CN111203256A - SnS2/Au/g-C3N4Preparation method and application of composite photocatalyst - Google Patents
SnS2/Au/g-C3N4Preparation method and application of composite photocatalyst Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 66
- 239000002131 composite material Substances 0.000 title claims abstract description 62
- 238000000034 method Methods 0.000 title claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000008367 deionised water Substances 0.000 claims abstract description 35
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 35
- 239000002243 precursor Substances 0.000 claims abstract description 29
- 238000003756 stirring Methods 0.000 claims abstract description 24
- 238000002360 preparation method Methods 0.000 claims abstract description 21
- 229910004042 HAuCl4 Inorganic materials 0.000 claims abstract description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 70
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 16
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 16
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- 239000011259 mixed solution Substances 0.000 claims description 6
- 238000001354 calcination Methods 0.000 claims description 5
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- KHMOASUYFVRATF-UHFFFAOYSA-J tin(4+);tetrachloride;pentahydrate Chemical compound O.O.O.O.O.Cl[Sn](Cl)(Cl)Cl KHMOASUYFVRATF-UHFFFAOYSA-J 0.000 claims description 2
- BWGNESOTFCXPMA-UHFFFAOYSA-N Dihydrogen disulfide Chemical compound SS BWGNESOTFCXPMA-UHFFFAOYSA-N 0.000 claims 1
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- 239000000243 solution Substances 0.000 description 25
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 18
- 239000003054 catalyst Substances 0.000 description 11
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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
-
- B01J35/39—
-
- B01J35/396—
-
- B01J35/40—
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/40—Carbon monoxide
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C1/00—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon
- C07C1/02—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon
- C07C1/12—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon from oxides of a carbon from carbon dioxide with hydrogen
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2527/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- C07C2527/24—Nitrogen compounds
Abstract
The invention belongs to the technical field of preparation of green energy materials, and particularly relates to SnS2/Au/g‑C3N4A preparation method and application of the composite photocatalyst; the invention first prepares g-C3N4Precursor and SnS2/g‑C3N4A composite photocatalyst; then SnS2/g‑C3N4Dissolving in deionized water, stirring, ultrasonic treating, and adding HAuCl4The SnS is obtained after the SnS is irradiated by an ultraviolet lamp, cooled to room temperature, cleaned and dried2/Au/g‑C3N4A composite photocatalyst is provided. The preparation method is simple, does not cause resource waste and secondary pollution, and is a green, environment-friendly and efficient pollution treatment technology; obtained SnS2/Au/g‑C3N4Composite photocatalyst for reducing CO2In order to solve the current energy crisis and environmental problems.
Description
Technical Field
The invention relates to a SnS2/Au/g-C3N4A preparation method of a composite photocatalyst and application research thereof belong to the technical field of energy material preparation.
Background
At present, energy crisis and environmental problems are main problems facing us, a large amount of fossil energy is combusted, a large amount of carbon dioxide gas is released, and how to release CO2The conversion into fuel with added value has attracted the attention of most scientific research works, so a novel green, nontoxic and secondary pollution-free efficient environmental treatment new method is urgently needed to be developed, wherein the photocatalytic reduction technology is considered to be an ideal method for realizing carbon cycle at present.
The photocatalysis technology using semiconductor material as photocatalyst and solar energy as driving force has the advantages of green, no toxicity, no secondary pollution and the like, and in recent years, researchers have achieved a series of achievements in continuously exploring new and efficient semiconductor processes. Such as TiO2、ZnO、g-C3N4、CdS、CeVO4And BiXO and other semiconductor materials are widely used in the fields of electrocatalysis, lithium batteries, photocatalysis, and the like.
