CN114768790A - Carbon/bismuth oxide composite photocatalyst and preparation method and application thereof - Google Patents

Carbon/bismuth oxide composite photocatalyst and preparation method and application thereof Download PDF

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CN114768790A
CN114768790A CN202210510207.8A CN202210510207A CN114768790A CN 114768790 A CN114768790 A CN 114768790A CN 202210510207 A CN202210510207 A CN 202210510207A CN 114768790 A CN114768790 A CN 114768790A
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bismuth
carbon
bismuth oxide
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CN114768790B (en
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邸丽景
李红琴
县涛
孙小锋
马雪莲
马珂
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Qinghai Normal University
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Abstract

The invention relates to the technical field of photocatalysts, and provides a preparation method of a carbon/bismuth oxide composite photocatalyst. According to the invention, the grifola frondosa is used as a carbon source, so that the grifola frondosa is easy to carbonize and has a rough surface, bismuth ions in bismuth salt can be easily deposited on the surface of the grifola frondosa and do not fall off, and the bismuth oxide with a nanosheet structure can be obtained; in the hydrothermal process, carbon particles formed by carbonization are modified on the surface of the bismuth oxide nanosheet. In the process of catalyzing organic matters by the catalyst prepared by the preparation method, the carbon loaded on the catalyst can inhibit the composition of photo-generated charges and enhance the reactive sites of bismuth oxide, so that the photocatalytic efficiency is enhanced; the nano-sheet structure of the bismuth oxide increases the contact area of the organic matter and the catalyst, thereby further enhancing the catalytic effect.

Description

Carbon/bismuth oxide composite photocatalyst and preparation method and application thereof
Technical Field
The invention belongs to the technical field of photocatalysts, and particularly relates to a carbon/bismuth oxide composite photocatalyst as well as a preparation method and application thereof.
Background
With the development of society, the problem of environmental pollution caused by organic matters is more and more serious, and the organic matters are degraded by utilizing a photocatalysis technology, so that the method is an effective means for solving the organic matter pollution. The photocatalysis technology refers to that the semiconductor photocatalyst can degrade organic matters and decompose water to produce hydrogen under the drive of solar energy, and is considered as a 'green' ideal technology for solving the environmental pollution and the energy shortage.
Conventional photocatalysts such as TiO2And ZnO can only carry out photocatalytic reaction under the irradiation of ultraviolet light. In order to make better use of solar energy, the development of visible light photocatalysts is becoming the focus of research. Wherein the Bi-based photocatalyst (e.g. Bi)2O3BiOBr and BiFeO3Etc.) has received wide attention from people, and has good application potential as a visible light photocatalyst in the aspects of photocatalytic degradation of organic matters and the like.
In order to better develop the potential of the Bi-based photocatalyst, expand the light absorption range, inhibit the separation of photo-generated charges, and improve the photocatalytic efficiency, the Bi-based photocatalyst is usually required to be modified. A commonly used modification means in the prior art is to modify a Bi photocatalyst with a noble metal. Because the content of noble metal is rare in nature. Therefore, it is desired to provide a Bi-based photocatalyst having high catalytic efficiency without using a noble metal.
Disclosure of Invention
In view of this, the present invention aims to provide a preparation method of a carbon/bismuth oxide composite photocatalyst. The Bi-based photocatalyst obtained by the preparation method provided by the invention has higher photocatalytic effect without using noble metal.
In order to achieve the above purpose, the invention provides the following technical scheme:
the invention provides a preparation method of a carbon/bismuth oxide composite photocatalyst, which comprises the following steps:
mixing the dispersing agent, bismuth salt, grifola frondosa, alkali and water, and carrying out hydrothermal reaction to obtain the carbon/bismuth oxide.
Preferably, the dispersant comprises sodium sulfate and/or potassium sulfate.
Preferably, the bismuth salt includes at least one of bismuth nitrate, bismuth sulfate, and bismuth chloride.
Preferably, the base comprises at least one of sodium hydroxide, potassium hydroxide and lithium hydroxide.
Preferably, the mass ratio of the grifola frondosa to the bismuth salt is (0.1-1.2): 1.
preferably, the using amount ratio of the dispersing agent to water to the bismuth salt is (1-5) mmol: (30-50) mL: (0.5-1.5) mmol.
