CN115318319A - MoS 2 Preparation method of base heterojunction composite catalyst - Google Patents
MoS 2 Preparation method of base heterojunction composite catalyst Download PDFInfo
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- CN115318319A CN115318319A CN202210842902.4A CN202210842902A CN115318319A CN 115318319 A CN115318319 A CN 115318319A CN 202210842902 A CN202210842902 A CN 202210842902A CN 115318319 A CN115318319 A CN 115318319A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
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- 238000000034 method Methods 0.000 claims description 18
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- 150000003463 sulfur Chemical class 0.000 claims description 7
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- TVXXNOYZHKPKGW-UHFFFAOYSA-N sodium molybdate (anhydrous) Chemical compound [Na+].[Na+].[O-][Mo]([O-])(=O)=O TVXXNOYZHKPKGW-UHFFFAOYSA-N 0.000 claims description 4
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Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- 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
- B01J27/24—Nitrogen compounds
-
- B01J35/33—
-
- B01J35/39—
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The present disclosure discloses a MoS 2 The preparation method of the base heterojunction composite catalyst comprises the following steps: dissolving soluble cobalt salt, soluble ferric salt, an alkali source and a surfactant in a solvent, and preparing a magnetic cobalt ferrite precursor by a one-step solvothermal method; calcining the magnetic cobalt ferrite precursor to obtain a cobalt ferrite ball; calcining melamine or urea, carrying out ultrasonic acidification, washing and drying to obtain graphitized carbon nitride nanowires; placing cobalt ferrite balls, soluble molybdenum salt and soluble iron salt in a solvent, and carrying out high-temperature hydrothermal synthesis on the mixture; the mixture and the graphitized carbon nitride nanowire are subjected to in-situ preparation by a one-step hydrothermal method to obtain MoS 2 A base heterojunction composite catalyst.
Description
Technical Field
The disclosure belongs to the technical field of nano material preparation, and particularly relates to a MoS 2 A preparation method of a base heterojunction composite catalyst.
Background
With the rapid development of socioeconomic performance in China, volatile Organic Compounds (VOCs), nitrogen oxides, sulfur dioxide, ammonia gas and the like which are produced by various large-scale chemical engineering projects and discharged in an unorganized mode seriously affect the surrounding ecological environment and the healthy life of people, the problem of atmospheric environmental pollution is increasingly severe, and the efficient prevention and control of the VOCs and the nitrogen oxides are very important.
The current mainstream technology improves the condition of chemical waste gas pollution to a great extent, but has the defects of high treatment cost, short service life of equipment and catalyst, long catalyst regeneration period, secondary pollution and the like. Different from the traditional chemical waste gas treatment technology, the photocatalytic oxidation technology is simple and convenient to operate, green, economical, practical and efficient, and the core of the photocatalytic oxidation technology lies in research and development of a high-performance catalyst.
Graphitized carbon nitride (g-C) 3 N 4 ) Is a typical polymer semiconductor with a narrow band gap (2.7 eV) and a suitable redox potential, however, pure g-C 3 N 4 Electron (e) of - ) And cavity (hours) + ) Leads to a short lifetime of the electrons and thus to pure g-C 3 N 4 Has poor photocatalytic activity. Then, in order to improve the photocatalytic activity, the photocatalytic activity is further improved for g-C 3 N 4 A series of improvements are made on the materials, and a great deal of research is mainly focused on developing nanoscale g-C 3 N 4 And synthesizing the heterostructure composite. In one aspect, 0D g-C 3 N 4 The formation of the nanostructure can increase the g-C 3 N 4 On the other hand, the formation of the heterojunction facilitates the separation of the photogenerated carriers to give it a higher quantum yield. MoS 2 As an ideal semiconductor, has two-dimensional semiconductor characteristics, and g-C 3 N 4 With well-matched energy band positions, the heterojunction can be constructed to provide higher charge mobility. Furthermore, coFe 2 O 4 The semiconductor with narrow band gap can be excited under visible light, and has unique magnetic anisotropy, electrical property, physical and chemical stability and low cost.