Wherein g-C3N4Is a typical polymer semiconductor with a structure in which the CN atom is sp2Hybridization results in the formation of highly delocalized pi-conjugated systems. Wherein the Npz orbital component is g-C3N4The Highest Occupied Molecular Orbital (HOMO) and the Cpz orbital form the Lowest Unoccupied Molecular Orbital (LUMO), the forbidden band width is 2.7eV, and the blue-violet light with the wavelength less than 475 in the solar spectrum can be absorbed. g-C3N4Has very suitable semiconductor band edge positions and meets the thermodynamic requirements of photolysis of water to produce hydrogen and oxygen. With conventional TiO2Photocatalyst phase ratio, g-C3N4And can also effectively activate molecular oxygen to generate superoxide radical for the photocatalytic conversion of organic functional groups and the photocatalytic degradation of organic pollutants. g-C3N4Has good thermal stability and chemical stability, and can be stable at high temperature. The thermal stability begins to decrease only above 600 ℃, g-C3N4Can keep stable performance under strong acid and strong alkali, and tests show that the compound can be used for testing acute oral toxicity LD50 of SPF-grade KM mice>5000mg/kg BW, which is practically nontoxic. Has good antibacterial effect on Escherichia coli and Staphylococcus aureus. g-C3N4The method is environment-friendly, has no secondary pollution, can be prepared by various nitrogen-rich precursors (such as dicyandiamide, urea, melamine, thiourea and the like) and various preparation methods, and has the characteristics of short process flow, less used equipment, low requirement on equipment, short preparation time and the like. However, the problems of low yield, low stability of finished products and the like exist, the preparation is mainly carried out in a small amount in a laboratory level, and enterprises can successfully realize large-scale mass production.
In addition, SnS2S being an important n-type transition metal sulfide semiconductor material, being densely packed by two layers of flow2-And Sn sandwiched therebetween4+Composition of each Sn4+Form regular octahedral coordination with six surrounding sulfur atoms, each S is embedded in the definite language of a triangle of Sn atoms, and adjacent S-Sn-S layers are connected through Van der Waals force. The special crystal structure leads to SnS2The electronic structure of (A) has better advantages than other materials, higher thermal stability, chemical stability and higher kinetic constant. The forbidden band width at room temperature is about 2.2-2.35eV, the photocatalyst has good stability in acidic and neutral aqueous solutions, has certain thermal stability and oxidation resistance in air, and is a photocatalytic material with certain development prospect.
At present, a two-dimensional/two-dimensional Z-shaped heterojunction is prepared by adopting a solvothermal method, and the two-dimensional/two-dimensional Z-shaped heterojunction shows good catalyst activity when used in an environment repairing process; there is also literature on the successful preparation of SnS by hydrothermal method2/g-C3N4The composite material shows excellent energy storage performance in a super capacitor; however, the above composite materials also have problems such as a high recombination rate of photogenerated carriers and a low electron transport rate.
Therefore, the invention aims to construct 2D/2D SnS2/g-C3N4The heterojunction is combined with the good electron transmission capacity of the Au nanoparticles, and the bridge built by the Au nanoparticles effectively promotes the separation of photo-generated electron hole pairs in the composite catalyst to construct the efficient and stable intercalation SnS2/Au/g-C3N4Ternary composite photocatalytic material and application thereof in photocatalytic reduction of CO2Research in the field.
Disclosure of Invention
The invention adopts a hydrothermal technical means to prepare SnS2/Au/g-C3N4A composite photocatalyst; aiming at solving the defects of high recombination rate of photon-generated carriers, few photon-generated electrons and the like.
The present invention achieves the above-described object by the following technical means.
SnS2/Au/g-C3N4The preparation method of the composite photocatalyst comprises the following steps:
(1) preparation of g-C3N4Precursor: putting urea into a crucible, wrapping the crucible with tinfoil, putting the crucible into a tubular furnace for calcining, acidifying the obtained sample in nitric acid with the pH value of 1, reacting at a certain temperature, washing with deionized water and ethanol for multiple times, and centrifugally drying to obtain a solid, namely g-C3N4A precursor;
(2)SnS2/g-C3N4preparing a composite photocatalyst:
adding stannic chloride pentahydrate (SnCl)4·5H2O) in ethylene glycol andadding L-cysteine and sodium dodecyl benzene sulfonate into the mixed solution of the ionized water, and uniformly stirring to prepare tin disulfide; finally adding the g-C prepared in the step (1)3N4Forming a mixed solution, adding the mixed solution into a reaction kettle for hydrothermal reaction, washing, centrifuging and drying a product after the reaction to obtain SnS2/g-C3N4A composite photocatalyst;
(3)SnS2/Au/g-C3N4preparation of composite photocatalyst
SnS prepared in the step (2)2/g-C3N4Dissolving in deionized water, stirring, ultrasonic treating, and adding HAuCl4Irradiating with ultraviolet lamp, taking out, naturally cooling to room temperature, washing with deionized water and ethanol for several times, and drying to obtain SnS2/Au/g-C3N4A composite photocatalyst is provided.
