CN111871436A - Bismuth sulfide-carbon nitride heterojunction photocatalyst material and preparation method thereof - Google Patents
Bismuth sulfide-carbon nitride heterojunction photocatalyst material and preparation method thereof Download PDFInfo
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- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 claims description 14
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/20—Carbon compounds
- B01J27/22—Carbides
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- B01J35/00—Catalysts, in general, characterised by their form or physical properties
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Abstract
The invention discloses a bismuth sulfide-carbon nitride heterojunction photocatalyst material, Bi2S3Is uniformly dispersed in g-C3N4On the surface of (2), said g-C3N4Exist in a two-dimensional sheet shape, and the Bi2S3Mainly consists of nano particles, and the diameter of the nano particles is about 20-30 nm. The invention relates to a preparation method of a bismuth sulfide-carbon nitride heterojunction photocatalyst material, which adopts a hydrothermal method to prepare g-C3N4And Bi2S3Preparation of Bi as a starting Material2S3/g‑C3N4Sample, the invention is prepared by mixing metal sulfide (Bi)2S3) And g-C3N4Compounding to improve g-C3N4The invention adopts a thermal polycondensation method to obtain g-C3N4A light yellow powdery sample is prepared by adopting a hydrothermal reaction method at g-C3N4Middle load Bi2S3To obtain different Bi2S3Bi of supported amount2S3/g‑C3N4The bismuth sulfide-carbon nitride heterojunction photocatalyst material prepared by the invention has the advantages of stable chemical property, no toxicity, low price, simplicity and easy obtainment.
Description
Technical Field
The invention belongs to the field of textile engineering, relates to a bismuth sulfide-carbon nitride heterojunction photocatalyst material, and further relates to a preparation method of the bismuth sulfide-carbon nitride heterojunction photocatalyst material.
Background
The rapid development of the printing and dyeing industry causes a great deal of organic dye pollution and is very harmful to the environment. The gradual deterioration of the ecological environment seriously hinders the sustainable development of human beings, the two problems of resource exhaustion and environmental pollution break the balance of the ecological system and threaten the physical health of people, and therefore, the development of new measures for protecting the environment is an urgent task. Solar energy is an energy source which is wide in coverage range, clean, harmless and inexhaustible, and can effectively utilize the solar energy, so that great contribution can be made to solving the social energy problem. Therefore, the photocatalytic technology is a high-efficiency way to solve energy and environmental crisis by using solar energy, and is widely concerned by various research fields in society. The photocatalytic reaction refers to that under the illumination of ultraviolet light to infrared light wavelength range (about 100-1000 nm), when the solar energy is larger than the forbidden bandwidth of the catalyst, the Valence Band (VB) electrons of the catalyst can be excited and transited to the Conduction Band (CB), and in the process, a large amount of photo-generated electrons (e) are accompanied-) Generation, and at the same time, holes (h) are formed at positions on VB where electrons are lost due to electron transfer+). Only a part of the generated photogenerated carriers can migrate to the surface of the catalyst, gather on the surface and contact with reactants to react: e.g. of the type-Has the advantages ofStrong reducibility, can convert O into2Reduction of molecules, H2Disproportionation of O to CO2Organic matters and the like are subjected to reduction reaction; h is+Has strong oxidizing property, and can promote H2O、OH-And organic matters and the like are subjected to oxidation reaction, so that pollutants are degraded, and the other part of carriers cannot reach the surface of the catalyst and are recombined in the migration process.
The photocatalysis technology can be developed and applied to the fields of environmental management and energy: photocatalytic production of hydrogen, conversion of solar energy into hydrogen energy form and storage, and H2Is a good clean energy; the carbon dioxide is subjected to photocatalytic reduction to generate chemical fuels such as methane, methanol, formaldehyde and the like which can be used by human beings, so that carbon circulation is realized, and the problem of resource shortage is relieved; in addition, the photocatalysis can degrade organic pollutants such as dye, pesticide and the like into CO2And H2O, has important significance for environmental treatment. Therefore, the preparation of the photocatalytic material and the improvement of the performance of the photocatalytic material become research hotspots for solving the resource problem and the environmental problem.