Disclosure of Invention
In view of the deficiencies in the prior art, it is an object of the present disclosure to provideFor supplying a MoS 2 Preparation method of base heterojunction composite catalyst and MoS prepared by method 2 The base heterojunction composite catalyst has magnetism and is easy to recover in the practical application process.
In order to achieve the above purpose, the present disclosure provides the following technical solutions:
MoS 2 The preparation method of the base heterojunction composite catalyst comprises the following steps:
s100: dissolving soluble cobalt salt, soluble ferric salt, an alkali source and a surfactant in a solvent, and preparing a magnetic cobalt ferrite precursor by a one-step solvothermal method;
s200: calcining the magnetic cobalt ferrite precursor to obtain a cobalt ferrite ball;
s300: calcining melamine, carrying out ultrasonic acidification, washing and drying to obtain graphitized carbon nitride nanowires;
s400: placing cobalt ferrite balls, soluble molybdenum salt and soluble iron salt in a solvent, and carrying out high-temperature hydrothermal synthesis on the mixture;
s500: the mixture and the graphitized carbon nitride nanowire are subjected to in-situ preparation by a one-step hydrothermal method to obtain MoS 2 A base heterojunction composite catalyst.
Preferably, in step S100, the molar ratio of the soluble cobalt salt to the soluble iron salt is 1:2.
Preferably, the soluble cobalt salts include, but are not limited to: cobalt nitrate, cobalt chloride, cobalt sulfate and cobalt acetate.
Preferably, the iron salts include, but are not limited to: ferric chloride, ferric trichloride, and ferric nitrite.
Preferably, the surfactants include, and are not limited to: polyethylene glycol, polyvinylpyrrolidone and a compound containing a catechol structure.
Preferably, the solvent includes, but is not limited to: water, ethanol, diethylene glycol and ethylene glycol.
Preferably, the mass ratio of the soluble molybdenum salt to the soluble sulfur salt is 1:2.
Preferably, the soluble molybdenum salts include sodium molybdate and ammonium molybdate.
Preferably, the soluble sulfur salts include thiourea and thioacetamide.
Preferably, in step S200, the calcination temperature of the magnetic cobalt ferrite precursor is 300 to 600 ℃, and the calcination time is 2 to 6 hours.
Compared with the prior art, the beneficial effect that this disclosure brought does:
1. zero-dimensional (0D) semiconductor Quantum Dots (QDs) have attracted attention in the fields of photoelectrochemistry and photocatalysis because of their outstanding edges and unique advantages such as quantum confinement effect, large surface area and short effective charge transfer length. However, in the particular case of photocatalysis, quantum dots suffer from several disadvantages: they tend to self-aggregate and the large number of surface defects makes them unstable compared to their bulk counterparts. In addition, their high photoluminescence results in a high recombination rate of photoexcited electrons and holes. The present disclosure provides morphology optimization of graphitized carbon nitride, converting two-dimensional graphitized carbon nitride into zero-dimensional graphitized carbon nitride, and two-dimensional MoS 2 The heterojunction is constructed, so that the QDs are more dispersed and stable to obviously improve the photoelectric performance.
2. By introducing the cobalt ferrite with unique magnetic anisotropy, the catalyst which is easy to recycle is constructed, and the practical application is facilitated.
Drawings
FIG. 1 is a MoS according to an embodiment of the present disclosure 2 A flow chart of a preparation method of the base heterojunction composite catalyst;
fig. 2 is a transmission electron microscope image of graphitized carbon nitride quantum dots provided by an embodiment of the present disclosure;
fig. 3 is a transmission electron microscope image of molybdenum sulfide nanosheets provided by one embodiment of the present disclosure;
FIG. 4 is a transmission electron microscope image of a cobalt ferrite sphere provided by an embodiment of the present disclosure;
FIG. 5 is a MoS provided by an embodiment of the present disclosure 2 Transmission electron micrograph of the base heterojunction composite catalyst.