Preferably, the calcination in step (1) is carried out at 550 ℃ for 4 h.
Preferably, the certain temperature in the step (1) is 80 ℃, and the reaction time is 8 h.
Preferably, in the step (2), the mass ratio of the tin chloride pentahydrate to the ethylene glycol to the deionized water to the L-cysteine to the sodium dodecyl benzene sulfonate is 0.0877 g: 20mL, 10mL, 0.2423 g: 0.5645 g.
Preferably, in the step (2), the mass ratio of tin disulfide to carbon nitride is 1: (0.25-4).
Preferably, in the step (2), the mass ratio of the tin disulfide to the carbon nitride is 1: 4.
preferably, in the step (2), the temperature of the hydrothermal treatment is 150-200 ℃; the hydrothermal treatment time was 10 h.
Preferably, in the step (3), the SnS2/g-C3N4Deionized water and HAuCl4The amounts of the components are respectively 50 mg: 50 ml:1 to 7 ml.
Preferably, in the step (3), the stirring time is 20-30 min; the ultrasonic treatment time is 40-60 min.
Preferably, in the step (3), the power of the ultraviolet lamp is 8W, and the irradiation time is 10-15 min
Preferably, in the step (3), SnS is obtained2/Au/g-C3N4In the composite photocatalyst, SnS2/g-C3N4The mass ratio of (a) to Au is 1: 49.
the SnS of the invention2/Au/g-C3N4The shape of the nano-particles is a sandwich-shaped intercalation structure, and the size of the nano-particles is 20-100 nm.
SnS prepared by the invention2/Au/g-C3N4Use of a composite photocatalyst for the reduction of carbon dioxide.
The invention has the beneficial effects that:
(1) the invention uses SnS2/g-C3N4The composite material has higher visible light response capability, plays a role of transferring an electron bridge through the Au nano-particle conductor, has more hot electrons due to the plasma resonance effect, and greatly improves the SnS2/Au/g-C3N4Efficiency of photocatalytic reduction of carbon dioxide.
(2) Prepared SnS2Is in a 2-dimensional structure, and Au nano particles are uniformly dispersed in SnS2And g-C3N4And an intercalated morphology structure is formed, so that the conductivity and a multistage electron transmission mechanism of the composite photocatalyst are increased to a greater extent, and more electrons can be effectively added into carbon dioxide reduction.
(3) The invention can prepare SnS through convenient hydrothermal method2/Au/g-C3N4The composite photocatalyst is efficient and stable by building a bridge with the Au nanoparticles.
(4) The invention realizes the purpose of using SnS2/Au/g-C3N4The nano composite material is used as a photocatalyst for reducing carbon dioxide. The semiconductor material is used as a photocatalyst, and under the excitation condition of visible light, the photo-generated electrons realize a special catalysis or conversion process through the interface interaction effect with carbon dioxide gas molecules, so that the carbon dioxide gas is reduced into organic fuelThe method does not cause resource waste and secondary pollution, is simple and convenient to operate, and is a green, environment-friendly and efficient pollution treatment technology.
Drawings
In FIG. 1, a is g-C prepared in example 13N4B is the SnS prepared in example 22C is the SnS prepared in example 52/g-C3N4D is the SnS prepared in example 62/Au/g-C3N4XRD pattern of (a).
In FIG. 2, a is g-C prepared in example 13N4Raman of (a) and b is the SnS prepared in example 22Raman of (5), c is SnS prepared in example 52/g-C3N4Raman of (a) and d is SnS prepared in example 62/Au/g-C3N4Raman map of (a).
FIG. 3 is SnS prepared in example 62/Au/g-C3N4TEM image of composite photocatalyst.
Detailed Description
The invention is further described with reference to the drawings and the detailed description.
Photocatalytic activity evaluation of the photocatalyst prepared in the present invention: under visible light conditions, 0.02g of catalyst and 5ml of Triethanolamine (TEOA) were added to a photoreactor, 100ml of 0.1M sodium hydroxide solution were added and CO was passed in at a large flow rate2Injecting CO at a certain pressure after the gas in the kettle is exhausted2A gas. The custom xenon lamp was turned on under magnetic stirring and samples were analyzed at 1h intervals. Finally, CO is obtained through calculation2Gas reduction of CO and CH4Yield.