g-C3N4As one of the most promising photocatalytic materials, the material has the advantages of stable chemical property, no toxicity, low price, simplicity, easy obtainment and the like, and is widely applied to the field of photocatalysis. However, g-C3N4There are also a number of inherent drawbacks affecting its photocatalytic efficiency: first, the photocatalytic reactions are all carried out on the surface of the catalyst, and g-C3N4The specific surface area of the catalyst is small, so that the catalyst is not in sufficient contact with pollutants and the reaction is not sufficient; secondly, g-C3N4In the visible light wave band, the utilization of the solar energy is low; and, g-C3N4E of-、h+Very easily in g-C3N4The internal recombination can not reach the surface of the catalyst to participate in the reaction, and the quantum efficiency is low. We mainly pass metal sulfide (Bi)2S3) And g-C3N4Compounding to improve g-C3N4Thereby improving the photocatalytic performance thereof. By thermal polycondensation to obtain g-C3N4A light yellow powdery sample is prepared by adopting a hydrothermal reaction method at g-C3N4Middle load Bi2S3To obtain different Bi2S3Bi of supported amount2S3/g-C3N4And (c) a complex.
Disclosure of Invention
The first purpose of the invention is to provide a bismuth sulfide-carbon nitride heterojunction photocatalyst material, which solves the problem of g-C existing in the prior art3N4The specific surface area of (2) is small, the catalyst surface can not be reached to participate in the reaction, and the quantum efficiency is low.
The invention also aims to provide a preparation method of the bismuth sulfide-carbon nitride heterojunction photocatalyst material, which solves the problem of g-C existing in the prior art3N4E of-、h+Very easily in g-C3N4The internal recombination can not reach the surface of the catalyst to participate in the reaction, and the quantum efficiency is low and sufficient.
The first technical proposal adopted by the invention is that a bismuth sulfide-carbon nitride heterojunction photocatalyst material is Bi2S3Is uniformly dispersed in g-C3N4On the surface of (a), g-C3N4In the form of two-dimensional flakes, Bi2S3Mainly consists of nano particles, and the diameter of the nano particles is about 20-30 nm.
The invention adopts another technical scheme that the preparation method of the bismuth sulfide-carbon nitride heterojunction photocatalyst material is used for preparing the bismuth sulfide-carbon nitride heterojunction photocatalyst material and is implemented according to the following steps:
step 1, dissolving bismuth nitrate pentahydrate in an acetone solution, and uniformly stirring to dissolve the bismuth nitrate to obtain a bismuth nitrate acetone solution;
and 4, automatically cooling the reaction kettle to room temperature after the reaction is finished, taking out a sample, sequentially washing the sample with ethanol and deionized water for 3-5 times respectively, and drying and grinding the washed sample to obtain the composite material Bi2S3/g-C3N4And (5) obtaining the bismuth sulfide-carbon nitride heterojunction photocatalyst material by powder.
The invention is also characterized in that:
in the step 1, the mass ratio of the bismuth nitrate pentahydrate to the volume of the acetone solution is 0.0081-0.81 g: 3.5-350 mL, and the stirring time is 10-120 min.
Volume of bismuth nitrate acetone solution in step 2, g-C3N4The mass ratio of the sodium thiosulfate to the sodium thiosulfate is 3.5-350 mL: 0.143-0.429 g: 0.0062-0.62 g; the stirring time is 10-120 min.
The inner container in the step 3 is a polytetrafluoroethylene inner container; the reaction temperature is 150-250 ℃; the reaction time is 15-48 h.
And 4, drying at 50-80 ℃.
The invention has the beneficial effects that:
1. the invention is prepared by mixing metal sulfide (Bi)2S3) And g-C3N4Compounding to improve g-C3N4Thereby improving the photocatalytic performance thereof.
2. The invention adopts a thermal polycondensation method to obtain g-C3N4A light yellow powdery sample is prepared by adopting a hydrothermal reaction method at g-C3N4Middle load Bi2S3To obtain different Bi2S3Bi of supported amount2S3/g-C3N4And (c) a complex.
3. The bismuth sulfide-carbon nitride heterojunction photocatalyst material prepared by the invention has the advantages of stable chemical property, no toxicity, low price, simplicity and easiness in obtaining.