Detailed Description
Specific embodiments of the present disclosure will be described in detail below with reference to fig. 1 to 5. While specific embodiments of the disclosure are shown in the drawings, it should be understood that the disclosure may be embodied in various forms and should not be limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the disclosure to those skilled in the art.
It should be noted that certain terms are used throughout the description and claims to refer to particular components. As one skilled in the art will appreciate, various names may be used to refer to a component. This specification and claims do not intend to distinguish between components that differ in name but not function. In the following description and in the claims, the terms "include" and "comprise" are used in an open-ended fashion, and thus should be interpreted to mean "include, but not limited to. The description which follows is a preferred embodiment of the disclosure, but is made for the purpose of illustrating the general principles of the disclosure and not for the purpose of limiting the scope of the disclosure. The scope of the present disclosure is to be determined by the terms of the appended claims.
To facilitate an understanding of the embodiments of the present disclosure, the following detailed description is to be considered in conjunction with the accompanying drawings, and the drawings are not to be construed as limiting the embodiments of the present disclosure.
In one embodiment, as shown in FIG. 1, the present disclosure provides a magnetically recoverable MoS 2 The preparation method of the base heterojunction composite catalyst comprises the following steps:
s100: dissolving soluble cobalt salt, soluble ferric salt and a surfactant in a solvent, and preparing a magnetic cobalt ferrite precursor by a one-step solvothermal method;
s200: calcining the magnetic cobalt ferrite precursor to obtain a cobalt ferrite ball;
s300: calcining melamine, carrying out ultrasonic acidification, washing and drying to obtain graphitized carbon nitride nanowires;
s400: placing cobalt ferrite balls, soluble molybdenum salt and soluble sulfur salt in a solvent, and carrying out high-temperature hydrothermal synthesis on the mixture;
s500: the mixture and the graphitized carbon nitride nanowire are prepared in situ by a one-step solvothermal method to obtain MoS 2 A base heterojunction composite catalyst.
In this example, the MoS prepared by the above method was used 2 The base heterojunction composite catalyst sample is dispersed in a container filled with aqueous solution to be in a suspended state, then the sample moves on the outer wall of the container by using a magnet, and the sample can be clearly observed to rapidly settle along with the attraction of the magnet, so that the MoS prepared by the method is proved 2 The base heterojunction composite catalyst has magnetism and is easy to recover.
Hereinafter, the present disclosure will explain the above preparation method in detail with reference to specific examples.
Example 1:
1. adding 6m mol of cobalt nitrate, 12m mol of ferric trichloride and 80m mol of sodium acetate as solvents into water, stirring by magnetic force to completely dissolve, adding 5m mol/L of polyethylene glycol, and stirring for 30 minutes again to obtain a mixed solution. And transferring the mixed solution to a reaction kettle with polytetrafluoroethylene as a lining for solvothermal reaction, preserving heat at 200 ℃ for 12 hours, naturally cooling to room temperature to obtain a magnetic cobalt ferrite precursor with solvent impurities on the surface, alternately washing the precursor with ethanol and deionized water for 3-5 times to remove the redundant solvent impurities until the supernatant is transparent, and finally drying in a vacuum oven at 60 ℃ for 12 hours to obtain the magnetic cobalt ferrite precursor.
2. Placing a magnetic cobalt ferrite precursor in a tube furnace, heating to 300 ℃ at a heating rate of 5 ℃/min, and calcining for 2 hours to obtain a cobalt ferrite ball; FIG. 4 is a transmission electron microscope image of a cobalt ferrite sphere, and FIG. 4 shows a spherical morphology with a diameter of about 150nm and good crystallinity.