Example 1:
(1)g-C3N4preparing a precursor:
weighing 10g of urea, putting the urea into a crucible, wrapping the urea by using tin foil paper, and heating the urea to 550 ℃ in a tube furnace at the speed of 5 ℃/min and maintaining the temperature for 4 hours; then acidifying in nitric acid solution with pH of 1 at a temperature of 80 deg.C/8 h, taking out, naturally cooling to room temperature, and removing ionsWashing with water and ethanol for several times, and drying to obtain g-C3N4A precursor;
(2)SnS2/g-C3N4preparing a composite photocatalyst:
0.0877g SnCl was weighed out4·5H2Placing O (stannic chloride pentahydrate) into a glass beaker, adding 10mL of deionized water and 20mL of ethylene glycol to completely dissolve the O (stannic chloride pentahydrate), magnetically stirring, adding 0.2423g of L-cysteine and 0.5645g of sodium dodecyl benzene sulfonate to generate white precipitate, and continuously stirring for 0.5 h; mixing 0.0212g g-C3N4Adding the precursor into the solution, uniformly mixing, and then pouring the obtained suspension into a 50ml reaction kettle to heat for 12 hours at 160 ℃. Washing, centrifuging and drying to obtain SnS2/g-C3N4A composite photocatalyst;
(3) taking 0.02g of the catalyst and 5ml of Triethanolamine (TEOA) from the sample in (2), adding 95ml of 0.1M sodium hydroxide solution and introducing CO at a large flow rate2Injecting CO at a certain pressure after the gas in the kettle is exhausted2A gas. The custom xenon lamp was turned on under magnetic stirring and samples were analyzed at 1h intervals. After 5h of irradiation, CO was calculated2Gas reduction of CO and CH4The yields were 24.5. mu. mol/g and 17.3. mu. mol/g, respectively.
Example 2:
(1)g-C3N4preparing a precursor:
weighing 10g of urea, putting the urea into a crucible, wrapping the urea by using tin foil paper, and heating the urea to 550 ℃ in a tube furnace at the speed of 5 ℃/min and maintaining the temperature for 4 hours; then acidizing in nitric acid solution with pH value of 1 at 80 deg.C/8 h, taking out, naturally cooling to room temperature, washing with deionized water and ethanol for multiple times, and drying to obtain g-C3N4And (3) precursor.
(2)SnS2/g-C3N4Preparing a composite photocatalyst:
0.0877g SnCl was weighed out4·5H2O (stannic chloride pentahydrate) was placed in a glass beaker, 10mL of deionized water and 20mL of ethylene glycol were added to dissolve completely, magnetic stirring was performed, and 0.2423g of L-cysteine and 0.5645g of dodecaSodium alkyl benzene sulfonate to generate white precipitate, and stirring is continued for 0.5 h. 0.0425g g-C3N4Adding the precursor into the solution, uniformly mixing, and then pouring the obtained suspension into a 50ml reaction kettle to heat for 12 hours at 160 ℃. Washing, centrifuging and drying to obtain SnS2/g-C3N4A composite photocatalyst is provided.
(3) Taking 0.02g of the catalyst and 5ml of Triethanolamine (TEOA) from the sample in (2), adding 95ml of 0.1M sodium hydroxide solution and introducing CO at a large flow rate2Injecting CO at a certain pressure after the gas in the kettle is exhausted2A gas. The custom xenon lamp was turned on under magnetic stirring and samples were analyzed at 1h intervals. After 5h of irradiation, CO was calculated2Gas reduction of CO and CH4The yields were 29.6. mu. mol/g and 21.3. mu. mol/g, respectively.
Example 3:
(1)g-C3N4preparing a precursor:
weighing 10g of urea, putting the urea into a crucible, wrapping the urea by using tin foil paper, and heating the urea to 550 ℃ in a tube furnace at the speed of 5 ℃/min and maintaining the temperature for 4 hours; then acidizing in nitric acid solution with pH value of 1 at 80 deg.C/8 h, taking out, naturally cooling to room temperature, washing with deionized water and ethanol for multiple times, and drying to obtain g-C3N4And (3) precursor.
