CN112044451B - Pt 3 Atomic layer SnS modified by Co alloy 2 Preparation method and application of composite photocatalyst - Google Patents

Pt 3 Atomic layer SnS modified by Co alloy 2 Preparation method and application of composite photocatalyst Download PDF

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CN112044451B
CN112044451B CN202010850914.2A CN202010850914A CN112044451B CN 112044451 B CN112044451 B CN 112044451B CN 202010850914 A CN202010850914 A CN 202010850914A CN 112044451 B CN112044451 B CN 112044451B
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尹世康
王会琴
蒋浩鹏
沈东�
李鑫
李金择
宋相海
霍鹏伟
闫永胜
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Abstract

The invention belongs to the technical field of energy materials, and provides a Pt 3 Co alloy modified atomic layer SnS 2 A composite photocatalyst and a preparation method and application thereof. The invention comprises the following steps: (1) Pt 3 Preparation of Co (2) SnS 2 /Pt 3 Preparing a Co composite photocatalyst: taking a mixed solution of deionized water and ethylene glycol as a solvent, taking stannic chloride pentahydrate, L-cysteine and sodium dodecyl benzene sulfonate as raw materials, and adding a certain amount of Pt into the synthesized tin disulfide 3 Co gel solution is stirred and poured into a vacuum reaction kettle for hydrothermal reaction, after the mixture is naturally cooled, the mixture is washed and put into a drying oven for drying, and SnS is obtained 2 /Pt 3 A Co composite photocatalyst; the method has the advantages of low cost, simple preparation, no resource waste and no secondary pollution, is a green, stable and efficient photoreduction technology, and aims to be used for photoreduction of CO 2 The problems of energy crisis and environment at present are solved.