3. Weighing 5g of melamine, placing the melamine in a high-temperature tube furnace, heating to 550 ℃ at the speed of 5 ℃/min in the air, and preserving heat for 4 hours; and then grinding into fine powder, calcining again, heating to 500 ℃ at the speed of 2.5 ℃/min, and preserving heat for 2 hours to obtain the graphitized carbon nitride nanosheet with the two-dimensional scale. And then weighing 200mg of graphitized carbon nitride nanosheets with two-dimensional dimensions, placing the graphitized carbon nitride nanosheets in a mixed solution consisting of 20ml of concentrated sulfuric acid and 20ml of concentrated nitric acid, carrying out continuous ultrasonic acidification for 18 hours to strip the graphitized carbon nitride nanosheets, and then carrying out vacuum filtration, washing and drying to obtain the graphitized carbon nitride nanowires.
4. 0.2060g ammonium molybdate and 0.4440g thiourea are weighed and placed in 30ml deionized water, 100mg cobalt ferrite balls are added after stirring till dissolution, the mixture is placed in a high-pressure reaction kettle after continuous stirring for 30min, hydrothermal reaction is carried out at the temperature of 200 ℃, the mixture is naturally cooled to room temperature after heat preservation for 24 hours, ethanol and deionized water are used for alternately washing for 3-5 times, and then the mixture is dried for 12 hours in a vacuum oven at the temperature of 60 ℃ to obtain MoS 2 /CoFe 2 O 4 A composite material.
5. 0.05g of MoS was weighed 2 /CoFe 2 O 4 The composite material and 0.05g of graphitized carbon nitride nano-wire are placed in 20ml of deionized water for ultrasonic dispersion (used for MoS 2 /CoFe 2 O 4 The composite material and the graphitized carbon nitride nano wire are uniformly dispersed) for 1 hour, then the obtained product is put into a reaction kettle at 200 ℃ for hydrothermal reaction for 10 hours, and the magnetic recoverable MoS is obtained 2 A base heterojunction composite catalyst. FIG. 5 is a MoS 2 As can be seen from fig. 5, the cobalt ferrite spheres can be well supported on the molybdenum sulfide nanosheets (the graphitized carbon nitride quantum dots on the nanosheets are not obvious because the graphitized carbon nitride quantum dots have small sizes and are not consistent with the contrast of the nanosheets in the electron microscope), because of MoS 2 /CoFe 2 O 4 CoFe in composite materials 2 O 4 Is an important ferromagnetic material and is also a good semiconductor, and the obtained MoS can be obtained after the ferromagnetic material and the good semiconductor are compounded 2 The base heterojunction composite catalyst has magnetism.
Example 2:
1. 6m mol of cobalt chloride, 12m mol of ferric chloride and 80m mol of sodium citrate are taken as solvents and added into ethanol, after the cobalt chloride, the ferric chloride and the sodium citrate are completely dissolved by magnetic stirring, 10m mol/L of polyvinylpyrrolidone (PVP) is added, and the mixture is stirred for 30 minutes again to obtain a mixed solution. And transferring the mixed solution to a reaction kettle with polytetrafluoroethylene as a lining for solvothermal reaction, preserving heat at 200 ℃ for 12 hours, naturally cooling to room temperature to obtain a magnetic cobalt ferrite precursor with solvent impurities on the surface, alternately washing the precursor with ethanol and deionized water for 3-5 times to remove the redundant solvent impurities until the supernatant is transparent, and finally drying in a vacuum oven at 60 ℃ for 12 hours to obtain the magnetic cobalt ferrite precursor.
2. And (3) placing the magnetic cobalt ferrite precursor into a tube furnace, heating to 400 ℃ at the heating rate of 5 ℃/min, and calcining for 4 hours to obtain the cobalt ferrite ball.
3. Weighing 5g of melamine, placing the melamine in a high-temperature tube furnace, heating to 550 ℃ at the speed of 5 ℃/min in the air, and preserving heat for 4 hours; and then grinding into fine powder, calcining again, heating to 500 ℃ at the speed of 2.5 ℃/min, and preserving heat for 2 hours to obtain the graphitized carbon nitride nanosheet with the two-dimensional scale. And then weighing 200mg of graphitized carbon nitride nanosheets with two-dimensional dimensions, placing the graphitized carbon nitride nanosheets in a mixed solution consisting of 20ml of concentrated sulfuric acid and 20ml of concentrated nitric acid, carrying out continuous ultrasonic acidification for 18 hours to strip the graphitized carbon nitride nanosheets, and then carrying out vacuum filtration, washing and drying to obtain the graphitized carbon nitride nanowires.