(2)SnS2/g-C3N4Preparing a composite photocatalyst:
0.0877g SnCl was weighed out4·5H2Placing O (stannic chloride pentahydrate) into a glass beaker, adding 10mL of deionized water and 20mL of ethylene glycol to completely dissolve the O (stannic chloride pentahydrate), magnetically stirring, adding 0.2423g of L-cysteine and 0.5645g of sodium dodecyl benzene sulfonate to generate white precipitate, and continuously stirring for 0.5 h; 0.0849g g-C3N4Adding the precursor into the solution, uniformly mixing, and then pouring the obtained suspension into a 50ml reaction kettle to heat for 12 hours at 160 ℃. Washing, centrifuging and drying to obtain SnS2/g-C3N4A composite photocatalyst is provided.
(3) 0.02g of the catalyst from (2) and 5ml of Triethanolamine (TEOA) were taken and charged into the photoreactor, and 0 was added.95ml of 1M sodium hydroxide solution and CO were passed through at a large flow rate2Injecting CO at a certain pressure after the gas in the kettle is exhausted2A gas. The custom xenon lamp was turned on under magnetic stirring and samples were analyzed at 1h intervals. After 5h of irradiation, CO was calculated2Gas reduction of CO and CH4The yields were 42.5. mu. mol/g and 33.3. mu. mol/g, respectively.
Example 4:
(1)g-C3N4preparing a precursor:
weighing 10g of urea, putting the urea into a crucible, wrapping the urea by using tin foil paper, and heating the urea to 550 ℃ in a tube furnace at the speed of 5 ℃/min and maintaining the temperature for 4 hours; then acidizing in nitric acid solution with pH value of 1 at 80 deg.C/8 h, taking out, naturally cooling to room temperature, washing with deionized water and ethanol for multiple times, and drying to obtain g-C3N4And (3) precursor.
(2)SnS2/g-C3N4Preparing a composite photocatalyst:
0.0877g SnCl was weighed out4·5H2Placing O (stannic chloride pentahydrate) into a glass beaker, adding 10mL of deionized water and 20mL of ethylene glycol to completely dissolve the O (stannic chloride pentahydrate), magnetically stirring, adding 0.2423g of L-cysteine and 0.5645g of sodium dodecyl benzene sulfonate to generate white precipitate, and continuously stirring for 0.5 h; 0.0106g g-C3N4Adding the precursor into the solution, uniformly mixing, and then pouring the obtained suspension into a 50ml reaction kettle to heat for 12 hours at 160 ℃. Washing, centrifuging and drying to obtain SnS2/g-C3N4A composite photocatalyst is provided.
(3) Taking 0.02g of the catalyst and 5ml of Triethanolamine (TEOA) from the sample in (2), adding 95ml of 0.1M sodium hydroxide solution and introducing CO at a large flow rate2Injecting CO at a certain pressure after the gas in the kettle is exhausted2A gas. The custom xenon lamp was turned on under magnetic stirring and samples were analyzed at 1h intervals. After 5h of irradiation, CO was calculated2Gas reduction of CO and CH4The yields were 20.5. mu. mol/g and 12.3. mu. mol/g, respectively.
Example 5:
(1)g-C3N4preparing a precursor:
weighing 10g of urea, putting the urea into a crucible, wrapping the urea by using tin foil paper, and heating the urea to 550 ℃ in a tube furnace at the speed of 5 ℃/min and maintaining the temperature for 4 hours; then acidizing in nitric acid solution with pH value of 1 at 80 deg.C/8 h, taking out, naturally cooling to room temperature, washing with deionized water and ethanol for multiple times, and drying to obtain g-C3N4And (3) precursor.