Preferably, the ratio of the amounts of the bismuth salt and the base is (0.5-3): (15-25).
Preferably, the temperature of the hydrothermal reaction is 100-150 ℃, and the time of the hydrothermal reaction is 3-12 h.
The invention provides a carbon/bismuth oxide composite photocatalyst prepared by the preparation method in the scheme, which comprises a bismuth oxide nanosheet and carbon particles loaded on the surface of the bismuth oxide nanosheet.
The invention also provides application of the carbon/bismuth oxide composite photocatalyst in the scheme in catalytic degradation of organic matters.
The invention provides a preparation method of a carbon/bismuth oxide composite photocatalyst, which comprises the following steps: mixing the dispersing agent, bismuth salt, grifola frondosa, alkali and water, and carrying out hydrothermal reaction to obtain the carbon/bismuth oxide composite photocatalyst. The invention promotes the bismuth salt to be uniformly dispersed in the reaction system by adding the dispersant into the reaction system; the alkali provides hydroxide required by the transformation of bismuth salt into bismuth hydroxide and an alkaline environment required by hydrothermal reaction; bismuth hydroxide generated by bismuth salt and alkali is decomposed into bismuth oxide in hydrothermal reaction; by selecting the griffonia simplicifolia as a carbon source, the petals of the griffonia simplicifolia are thin and easy to carbonize, and meanwhile, the surface of the griffiaria is rough, so that bismuth ions in bismuth salt can be easily deposited on the surface of the griffiaria, the bismuth ions do not fall off, and the bismuth salt is favorable for obtaining bismuth oxide with a nanosheet structure in a hydrothermal reaction; in the hydrothermal reaction, carbon particles formed by carbonizing the grifola frondosa are modified on the surface of the bismuth oxide nanosheet, and finally the carbon/bismuth oxide composite photocatalyst is obtained. In the process of catalyzing organic matters by the photocatalyst prepared by the preparation method, the carbon loaded on the catalyst can inhibit the recombination of photo-generated charges and enhance the reactive active sites of bismuth oxide, thereby enhancing the photocatalytic efficiency; the nano-sheet structure of the bismuth oxide increases the contact area of the organic matter and the catalyst, thereby further enhancing the catalytic effect. Experimental results show that when the photocatalyst provided by the invention is used for catalyzing acid orange seven, the reaction lasts for 60min, and the catalysis efficiency can reach 91%.
Drawings
FIG. 1 is a flowchart of the preparation of a carbon/bismuth oxide composite photocatalyst in example 1 of the present invention;
fig. 2 is XRD patterns of the bismuth oxide prepared in comparative example 3 and the carbon/bismuth oxide composite photocatalyst prepared in example 1;
FIG. 3 is an SEM image of bismuth oxide prepared in comparative example 3;
FIG. 4 is an SEM image of the carbon/bismuth oxide composite photocatalyst prepared in example 1;
FIG. 5 is an EDS diagram of the carbon/bismuth oxide composite photocatalyst prepared in example 1;
FIG. 6 is a PL spectrum of a bismuth oxide composite photocatalyst prepared in comparative example 3 and a carbon/bismuth oxide composite photocatalyst prepared in example 1;
FIG. 7 is a graph showing the photocatalytic efficiency of the carbon/bismuth oxide composite photocatalyst AO7 prepared in example 1;
FIG. 8 is a schematic diagram showing the catalytic mechanism of the carbon/bismuth oxide composite photocatalyst prepared in example 1, wherein CB represents the conduction band, VB represents the valence band, and h+Representing a hole.
Detailed Description
The invention provides a preparation method of a carbon/bismuth oxide composite photocatalyst, which comprises the following steps:
mixing a dispersing agent, bismuth salt, Grifola frondosa, alkali and water, and carrying out hydrothermal reaction to obtain the carbon/bismuth oxide composite photocatalyst.
The preparation method comprises the steps of mixing a dispersing agent, bismuth salt, Grifola frondosa, alkali and water, and carrying out hydrothermal reaction to obtain the carbon/bismuth oxide composite photocatalyst.