Drawings
FIG. 1 is a flow chart of an embodiment 1 of a method for preparing a bismuth sulfide-carbon nitride heterojunction photocatalyst material according to the present invention;
FIG. 2a is a transmission electron microscope 1 of example 1 of a method for preparing a bismuth sulfide-carbon nitride heterojunction photocatalyst material according to the present invention;
FIG. 2b is a transmission electron microscope 2 of example 1 of a method for preparing a bismuth sulfide-carbon nitride heterojunction photocatalyst material according to the present invention;
FIG. 2c is a transmission electron microscope image 3 of example 1 of a method for preparing a bismuth sulfide-carbon nitride heterojunction photocatalyst material according to the present invention;
FIG. 2d is a transmission electron microscope image 4 of example 1 of a method for preparing a bismuth sulfide-carbon nitride heterojunction photocatalyst material according to the present invention;
FIG. 3 is an evaluation diagram of photocatalytic degradation of rhodamine B in example 1 of a bismuth sulfide-carbon nitride heterojunction photocatalyst material of the invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
Example 1
The invention relates to a bismuth sulfide-carbon nitride heterojunction photocatalyst material, Bi2S3Is uniformly dispersed in g-C3N4On the surface of (a), g-C3N4In the form of two-dimensional flakes, Bi2S3Mainly consists of nano particles, and the diameter of the nano particles is about 20-30 nm.
The invention relates to a preparation method of a bismuth sulfide-carbon nitride heterojunction photocatalyst material, which adopts a hydrothermal method to prepare g-C3N4And Bi2S3Preparation of Bi as a starting Material2S3/g-C3N4The sample, as shown in fig. 1, was specifically performed according to the following steps:
step 1, dissolving bismuth nitrate pentahydrate in an acetone solution, and uniformly stirring to dissolve the bismuth nitrate to obtain a bismuth nitrate acetone solution;
step 4, reaction completionThe reaction kettle is automatically cooled to room temperature, a sample is taken out, ethanol and deionized water are sequentially used for cleaning for 5 times respectively, and the composite material Bi is obtained by drying and grinding2S3/g-C3N4And (5) obtaining the bismuth sulfide-carbon nitride heterojunction photocatalyst material by powder.
In the step 1, the mass ratio of the bismuth nitrate pentahydrate to the volume of the acetone solution is 0.0081 g: 3.5mL, stirring time 10 min.
Volume of bismuth nitrate acetone solution in step 2, g-C3N4The ratio of the sodium thiosulfate to the sodium thiosulfate is 3.5 mL: 0.143 g: 0.0062 g; the stirring time was 10 min.
The inner container in the step 3 is a polytetrafluoroethylene inner container; the reaction temperature is 150 ℃; the reaction time was 15 h.
The drying temperature in step 4 is 50 ℃.
As can be seen in fig. 2: g-C3N4In the form of two-dimensional flakes, Bi2S3Mainly composed of nanoparticles with a diameter of about 20-30 nm and Bi2S3Is uniformly dispersed in g-C3N4On the surface of (a). Bi2S3/g-C3N4TEM image of (B) shows Bi2S3Nanoparticle ratio g-C3N4Dark due to Bi2S3Are heavy atoms. Bi2S3Are well dispersed in g-C3N4On the surface, and the two have intimate interfacial contact. Bi2S3/g-C3N4The formation structure of (c) can be described as follows: first, g-C3N4Effectively mix Bi3+Adsorbed on the surface, and subjected to hydrothermal treatment to form S2-And is combined with Bi3+Reaction to obtain Bi2S3. In addition, after half an hour of sonication, Bi was observed2S3Nanoparticles in g-C3N4Close attachment of the surface, presumably g-C3N4And Bi2S3May have strong interaction with each other, and verifies Bi2S3/g-C3N4And (4) forming a heterojunction.
As can be seen in fig. 3: FIG. 3a is Bi2S3/g-C3N4First order degradation reaction kinetics curve of the complex: -ln (C/C)0) Kt, FIG. 3b is a histogram of the slope of the kinetic curve, which results when g-C3N4When the content of (B) is 0.358g, that is, Bi2S3/g-C3N4the-B is optimal for the degradation rate of rose bengal solution. The result is consistent with the photoelectric performance, namely PL and photocurrent test results.
Example 2
The invention relates to a bismuth sulfide-carbon nitride heterojunction photocatalyst material, Bi2S3Is uniformly dispersed in g-C3N4On the surface of (a), g-C3N4In the form of two-dimensional flakes, Bi2S3Mainly consists of nano particles, and the diameter of the nano particles is about 20-30 nm.