(2)SnS2/g-C3N4Preparing a composite photocatalyst:
0.0877g SnCl was weighed out4·5H2Placing O (stannic chloride pentahydrate) into a glass beaker, adding 10mL of deionized water and 20mL of ethylene glycol to completely dissolve the O (stannic chloride pentahydrate), magnetically stirring, adding 0.2423g of L-cysteine and 0.5645g of sodium dodecyl benzene sulfonate to generate white precipitate, and continuously stirring for 0.5 h; 0.0849g g-C3N4Adding the precursor into the solution, uniformly mixing, and then pouring the obtained suspension into a 50ml reaction kettle to heat for 12 hours at 160 ℃. Washing, centrifuging and drying to obtain SnS2/g-C3N4A composite photocatalyst;
(3)SnS2/Au/g-C3N4preparing a composite photocatalyst:
then SnS prepared in the step (2)2/g-C3N4Dissolving in 50ml deionized water, stirring for 0.5h, sonicating for 1h, and adding 1ml HAuCl4Irradiating with 8w ultraviolet lamp for 10min, taking out, naturally cooling to room temperature, washing with deionized water and ethanol for multiple times, and drying to obtain SnS2/Au/g-C3N4A composite photocatalyst is provided.
(4) Taking 0.02g of the catalyst and 5ml of Triethanolamine (TEOA) from the sample in (3), adding 95ml of 0.1M sodium hydroxide solution into the photoreactor, and introducing CO at a large flow rate2Injecting CO at a certain pressure after the gas in the kettle is exhausted2A gas. The custom xenon lamp was turned on under magnetic stirring and samples were analyzed at 1h intervals. After 5h of irradiation, CO was calculated2Gas reduction of CO and CH4The yields were 30.5. mu. mol/g and 21.3. mu. mol/g, respectively.
Example 6:
(1)g-C3N4preparing a precursor:
weighing 10g of urea, putting the urea into a crucible, wrapping the urea by using tin foil paper, and heating the urea to 550 ℃ in a tube furnace at the speed of 5 ℃/min and maintaining the temperature for 4 hours; then acidizing in nitric acid solution with pH value of 1 at 80 deg.C/8 h, taking out, naturally cooling to room temperature, washing with deionized water and ethanol for multiple times, and drying to obtain g-C3N4And (3) precursor.
(2)SnS2/g-C3N4Preparing a composite photocatalyst:
0.0877g SnCl was weighed out4·5H2O (stannic chloride pentahydrate) is put into a glass beaker, 10mL of deionized water and 20mL of ethylene glycol are added to completely dissolve the O, the mixture is magnetically stirred, 0.2423g of L-cysteine and 0.5645g of sodium dodecyl benzene sulfonate are added to generate white precipitate, and the stirring is continued for 0.5 h. 0.0849g g-C3N4Adding the precursor into the solution, uniformly mixing, and then pouring the obtained suspension into a 50ml reaction kettle to heat for 12 hours at 160 ℃. Washing, centrifuging and drying to obtain SnS2/g-C3N4A composite photocatalyst;
(3)SnS2/Au/g-C3N4preparing a composite photocatalyst:
then SnS prepared in the step (2)2/g-C3N4Dissolving in 50ml deionized water, stirring for 0.5h, sonicating for 1h, and adding 3ml HAuCl4Irradiating with 8w ultraviolet lamp for 10min, taking out, naturally cooling to room temperature, washing with deionized water and ethanol for multiple times, and drying to obtain SnS2/Au/g-C3N4A composite photocatalyst is provided.
(4) Taking 0.02g of the catalyst and 5ml of Triethanolamine (TEOA) from the sample in (3), adding 95ml of 0.1M sodium hydroxide solution into the photoreactor, and introducing CO at a large flow rate2Injecting CO at a certain pressure after the gas in the kettle is exhausted2A gas. The custom xenon lamp was turned on under magnetic stirring and samples were analyzed at 1h intervals. After 5h of irradiation, CO was calculated2Gas reduction of CO and CH4The yields were 62.5. mu. mol/g and 45.3μmol/g。
Example 7:
(1)g-C3N4preparing a precursor:
weighing 10g of urea, putting the urea into a crucible, wrapping the urea by using tin foil paper, and heating the urea to 550 ℃ in a tube furnace at the speed of 5 ℃/min and maintaining the temperature for 4 hours; then acidizing in nitric acid solution with pH value of 1 at 80 deg.C/8 h, taking out, naturally cooling to room temperature, washing with deionized water and ethanol for multiple times, and drying to obtain g-C3N4And (3) precursor.