4. Weighing 0.2060g of ammonium molybdate and 0.4440g of thiourea, placing the materials into 30ml of deionized water, stirring the materials until the materials are dissolved, adding 200mg of cobalt ferrite balls, continuously stirring the materials for 30min, placing the materials into a high-pressure reaction kettle, carrying out hydrothermal reaction at the temperature of 200 ℃, preserving the temperature for 24 hours, naturally cooling the materials to room temperature, alternately washing the materials with ethanol and deionized water for 3 to 5 times, and then drying the materials in a vacuum oven at the temperature of 60 ℃ for 12 hours to obtain MoS 2 /CoFe 2 O 4 A composite material.
5. 0.05g of MoS was weighed out 2 /CoFe 2 O 4 And (3) placing the composite material and 0.1g of graphitized carbon nitride nano wire in 20ml of deionized water, performing ultrasonic dispersion for 1 hour, and then placing the mixture in a reaction kettle at 200 ℃ for hydrothermal reaction for 10 hours to obtain the magnetic recyclable MoS 2-based heterojunction composite catalyst.
Comparative example 1, example 2 was conducted by replacing the soluble cobalt salt and iron salt in step 1 of example 1 with cobalt chloride and iron chloride, adjusting the calcination temperature in step 2 to 400 ℃, the calcination time to 4 hours, and MoS in step 5 2 /CoFe 2 O 4 And the ratio of the graphitized carbon nitride nanowires is adjusted to 1:2, the specific preparation method and operation method are the same as those in the example 1, and the obtained result is basically consistent with that in the example 1.
Example 3:
1. 6m mol of cobalt nitrate hexahydrate, 12m mol of ferric nitrate and 80m mol of ammonia water are added into ethylene glycol, and after the cobalt nitrate hexahydrate, the ferric nitrate and the ammonia water are completely dissolved by magnetic stirring, 15m mol/L dopamine is added, and the mixture is stirred for 30 minutes again to obtain a mixed solution. And transferring the mixed solution to a reaction kettle with polytetrafluoroethylene as a lining for solvothermal reaction, preserving heat at 200 ℃ for 12 hours, naturally cooling to room temperature to obtain a magnetic cobalt ferrite precursor with solvent impurities on the surface, alternately washing the precursor with ethanol and deionized water for 3-5 times to remove the redundant solvent impurities until the supernatant is transparent, and finally drying in a vacuum oven at 60 ℃ for 12 hours to obtain the magnetic cobalt ferrite precursor.
2. And (3) placing the magnetic cobalt ferrite precursor into a tube furnace, heating to 500 ℃ at the heating rate of 5 ℃/min, and calcining for 5 hours to obtain the cobalt ferrite ball.
3. Weighing 5g of melamine, placing the melamine in a high-temperature tube furnace, heating to 550 ℃ at the speed of 5 ℃/min in the air, and preserving heat for 4 hours; and then grinding into fine powder, calcining again, heating to 500 ℃ at the speed of 2.5 ℃/min, and preserving heat for 2 hours to obtain the graphitized carbon nitride nanosheet with the two-dimensional scale. And then weighing 200mg of graphitized carbon nitride nanosheets with two-dimensional dimensions, placing the graphitized carbon nitride nanosheets in a mixed solution consisting of 20ml of concentrated sulfuric acid and 20ml of concentrated nitric acid, carrying out continuous ultrasonic acidification for 18 hours to strip the graphitized carbon nitride nanosheets, and then carrying out vacuum filtration, washing and drying to obtain the graphitized carbon nitride nanowires.