In the present invention, the dispersant preferably includes sodium sulfate and/or potassium sulfate. According to the invention, the dispersing agent is added into the reaction system, so that the solubility of the bismuth salt in water can be increased, and the bismuth salt is promoted to be uniformly dispersed in the reaction system; the sodium sulfate and/or potassium sulfate is used as the dispersing agent, so that the influence of the dispersing agent on the catalytic capability of the photocatalyst can be reduced, and the catalytic capability of the photocatalyst can be improved to a certain extent by using the metal salt as the dispersing agent.
In the present invention, the bismuth salt preferably includes at least one of bismuth nitrate, bismuth sulfate, and bismuth chloride, and more preferably bismuth nitrate. The invention selects bismuth atoms needed by common bismuth nitrate photocatalyst. In the embodiment of the present invention, the bismuth nitrate is preferably Bi (NO)3)3·5H2And (O). The bismuth nitrate present in the prior art is often present in the form of five crystal waters.
In the present invention, the alkali preferably includes at least one of sodium hydroxide, potassium hydroxide and lithium hydroxide, and more preferably sodium hydroxide. The invention selects common sodium hydroxide to provide hydroxide radical needed by bismuth salt to be converted into bismuth hydroxide, thereby obtaining the bismuth hydroxide and providing alkali environment needed by hydrothermal reaction. In the present invention, the base is preferably added in the form of an aqueous solution. In the invention, the concentration of the alkali aqueous solution is preferably (10-30) g/L, and more preferably (16-20) g/L. The amount of the aqueous solution of the alkali is not particularly specified, and the ratio of the mass of the bismuth salt to the mass of the alkali is (0.5-3): (15-25).
The invention has no special regulation on the source of the griffonia simplicifolia flower, and only needs to select fresh griffonia simplicifolia flower petals in nature. In the present invention, it is preferable that the petals of the griffonia simplicifolia are sequentially subjected to ethanol washing, drying, water washing, drying, and crushing treatments before use. The method for washing with ethanol and water is not particularly specified, and the impurities on the surface of the griffonia simplicifolia can be washed with ethanol and water by adopting a washing method well known to a person skilled in the art. In the present invention, the drying mode is preferably natural airing. The invention adopts a natural drying mode for drying, which is beneficial to ensuring the original shape of the grifola frondosa. The crushing operation is not specially specified, and the griffonia simplicifolia petals are crushed into small pieces by adopting a crushing mode well known to a person skilled in the art. In the present embodiment, the cutting tool is preferably directly torn into small pieces by hand.
In the invention, the dosage ratio of the dispersant, water and bismuth salt is preferably (1-5) mmol: (30-50) mL: (0.5 to 1.5) mmol, more preferably (2 to 4) mmol: (35-45) mL: (0.8 to 1.2) mmol. According to the invention, the dosage of the dispersing agent, the water and the bismuth salt is controlled within the above range, so that bismuth ions can be fully dispersed in the water, and the obtained catalyst has good catalytic capability.
In the present invention, the ratio of the amounts of the bismuth salt and the base is preferably (0.5 to 3): (15-25), more preferably 1: 18. The invention controls the dosage of the bismuth salt and the alkali within the range, on one hand, the bismuth salt and the alkali are beneficial to fully converting bismuth ions into bismuth hydroxide precipitates, and simultaneously, the alkaline environment required by hydrothermal reaction is provided.
In the invention, the mass ratio of the griffonia simplicifolia flower to the bismuth salt is preferably (0.1-1.2): 1, more preferably (0.5 to 1.1): 1, most preferably 1: 1. The method controls the using amount of the griffonia simplicifolia flower within the range, so that carbon particles carbonized from the griffonia simplicifolia flower are uniformly dispersed on a lamellar structure of the bismuth oxide, and the catalytic capability of the photocatalyst is improved.
According to the invention, the dispersant, the bismuth salt and the water are preferably mixed, and then the griffonia simplicifolia and the alkali are sequentially added. In the invention, bismuth salt is generally low in solubility in water, the solubility of bismuth salt can be increased by virtue of a dispersing agent, so that bismuth ions are promoted to be uniformly dispersed in an aqueous solution to obtain a uniform solution of bismuth salt, then the griffonia simplicifolia flower is added, so that the bismuth ions are favorably and uniformly dispersed on the griffonia simplicifolia flower, finally alkali is added, the bismuth ions and hydroxide radicals in the alkali are combined to form bismuth hydroxide precipitate, and the precipitate particles are uniformly dispersed on the griffonia simplicifolia flower.