(2)SnS2/g-C3N4Preparing a composite photocatalyst:
0.0877g SnCl was weighed out4·5H2O (stannic chloride pentahydrate) is put into a glass beaker, 10mL of deionized water and 20mL of ethylene glycol are added to completely dissolve the O, the mixture is magnetically stirred, 0.2423g of L-cysteine and 0.5645g of sodium dodecyl benzene sulfonate are added to generate white precipitate, and the stirring is continued for 0.5 h. 0.0849g g-C3N4Adding the precursor into the solution, uniformly mixing, and then pouring the obtained suspension into a 50ml reaction kettle to heat for 12 hours at 160 ℃. Washing, centrifuging and drying to obtain SnS2/g-C3N4A composite photocatalyst is provided.
(3)SnS2/Au/g-C3N4Preparing a composite photocatalyst:
then SnS prepared in the step (2)2/g-C3N4Dissolving in 50ml deionized water, stirring for 0.5h, sonicating for 1h, and adding 5ml HAuCl4Irradiating with 8w ultraviolet lamp for 10min, taking out, naturally cooling to room temperature, washing with deionized water and ethanol for multiple times, and drying to obtain SnS2/Au/g-C3N4A composite photocatalyst is provided.
(4) Taking 0.02g of the catalyst and 5ml of Triethanolamine (TEOA) from the sample in (3), adding 95ml of 0.1M sodium hydroxide solution into the photoreactor, and introducing CO at a large flow rate2Injecting CO at a certain pressure after the gas in the kettle is exhausted2A gas. The custom xenon lamp was turned on under magnetic stirring and samples were analyzed at 1h intervals. After 5h of irradiation, CO was calculated2Reduction of gasesCO and CH4The yields were 50.5. mu. mol/g and 36.7. mu. mol/g, respectively.
Example 8:
(1)g-C3N4preparing a precursor:
weighing 10g of urea, putting the urea into a crucible, wrapping the urea by using tin foil paper, and heating the urea to 550 ℃ in a tube furnace at the speed of 5 ℃/min and maintaining the temperature for 4 hours; then acidizing in nitric acid solution with pH value of 1 at 80 deg.C/8 h, taking out, naturally cooling to room temperature, washing with deionized water and ethanol for multiple times, and drying to obtain g-C3N4And (3) precursor.
(2)SnS2/g-C3N4Preparing a composite photocatalyst:
0.0877g SnCl was weighed out4·5H2Placing O (stannic chloride pentahydrate) into a glass beaker, adding 10mL of deionized water and 20mL of ethylene glycol to completely dissolve the O (stannic chloride pentahydrate), magnetically stirring, adding 0.2423g of L-cysteine and 0.5645g of sodium dodecyl benzene sulfonate to generate white precipitate, and continuously stirring for 0.5 h; 0.0849g g-C3N4Adding the precursor into the solution, uniformly mixing, and then pouring the obtained suspension into a 50ml reaction kettle to heat for 12 hours at 160 ℃. Washing, centrifuging and drying to obtain SnS2/g-C3N4A composite photocatalyst;
(3)SnS2/Au/g-C3N4preparing a composite photocatalyst:
then SnS prepared in the step (2)2/g-C3N4Dissolving in 50ml deionized water, stirring for 0.5h, sonicating for 1h, and adding 7ml HAuCl4Irradiating with 8w ultraviolet lamp for 10min, taking out, naturally cooling to room temperature, washing with deionized water and ethanol for multiple times, and drying to obtain SnS2/Au/g-C3N4A composite photocatalyst is provided.
(4) Taking 0.02g of the catalyst and 5ml of Triethanolamine (TEOA) from the sample in (3), adding 95ml of 0.1M sodium hydroxide solution into the photoreactor, and introducing CO at a large flow rate2Injecting CO at a certain pressure after the gas in the kettle is exhausted2A gas. The custom xenon lamp was turned on under magnetic stirring and samples were analyzed at 1h intervals. Warp beamAfter 5h of irradiation, the CO is calculated2Gas reduction of CO and CH4The yields were 26.8. mu. mol/g and 15.2. mu. mol/g, respectively.
FIG. 1 is an XRD pattern of a photocatalyst showing clearly g-C3N4，SnS2，SnS2/g-C3N4,SnS2/Au/g-C3N4All diffraction peaks matched well with the standard card, indicating successful preparation of the desired material.