4. Weighing 0.2060g of sodium molybdate and 0.4440g of thioacetamide, placing the materials into 30ml of deionized water, stirring the materials until the materials are dissolved, adding 300mg of cobalt ferrite balls, continuously stirring the materials for 30min, placing the materials into a high-pressure reaction kettle, carrying out hydrothermal reaction at the temperature of 200 ℃, preserving the heat for 24 hours, naturally cooling the materials to room temperature, alternately washing the materials with ethanol and deionized water for 3 to 5 times, and then drying the materials in a vacuum oven at the temperature of 60 ℃ for 12 hours to obtain MoS 2 /CoFe 2 O 4 A composite material.
5. 0.05g of MoS was weighed 2 -CoFe 2 O 4 The composite material and 0.2g of graphitized carbon nitride nano wire are placed in 20ml of deionized water, the ultrasonic dispersion is carried out for 1 hour, and then the composite material and the graphitized carbon nitride nano wire are placed in a reaction kettle at 200 ℃ for hydrothermal reaction for 10 hours, so that the magnetic recoverable MoS is obtained 2 A base heterojunction composite catalyst.
Comparative example 1, example 3 was conducted by replacing the soluble molybdenum salt and the sulfur salt in step 4 of example 1 with sodium molybdate and thioacetamide, adjusting the calcination temperature to 500 ℃ and the calcination time to 5 hours in step 2, and adjusting MoS in step 5 2 /CoFe 2 O 4 And the ratio of the graphitized carbon nitride nanowires is adjusted to 1:4, the specific preparation method and operation method are the same as those in the example 1, and the obtained result is basically consistent with that in the example 1.
Example 4:
1. adding 6m mol of cobalt nitrate hexahydrate, 12m mol of ferric trichloride and 80m mol of sodium acetate into diethylene glycol, completely dissolving the cobalt nitrate hexahydrate, the ferric trichloride and the sodium acetate by magnetic stirring, adding 20m mol/L of tannic acid or 3- (4-hydroxyphenyl) propionic acid (the two substances and dopamine belong to a compound containing a catechol structure, the compound can be firmly bonded with metal oxide molecules to modify the surface of the dopamine, and meanwhile, a plurality of hydroxyl groups in the structure can also effectively inhibit the growth of nanocrystals to play a role in surface activation), and stirring the mixture for 30 minutes again to obtain a mixed solution. And transferring the mixed solution to a reaction kettle with polytetrafluoroethylene as a lining for solvothermal reaction, preserving heat at 200 ℃ for 12 hours, naturally cooling to room temperature to obtain a magnetic cobalt ferrite precursor with solvent impurities on the surface, alternately washing the precursor with ethanol and deionized water for 3-5 times to remove the redundant solvent impurities until the supernatant is transparent, and finally drying in a vacuum oven at 60 ℃ for 12 hours to obtain the magnetic cobalt ferrite precursor.
2. And (3) placing the magnetic cobalt ferrite precursor into a tube furnace, heating to 300 ℃ at the heating rate of 5 ℃/min, and calcining for 2 hours to obtain the cobalt ferrite ball.
3. Weighing 20g of urea, placing the urea in a high-temperature tube furnace, heating to 550 ℃ at the speed of 5 ℃/min in the air, and preserving the heat for 4 hours to obtain the graphitized carbon nitride nanosheet with the two-dimensional scale (the urea is a porous agent, ammonia gas is released in the high-temperature calcination process, and loose and porous graphitized carbon nitride thin nanosheets can be obtained by one-time calcination). Weighing 200mg of graphitized carbon nitride nanosheets with two-dimensional scales, placing the graphitized carbon nitride nanosheets into a mixed solution consisting of 20ml of concentrated sulfuric acid and 20ml of concentrated nitric acid, carrying out continuous ultrasonic acidification for 18 hours, and then carrying out vacuum filtration, washing and drying to obtain graphitized carbon nitride nanowires;
4. weighing 0.2060g of ammonium molybdate and 0.4440g of thiourea, placing the materials into 30ml of deionized water, stirring the materials until the materials are dissolved, adding 400mg of cobalt ferrite balls, continuously stirring the materials for 30min, placing the materials into a high-pressure reaction kettle, carrying out hydrothermal reaction at the temperature of 200 ℃, keeping the temperature for 24 hours, naturally cooling the materials to room temperature, alternately washing the materials with ethanol and deionized water for 3 to 5 times, and then drying the materials in a vacuum oven at the temperature of 60 ℃ for 12 hours to obtain a product MoS 2 /CoFe 2 O 4 A composite material.