In the invention, the temperature of the hydrothermal reaction is preferably 100-150 ℃, and more preferably 120 ℃; the time of the hydrothermal reaction is preferably 3-12 h, and more preferably 6 h. The invention limits the temperature and time of the hydrothermal reaction within the range, is beneficial to full carbonization of the grifola frondosa, and simultaneously, the obtained catalyst has better catalytic capability.
After the hydrothermal reaction is finished, the products of the hydrothermal reaction are preferably washed and dried in sequence to obtain the carbon/bismuth oxide composite photocatalyst.
In the invention, the water washing mode is not particularly specified, and impurities on the product of the hydrothermal reaction can be removed by adopting the water washing mode which is well known to a person skilled in the art.
The drying method is not particularly limited in the present invention, and the water in the product of the hydrothermal reaction may be removed by a drying method known to those skilled in the art.
According to the invention, the grifola frondosa is used as a carbon source, so that the grifola frondosa is easy to carbonize and has a rough surface, bismuth ions in bismuth salt can be easily deposited on the surface of the grifola frondosa and do not fall off, and the bismuth oxide with a nanosheet structure can be obtained; in the hydrothermal process, carbon particles formed by carbonization are modified on the surface of the bismuth oxide nanosheet. In the process of catalyzing organic matters by the catalyst prepared by the preparation method, the carbon loaded on the catalyst can inhibit the recombination of photo-generated charges and enhance the reactive active sites of bismuth oxide, so that the photocatalytic efficiency is enhanced; the nano-sheet structure of the bismuth oxide increases the contact area of the organic matter and the catalyst, thereby further enhancing the catalytic effect.
The invention provides a carbon/bismuth oxide composite photocatalyst prepared by the preparation method in the scheme, which comprises a bismuth oxide nanosheet and carbon particles loaded on the surface of the bismuth oxide nanosheet. In the invention, the plate diameter of the bismuth oxide nanosheet is preferably 2-20 nm, and more preferably 5-10 nm. In the invention, the nano-sheet structure of the bismuth oxide increases the contact area between the organic matter and the catalyst, thereby enhancing the catalytic effect.
The invention also provides application of the carbon/bismuth oxide composite photocatalyst in the scheme in catalytic degradation of organic matters. The application of the invention is not specially specified, and the carbon/bismuth oxide composite photocatalyst is added into waste water containing organic matters. In the invention, the concentration of the organic matters in the wastewater is preferably (1-10) mg/L, and more preferably 5 mg/L. In the present invention, the ratio of the mass of the photocatalyst to the volume of the organic matter-containing wastewater is preferably (0.05 to 0.2) g/200mL, and more preferably 0.1g/200 mL. The invention limits the concentration of the organic matter and the dosage of the catalyst to the above range, and has better degradation capability to the catalyst. In the present invention, the wavelength of the light applied is preferably 300nm to 800 nm. In the embodiment of the invention, a 300W xenon light source is preferably adopted to provide the required illumination condition. In the embodiment of the invention, the distance between the xenon light source and the catalytic degradation organic system is preferably 20 cm. Experimental results show that when the photocatalyst provided by the invention is used for carrying out photocatalyst on acid orange seven (AO7), the degradation rate can reach 91% after 60 min.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Example 1
Carbon/bismuth oxide (C/Bi)2O3) The preparation method of the composite photocatalyst comprises the following steps:
(1) adding the geleaf polyporus petals into 100mL of absolute ethyl alcohol, ultrasonically washing for 3 times, filtering and drying the geleaf polyporus petals, washing for 3 times by using deionized water, drying, and shredding into small pieces by hands to obtain the small pieces of the washed and dried geleaf polyporus petals.
