nitride composite material according to any one of claims 2 to 9, wherein the concentration of the graphene oxide is 0.8 to 1.2 g L * and the concentration of the ethanolamine solution is 0.8 to 1.2 mol-L ™.
    [11]
    The method of preparing the two-dimensional BiVO, / graphene / carbon nitride composite material according to any one of claims 2 to 10, wherein the hydrothermal reaction temperature is 160 to 180 ° C and the hydrothermal reaction time is 8 am to 4 pm.
    [12]
    The method of preparing the two-dimensional BiVO./ graphene / carbon nitride composite material according to any one of claims 11, wherein the hydrothermal reaction temperature is 160 to 170 ° C and the hydrothermal reaction time is 10 to 14 hours. .
    [13]
    Use of the two-dimensional BiVO: / graphene / carbon nitride composite material according to claim 1 for photocatalytic degradation of organic contaminants in water.
    [14]
    A photocatalyst containing the two-dimensional BiVO./ graphene / carbon nitride composite material of claim 1.
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    同族专利:
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    引用文献:
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    CN112973757A|2021-03-08|2021-06-18|合肥工业大学|Bismuth vanadate quantum dot/RGO/graphite phase carbon nitride ternary composite photocatalyst and preparation method thereof|
    CN112973756A|2021-03-08|2021-06-18|合肥工业大学|Rod-shaped bismuth vanadate/RGO/graphite phase carbon nitride photocatalytic material and preparation method thereof|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    CN201910749895.1A|CN110327965A|2019-08-14|2019-08-14|A kind of two dimension pucherite/graphene/carbonitride composite material and preparation method and application|
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