The invention relates to a preparation method of a bismuth sulfide-carbon nitride heterojunction photocatalyst material, which adopts a hydrothermal method to prepare g-C3N4And Bi2S3Preparation of Bi as a starting Material2S3/g-C3N4The sample, as shown in fig. 1, was specifically performed according to the following steps:
step 1, dissolving bismuth nitrate pentahydrate in an acetone solution, and uniformly stirring to dissolve the bismuth nitrate to obtain a bismuth nitrate acetone solution;
and 4, automatically cooling the reaction kettle to room temperature after the reaction is finished, taking out a sample, sequentially washing the sample with ethanol and deionized water for 4 times respectively, and drying and grinding the sample to obtain the composite material Bi2S3/g-C3N4And (5) obtaining the bismuth sulfide-carbon nitride heterojunction photocatalyst material by powder.
In the step 1, the mass ratio of the bismuth nitrate pentahydrate to the volume of the acetone solution is 0.06 g: 10mL, stirring time 30 min.
Volume of bismuth nitrate acetone solution in step 2, g-C3N4The mass ratio of the sodium thiosulfate to the sodium thiosulfate is 20 mL: 0.161 g: 0.0073 g; the stirring time was 40 min.
The inner container in the step 3 is a polytetrafluoroethylene inner container; the reaction temperature is 170 ℃; the reaction time is 15-48 h.
The drying temperature in step 4 is 70 ℃.
Example 3
The invention relates to a bismuth sulfide-carbon nitride heterojunction photocatalyst material, Bi2S3Is uniformly dispersed in g-C3N4On the surface of (a), g-C3N4In the form of two-dimensional flakes, Bi2S3Mainly consists of nano particles, and the diameter of the nano particles is about 20-30 nm.
The invention relates to a preparation method of a bismuth sulfide-carbon nitride heterojunction photocatalyst material, which adopts a hydrothermal method to prepare g-C3N4And Bi2S3Preparation of Bi as a starting Material2S3/g-C3N4The sample is specifically implemented according to the following steps:
step 1, dissolving bismuth nitrate pentahydrate in an acetone solution, and uniformly stirring to dissolve the bismuth nitrate to obtain a bismuth nitrate acetone solution;
and 4, automatically cooling the reaction kettle to room temperature after the reaction is finished, taking out a sample, sequentially washing the sample for 3 times by using ethanol and deionized water respectively, and drying and grinding the washed sample to obtain the composite material Bi2S3/g-C3N4And (5) obtaining the bismuth sulfide-carbon nitride heterojunction photocatalyst material by powder.
In the step 1, the mass ratio of the bismuth nitrate pentahydrate to the volume of the acetone solution is 0.0081-0.81 g: 3.5-350 mL, and the stirring time is 10-120 min.
Volume of bismuth nitrate acetone solution in step 2, g-C3N4The mass ratio of the sodium thiosulfate to the sodium thiosulfate is 40 mL: 0.320 g: 0.55 g; stirring the mixtureThe time is 60 min.
The inner container in the step 3 is a polytetrafluoroethylene inner container; the reaction temperature is 180 ℃; the reaction time was 36 h.
And 4, drying at 50-80 ℃.
Example 4
The invention relates to a bismuth sulfide-carbon nitride heterojunction photocatalyst material, Bi2S3Is uniformly dispersed in g-C3N4On the surface of (a), g-C3N4In the form of two-dimensional flakes, Bi2S3Mainly composed of nanoparticles, with a diameter of about 24 nm.
The invention relates to a preparation method of a bismuth sulfide-carbon nitride heterojunction photocatalyst material, which adopts a hydrothermal method to prepare g-C3N4And Bi2S3Preparation of Bi as a starting Material2S3/g-C3N4The sample is specifically implemented according to the following steps:
step 1, dissolving bismuth nitrate pentahydrate in an acetone solution, and uniformly stirring to dissolve the bismuth nitrate to obtain a bismuth nitrate acetone solution;
and 4, automatically cooling the reaction kettle to room temperature after the reaction is finished, taking out a sample, sequentially washing the sample with ethanol and deionized water for 3-5 times respectively, and drying and grinding the washed sample to obtain the composite material Bi2S3/g-C3N4And (5) obtaining the bismuth sulfide-carbon nitride heterojunction photocatalyst material by powder.
In the step 1, the ratio of the mass of the bismuth nitrate pentahydrate to the volume of the acetone solution is 0.009 g: 9mL, stirring time 110 min.
Volume of bismuth nitrate acetone solution in step 2, g-C3N4The mass ratio of the sodium thiosulfate to the sodium thiosulfate is 100 mL: 0.150 g: 0.0145 g; the stirring time was 20 min.