(2) Materials and dosage: dispersing agent (Na)2SO4) Bismuth salt (Bi (NO)3)3·5H2O), water and base (NaOH);
wherein the dispersant (Na)2SO4) Water and bismuth salt (Bi (NO)3)3·5H2O) is 3 mmol: 40mL of: 1mmol, the mass ratio of the bismuth salt to the griffonia simplicifolia flower is 0.97: 1 (approach 1)1) the ratio of the amounts of the bismuth salt and the alkali substance is 1: 18.
adding 3mmol of Na2SO4Added to 40mL of deionized water, followed by 1mmol of Bi (NO)3)3·5H2And O, stirring for 45min, then putting 0.5g of clean gelsan flower petals into the solution, stirring for a period of time, then dripping 40mL of NaOH solution with the concentration of 18g/L into the solution to obtain milky solution, placing the milky solution into a reaction kettle, carrying out hydrothermal reaction (reacting for 6h at 120 ℃), washing with water, and drying to obtain the carbon/bismuth oxide composite photocatalyst.
The flow chart of the preparation process is shown in figure 1: adding Bi (NO)3)3·5H2Adding Na into O, Gesang flower and NaOH2SO4Reacting in the solution at 120 ℃ for 6h to obtain carbon/bismuth oxide (C/Bi)2O3) A composite photocatalyst in which particles C are supported on bismuth oxide.
The XRD pattern is shown in FIG. 2, and it can be seen from FIG. 2 that Bi appears in the obtained catalyst2O3And some changes occur, which is probably due to modification of the carbon particles to Bi2O3The intensity of the diffraction peak is changed, but the position of the diffraction peak is not obviously shifted, which shows that the bismuth oxide composite photocatalyst can be prepared by the method.
The SEM picture is shown in FIG. 4, and Bi is shown in FIG. 42O3Mainly exists in a nano-sheet form, and carbon nano-particles are modified in Bi2O3Nanosheet surface, and Bi2O3The surface of the nano sheet is clean and clean, and no other impurities are generated.
The EDS diagram is shown in figure 5, and the figure 5 shows that the composite contains three elements of Bi, O and C, and further confirms that the carbon/bismuth oxide composite photocatalyst is successfully prepared by the experimental method provided by the invention.
The PL spectrogram is shown in FIG. 6, and the fluorescence peak intensity of the carbon/bismuth oxide composite photocatalyst is obviously higher than that of pure Bi from FIG. 62O3Low. This is mainly due to the modification of the carbon nanoparticles to Bi2O3The separation efficiency of the neutral photo-generated charges is effectively improved.
Comparative example 1
The preparation method is the same as that of example 1 except that the hydrothermal temperature in step (2) is 120 ℃ for 1 hour. The experimental results are as follows: the gerbera petals can not be completely carbonized, and the carbon/bismuth oxide composite photocatalyst can not be obtained.
Comparative example 2
The preparation method is the same as that of example 1 except that the hydrothermal temperature in step (2) is 80 ℃ and the reaction is carried out for 6 hours. The experimental results are as follows: the gerbera petals can not be completely carbonized, and the carbon/bismuth oxide composite photocatalyst can not be obtained.
Comparative example 3
The preparation method is the same as example 1 except that no gerbera petals are added in step (2). The product produced is bismuth oxide (Bi)2O3) The shape is micron rod.
The XRD pattern is shown in FIG. 2, which is related to Bi2O3The XRD patterns of the standard products are consistent;
the SEM image is shown in FIG. 3, and Bi can be seen from FIG. 32O3The shape of the structure is a micron rod-shaped structure, and the surface is smooth;
the PL spectrum is shown in FIG. 6, and pure Bi can be seen from FIG. 62O3The intensity of the fluorescence peak is obviously higher than that of the carbon/bismuth oxide composite photocatalyst. This is mainly due to the modification of the carbon nanoparticles to Bi2O3The separation efficiency of the neutral photo-generated charges is effectively improved.
Comparative example 4
The preparation method is the same as that of example 1, except that the mass of the griffonia simplicifolia petals added in the step (2) is 1g, and the mass ratio of the bismuth salt to the griffonia simplicifolia is 0.485: 1. The experimental results are as follows: the carbon/bismuth oxide composite photocatalyst is not prepared.