5. 0.05g of MoS was weighed 2 -CoFe 2 O 4 The composite material and 0.3g of graphitized carbon nitride nano wire are placed in 20ml of deionized water, and are placed in a reaction kettle at 200 ℃ for reaction for 10 hours after being subjected to ultrasonic dispersion for 1 hour, so that the magnetic recoverable MoS is obtained 2 A base heterojunction composite catalyst.
Comparative example 1, example 3 was conducted by replacing the melamine in step 3 of example 1 with urea without performing a second calcination. MoS in step 5 2 /CoFe 2 O 4 And the ratio of the graphitized carbon nitride nanowires is adjusted to 1:6, the specific preparation method and operation method are the same as those in the example 1, and the obtained result is basically consistent with that in the example 1.
In the above embodiment, the molar ratio of the soluble cobalt salt to the soluble iron salt is fixed to 1:2, which is determined according to the crystal structure of the magnetic cobalt ferrite to be formed, and experiments prove that the crystal structure of the magnetic cobalt ferrite cannot be formed when the ratio is larger or smaller than this ratio.
The present disclosure has been described in detail, and the principles and embodiments of the present disclosure have been explained herein by using specific examples, which are provided only for the purpose of helping understanding the method and the core concept of the present disclosure; meanwhile, for those skilled in the art, according to the idea of the present disclosure, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present disclosure.
Claims (10)
1. MoS 2 The preparation method of the base heterojunction composite catalyst comprises the following steps:
s100: dissolving soluble cobalt salt, soluble ferric salt, an alkali source and a surfactant in a solvent, and preparing a magnetic cobalt ferrite precursor by a one-step solvothermal method;
s200: calcining the magnetic cobalt ferrite precursor to obtain a cobalt ferrite ball;
s300: calcining melamine or urea, carrying out ultrasonic acidification, washing and drying to obtain graphitized carbon nitride nanowires;
s400: placing cobalt ferrite balls, soluble molybdenum salt and soluble sulfur salt in a solvent, and carrying out high-temperature hydrothermal synthesis on the mixture;
s500: the mixture and the graphitized carbon nitride nanowire are subjected to in-situ preparation by a one-step hydrothermal method to obtain MoS 2 A base heterojunction composite catalyst.
2. The method of claim 1, wherein in step S100, the molar ratio of the soluble cobalt salt to the soluble iron salt is 1:2.
3. The method of claim 1, wherein the soluble cobalt salt includes and is not limited to: cobalt nitrate, cobalt chloride, cobalt sulfate and cobalt acetate.
4. The method of claim 1, wherein said iron salts include, without limitation: ferric chloride, ferric trichloride, and ferric nitrite.
5. The method of claim 1, wherein the surfactant includes and is not limited to: polyethylene glycol, polyvinylpyrrolidone and a compound containing a catechol structure.
6. The method of claim 1, wherein the solvent includes, and is not limited to: water, ethanol, diethylene glycol and ethylene glycol.
7. The method of claim 1, wherein the mass ratio of the soluble molybdenum salt to the soluble sulfur salt is 1:2.
8. The method of claim 1, wherein the soluble molybdenum salts comprise sodium molybdate and ammonium molybdate.
9. The method of claim 1, wherein the soluble sulfur salt comprises thiourea and thioacetamide.
10. The method according to claim 1, wherein in step S200, the calcination temperature of the magnetic cobalt ferrite precursor is 300-600 ℃ and the calcination time is 2-6 hours.
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