FIG. 2 is a Raman diagram of a photocatalyst, showing g-C clearly3N4，SnS2，SnS2/g-C3N4And compared with other documents, the key vibration mode of the compound material is shown to be a classical vibration peak of the compound material.
FIG. 3 shows SnS2/Au/g-C3N4TEM image of composite photocatalyst, from which SnS can be seen2/Au/g-C3N4The morphology of the nano-particles is a sandwich intercalation structure, and the size of the nano-particles is 20-100 nm.
The present invention is not limited to the above-described embodiments, and any obvious improvements, substitutions or modifications can be made by those skilled in the art without departing from the spirit of the present invention.
Claims (10)
1. SnS2/Au/g-C3N4The preparation method of the composite photocatalyst is characterized by comprising the following specific steps:
(1) putting urea into a crucible, wrapping the crucible with tinfoil, putting the crucible into a tubular furnace for calcining, acidifying the obtained product in nitric acid with the pH value of 1, reacting at a certain temperature, washing with deionized water and ethanol for multiple times, and centrifugally drying to obtain a solid, namely g-C3N4A precursor;
(2) dissolving tin chloride pentahydrate in a mixed solution of ethylene glycol and deionized water, then adding L-cysteine and sodium dodecyl benzene sulfonate, and uniformly stirring to prepare the tin chloride pentahydrateTin disulfide; finally adding g-C3N4Forming a mixed solution, adding the mixed solution into a reaction kettle for hydrothermal reaction, washing, centrifuging and drying a product after the reaction to obtain SnS2/g-C3N4A composite photocatalyst;
(3)SnS2/Au/g-C3N4preparing a composite photocatalyst: SnS prepared in the step (2)2/g-C3N4Dissolving the composite photocatalyst in deionized water, stirring, performing ultrasonic treatment, and adding HAuCl4Irradiating with ultraviolet lamp, taking out, naturally cooling to room temperature, washing with deionized water and ethanol for several times, and drying to obtain SnS2/Au/g-C3N4A composite photocatalyst is provided.
2. An SnS according to claim 12/Au/g-C3N4The preparation method of the composite photocatalyst is characterized in that the calcination temperature in the step (1) is 550 ℃, and the calcination time is 4 hours; the certain temperature is 80 ℃, and the reaction time is 8 hours.
3. The method for preparing the SnS2/Au/g-C3N4 composite photocatalyst according to claim 1, wherein in the step (2), the mass ratio of the stannic chloride pentahydrate, the ethylene glycol, the deionized water, the L-cysteine and the sodium dodecylbenzenesulfonate is 0.0877 g: 20mL, 10mL, 0.2423 g: 0.5645 g.
4. An SnS according to claim 12/Au/g-C3N4The preparation method of the composite photocatalyst is characterized in that in the step (2), the mass ratio of the tin disulfide to the carbon nitride is 1: (0.25-4).
5. An SnS according to claim 42/Au/g-C3N4The preparation method of the composite photocatalyst is characterized in that in the step (2), the mass ratio of the tin disulfide to the carbon nitride is 1: 4.
6. an SnS according to claim 12/Au/g-C3N4The preparation method of the composite photocatalyst is characterized in that in the step (2), the temperature of the hydrothermal treatment is 150-200 ℃; the hydrothermal treatment time was 10 h.
7. An SnS according to claim 12/Au/g-C3N4The preparation method of the composite photocatalyst is characterized in that in the step (3), the SnS2/g-C3N4Deionized water and HAuCl4The amounts of the components are respectively 50 mg: 50 ml:1 to 7 ml.
8. The method for preparing the SnS2/Au/g-C3N4 composite photocatalyst as claimed in claim 1, wherein in the step (3), the stirring time is 20-30 min; the ultrasonic treatment time is 40-60 min; the power of the ultraviolet lamp is 8W, and the irradiation time is 10-15 min.
9. An SnS according to claim 12/Au/g-C3N4The preparation method of the composite photocatalyst is characterized in that in the step (3), the SnS2/Au/g-C3N4In the composite photocatalyst, SnS2/g-C3N4The mass ratio of (a) to Au is 1: 49.
10. SnS prepared by the preparation method according to any one of claims 1 to 92/Au/g-C3N4Use of a composite photocatalyst for the reduction of carbon dioxide.
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