0.1g of the catalyst prepared in example 1 was added to 200mL of AO7 (acid orange-seven, i.e., 2-naphthol azo sodium p-benzenesulfonate) solution with a concentration of 5mg/L, and photocatalytic reaction was performed under irradiation of a xenon lamp, and a sample was sampled every 10min, and centrifuged to obtain a supernatant, and the solution absorbance was measured by an ultraviolet-visible spectrophotometer to obtain the degradation rate. The test results are shown in FIG. 7.
0.1g of the catalyst prepared in comparative example 3 was added to 200mL of AO7 (acid orange seven, i.e., 2-naphthol azo sodium p-benzenesulfonate) solution at a concentration of 5mg/L, and photocatalytic reaction was performed under irradiation of a xenon lamp, and a sample was sampled every 10min, and centrifuged to obtain a supernatant, and the absorbance of the solution was measured by an ultraviolet-visible spectrophotometer to obtain the degradation rate. The test results are shown in FIG. 7.
As can be seen from FIG. 7, the carbon/bismuth oxide composite photocatalyst prepared in example 1 is compared with Bi prepared in comparative example 32O3The photocatalytic efficiency and the adsorption performance of the catalyst are effectively improved. This indicates that the carbon/bismuth oxide composite photocatalyst prepared in example 1 has a good practical value. Adsorption experiments show that Bi is in 30min2O3And the adsorption rates of the carbon/bismuth oxide photocatalyst were 2.6% and 24.9%, respectively. The photocatalysis experiment shows that the degradation rates of the bismuth oxide and the carbon/bismuth oxide photocatalyst reach 30 percent and 67.2 percent after being illuminated for 30 min. The degradation rate of the bismuth oxide and carbon/bismuth oxide photocatalyst reaches 49 percent and 91 percent after being irradiated for 60 min. (the negative values are shown on the horizontal axis in FIG. 7 because the art typically starts with 0 for light illumination and the previous absorption is considered negative by definition)
The catalytic mechanism of the carbon/bismuth oxide composite photocatalyst prepared in example 1 is schematically shown in FIG. 8. As can be seen from FIG. 8, Bi in the carbon/bismuth oxide composite photocatalyst2O3Under the excitation of sunlight, electrons in the valence band absorb energy and jump into the conduction band to form photo-generated electrons and holes in the conduction band and the valence band, respectively, and the photo-generated electrons can migrate to be modified in Bi2O3On the carbon particles on the surface of the photocatalyst, the photoproduction electrons and holes are effectively separated, and at the same time, the photoproduction electrons and Bi transferred to the carbon particles2O3The photo-generated holes in the valence band of the photocatalyst can generate oxidation-reduction reaction with organic matters attached to the surface of the catalyst, so that the aim of degrading the organic matters is fulfilled.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (10)

1. A preparation method of a carbon/bismuth oxide composite photocatalyst comprises the following steps:
mixing the dispersing agent, bismuth salt, grifola frondosa, alkali and water, and carrying out hydrothermal reaction to obtain the carbon/bismuth oxide composite photocatalyst.
2. The method of claim 1, wherein the dispersant comprises sodium sulfate and/or potassium sulfate.
3. The production method according to claim 1, wherein the bismuth salt includes at least one of bismuth nitrate, bismuth sulfate, and bismuth chloride.
4. The method of claim 1, wherein the base comprises at least one of sodium hydroxide, potassium hydroxide, and lithium hydroxide.
5. The preparation method according to claim 1, wherein the mass ratio of the griffonia simplicifolia flower to the bismuth salt is (0.1-1.2): 1.
6. the preparation method according to claim 1, wherein the amount ratio of the dispersant to water to the bismuth salt is (1 to 5) mmol: (30-50) mL: (0.5-1.5) mmol.
7. The method according to claim 1, wherein the ratio of the amounts of the bismuth salt and the base is (0.5 to 3): (15-25).
8. The preparation method according to claim 1, wherein the temperature of the hydrothermal reaction is 100 to 150 ℃ and the time of the hydrothermal reaction is 3 to 12 hours.
9. The carbon/bismuth oxide composite photocatalyst prepared by the preparation method of any one of claims 1 to 8, which comprises bismuth oxide nanosheets and carbon particles loaded on the surfaces of the bismuth oxide nanosheets.
10. The use of the carbon/bismuth oxide composite photocatalyst described in claim 9 in catalytic degradation of organic matters.
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