The inner container in the step 3 is a polytetrafluoroethylene inner container; the reaction temperature is 19 ℃; the reaction time was 40 h.
The drying temperature in step 4 was 77 ℃.
Example 5
The invention relates to a bismuth sulfide-carbon nitride heterojunction photocatalyst material, Bi2S3Uniformly dispersed on the surface of g-C3N4, g-C3N4In the form of two-dimensional flakes, Bi2S3Mainly consists of nano particles, and the diameter of the nano particles is about 20-30 nm.
The invention relates to a preparation method of a bismuth sulfide-carbon nitride heterojunction photocatalyst material, which adopts a hydrothermal method to prepare g-C3N4And Bi2S3Preparation of Bi as a starting Material2S3/g-C3N4The sample is specifically implemented according to the following steps:
step 1, dissolving bismuth nitrate pentahydrate in an acetone solution, and uniformly stirring to dissolve the bismuth nitrate to obtain a bismuth nitrate acetone solution;
and 4, automatically cooling the reaction kettle to room temperature after the reaction is finished, taking out a sample, sequentially washing the sample with ethanol and deionized water for 5 times respectively, and drying and grinding the sample to obtain the composite material Bi2S3/g-C3N4And (5) obtaining the bismuth sulfide-carbon nitride heterojunction photocatalyst material by powder.
In the step 1, the ratio of the mass of the bismuth nitrate pentahydrate to the volume of the acetone solution is 0.81 g: 350mL, stirring time 120 min.
Volume of bismuth nitrate acetone solution in step 2, g-C3N4The mass ratio of the sodium thiosulfate to the sodium thiosulfate is 350 mL: 0.429 g: 0.62 g; the stirring time was 120 min.
The inner container in the step 3 is a polytetrafluoroethylene inner container; the reaction temperature is 250 ℃; the reaction time was 48 h.
The drying temperature in step 4 is 80 ℃.
Claims (6)
1. A bismuth sulfide-carbon nitride heterojunction photocatalyst material is characterized in that Bi2S3Is uniformly dispersed in g-C3N4On the surface of (2), said g-C3N4Exist in a two-dimensional sheet shape, and the Bi2S3Mainly consists of nano particles, and the diameter of the nano particles is about 20-30 nm.
2. A preparation method of a bismuth sulfide-carbon nitride heterojunction photocatalyst material is used for preparing the bismuth sulfide-carbon nitride heterojunction photocatalyst material as claimed in claim 1, and is characterized by comprising the following steps:
step 1, dissolving bismuth nitrate pentahydrate in an acetone solution, and uniformly stirring to dissolve the bismuth nitrate to obtain a bismuth nitrate acetone solution;
step 2, adding g-C into the bismuth nitrate acetone solution obtained in the step 13N4Uniformly stirring the mixture and sodium thiosulfate to obtain a mixed solution;
step 3, placing the mixed solution in an inner container of a reaction kettle, and heating for continuous reaction;
and 4, automatically cooling the reaction kettle to room temperature after the reaction is finished, taking out a sample, sequentially washing the sample with ethanol and deionized water for 3-5 times respectively, and drying and grinding the washed sample to obtain the composite material Bi2S3/g-C3N4And (5) obtaining the bismuth sulfide-carbon nitride heterojunction photocatalyst material by powder.
3. The method for preparing a bismuth sulfide-carbon nitride heterojunction photocatalyst material as claimed in claim 2, wherein the ratio of the mass of bismuth nitrate pentahydrate to the volume of acetone solution in the step 1 is 0.0081-0.81 g: 3.5-350 mL, and the stirring time is 10-120 min.
4. The method for preparing a bismuth sulfide-carbon nitride heterojunction photocatalyst material as claimed in claim 2, wherein the volume of the bismuth nitrate acetone solution in the step 2 is g-C3N4The mass ratio of the sodium thiosulfate to the sodium thiosulfate is 3.5 to350 mL: 0.143-0.429 g: 0.0062-0.62 g; the stirring time is 10-120 min.
5. The method for preparing a bismuth sulfide-carbon nitride heterojunction photocatalyst material as claimed in claim 2, wherein the inner container in the step 3 is a polytetrafluoroethylene inner container; the reaction temperature is 150-250 ℃; the reaction time is 15-48 h.
6. The method for preparing a bismuth sulfide-carbon nitride heterojunction photocatalyst material as claimed in claim 2, wherein the drying temperature in the step 4 is 50-80 ℃.
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