Description

Pt 3 Co alloy modified atomic layer SnS 2 Preparation method and application of composite photocatalyst
Technical Field
The invention relates to a Pt 3 Co alloy modified atomic layer SnS 2 A preparation method of a composite photocatalyst and application research thereof belong to the technical field of energy material preparation.
Background
With the rapid development of society, a great deal of fossil energy is consumed and simultaneously a great deal of greenhouse gas (the main product is CO) 2 And CH 4 Etc.), which raises a current set of energy crisis and environmental issues (e.g.: energy sources such as coal, petroleum and natural gas are gradually exhausted; sea level rise, glacier melting, and global warming). How to solve the energy crisis and environmental problems is a major challenge facing the twenty-first century. Most researchers are motivated by photosynthesis to concentrate on studying how to treat CO 2 The conversion into carbon-containing value-added fuel, therefore, the photocatalytic reduction technology is currently considered to be an ideal method for realizing carbon cycle, and the development of a novel green, efficient and stable photocatalyst is urgently needed.
In recent years, researchers have achieved a series of results in the continuous search for emerging high-efficiency semiconductors. Such as TiO 2 、ZnO、g-C 3 N 4 、SnS 2 、CdS、CeVO 4 And Bi x O y Cl z And the like are widely applied to the fields of electric catalysis, lithium batteries, photocatalysis and the like.
Wherein, snS 2 The crystal structure is in a layer shape and is formed by a sandwich structure which is closely connected, the sandwich structure shows that the upper layer and the lower layer are sulfur atoms, and the middle sandwich layer is tin atoms. It is important to note here that in this layered crystal structure, the interaction between S and Sn within the S-Sn-S layer is due to covalent bonds, while the adjacent S-Sn-S layers are due to weak van der Waals forces. SnS 2 Unique crystal structure determining SnS 2 Has good performance in optics, electricity and gas sensitivity. In addition, snS 2 The absorption wavelength threshold value is in a visible light range, and not only has good oxidation resistance and thermal stability, but also has good stability in an acidic solution and a neutral solution. Therefore, it is gradually considered as a potential photocatalyst with high quantum efficiency and is a hot point of research.
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; in addition, the hydrothermal method is adopted to successfully prepare the alloy modified semiconductor composite material, and the alloy modified semiconductor 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.
Thus, the present invention is directed to the construction of SnS 2 /Pt 3 The Co heterojunction realizes good photocatalytic reduction activity, the alloy modified semiconductor effectively promotes the separation of photo-generated electron hole pairs in the composite catalyst, expands the light absorption range of the material, enhances the photocatalytic activity of the material, and is applied to photocatalytic reduction of CO 2 Research in the field.
Disclosure of Invention
The invention adopts the technical means of solvothermal to successfully prepare the SnS 2 /Pt 3 A Co composite photocatalyst; aims to solve the problems of high recombination rate of photon-generated carriers, narrow photoresponse range and the like.
The present invention achieves the above-described object by the following technical means.
SnS 2 /Pt 3 The preparation method of the Co composite photocatalyst comprises the following steps:
(1) Preparation of Pt 3 Co precursor:
adding the platinum chloride solution and the cobalt chloride solution into a beaker in sequence, stirring, and then adding NaBH 4 Adding into the above mixed solution until the color of the solution changes from light yellow to black, standing the obtained solution at room temperature, washing with deionized water and ethanol for multiple times after standing to obtain Pt 3 A Co gel precursor; then diluting with deionized water to obtain Pt 3 The Co gel solution is reserved;
(2)SnS 2 /Pt 3 preparing a Co composite photocatalyst:
adding stannic chloride pentahydrate (SnCl) 4 ·5H 2 O) is dissolved in the mixed solution of glycol and deionized water, then L-cysteine and sodium dodecyl benzene sulfonate are added and stirred evenly to prepare tin disulfide; adding a certain amount of Pt 3 Co gel solutionAnd (2) forming a mixed solution, adding the mixed solution into a reaction kettle for hydrothermal reaction, naturally cooling to room temperature, washing, centrifuging and drying a product after the reaction to obtain SnS 2 /Pt 3 A Co composite photocatalyst.
In the step (1), the concentration of the platinum chloride solution is 1g/L, the concentration of the cobalt chloride solution is 1g/L, and NaBH is added 4 The concentration of the solution is 0.1M, the stirring time is 1h, the standing time is 3h 3 The concentration of the Co gel solution was 2mM.
In the step (2), the dosage ratio of the stannic chloride pentahydrate, the glycol, the deionized water, the L-cysteine and the sodium dodecyl benzene sulfonate is 0.0877g:15ml: 0.5645g.
In the step (2), the tin disulfide and Pt 3 Pt in Co gel solution 3 The mass ratio of Co is 1: (0.5-4).
In the step (2), the tin disulfide and Pt 3 Pt in Co gel solution 3 The mass ratio of Co is 1:3.2.
in the step (2), the temperature of the hydrothermal treatment is 150-180 ℃; the hydrothermal treatment time was 10h.
The SnS of the invention 2 /Pt 3 The morphology of Co is a sheet-particle structure, and the size of Co is 2-3nm.
Pt prepared by the invention 3 The application of the Co composite photocatalyst in reducing carbon dioxide.
In the technical scheme, the dosage of the deionized water can completely dissolve the soluble solid.
The invention has the beneficial effects that:
(1) The invention uses SnS 2 /Pt 3 The Co composite material has higher visible light response capability, and passes through Pt 3 Co is an electric conductor, the electron transmission is accelerated, the plasma resonance effect enables the SnS to have more hot electrons, and the SnS is improved to a greater extent 2 /Pt 3 Efficiency of Co photocatalytic reduction of carbon dioxide.
(2) Prepared SnS 2 Ultra-thin two-dimensional structure, pt 3 Co is uniformly dispersed in SnS 2 In addition, more reaction sites are provided, so that moreCan participate in the photoreduction of carbon dioxide.
(3) The invention can prepare SnS through convenient hydrothermal 2 /Pt 3 The Co composite photocatalyst takes the alloy as a bridge, so that the transmission of photon-generated carriers is accelerated, and the composite material is a high-efficiency and stable photocatalyst.
(4) The invention realizes the purpose of using SnS 2 /Pt 3 The Co nano composite material is used as a photocatalyst, 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 aim of converting the carbon dioxide gas into organic fuel is fulfilled.
Drawings
In FIG. 1, a is SnS prepared in example 1 2 XRD pattern of (a), b is SnS prepared in example 1 2 /Pt 3 XRD pattern of Co, c is SnS prepared in example 2 2 /Pt 3 XRD pattern of Co, d is SnS prepared in example 3 2 /Pt 3 XRD pattern of Co, e is SnS prepared in example 4 2 /Pt 3 XRD pattern of Co.
In FIG. 2, a is SnS prepared in example 1 2 DRS map of (a), b is SnS prepared in example 1 2 /Pt 3 DRS map of Co, c is SnS prepared in example 2 2 /Pt 3 DRS plot of Co, d is SnS prepared in example 3 2 /Pt 3 DRS map of Co, e is SnS prepared in example 4 2 /Pt 3 DRS plot of Co.
FIG. 3 is SnS prepared in example 3 2 /Pt 3 TEM image of Co 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 100ml of deionized water solution were added to the photoreactor, and CO was introduced at a large flow rate 2 Injecting CO at a certain pressure after the gas in the kettle is exhausted 2 A gas. The custom xenon lamp was turned on under magnetic stirring and samples were analyzed at 1h intervals. Finally, CO is obtained through calculation 2 Gas reduction CO yield.
Example 1:
(1)Pt 3 preparing a Co gel precursor:
adding 1g/L platinum chloride solution and 1g/L cobalt chloride solution into a beaker in sequence, stirring for 1h, and then adding NaBH 4 (0.1M) adding into the above mixed solution until the color of the solution changes from light yellow to black, standing the obtained solution at room temperature (3 h), washing with deionized water and ethanol for multiple times to obtain Pt 3 A Co gel precursor;
(2)SnS 2 /Pt 3 preparing a Co composite photocatalyst:
0.0877g of SnCl was weighed out 4 ·5H 2 Placing O (stannic chloride pentahydrate) into a glass beaker, adding 10mL of deionized water and 20mL of ethylene glycol to completely dissolve the O, magnetically stirring, adding 0.2423g of L-cysteine and 0.5645g of sodium dodecyl benzene sulfonate to generate white precipitate, and continuously stirring for 0.5h; 1ml of Pt 3 A Co (2 mM) precursor was added thereto and mixed well, and the resulting suspension was poured into a 50ml reaction vessel and heated at 160 ℃ for 10 hours. Washing, centrifuging and drying to obtain SnS 2 /Pt 3 A Co composite photocatalyst;
(3) Taking 0.02g of catalyst and 100ml of deionized water from the sample in the step (2), adding the catalyst and the deionized water into a photoreactor, and introducing CO at a large flow rate 2 Injecting CO at a certain pressure after the gas in the kettle is exhausted 2 A gas. The custom xenon lamp was turned on under magnetic stirring and samples were analyzed at 1h intervals. After 5h of irradiation, CO was calculated 2 The gas reduced CO yield was 24.5. Mu. Mol/g.
Example 2:
(1)Pt 3 preparation of Co gel precursor:
adding 1g/L platinum chloride solution and 1g/L cobalt chloride solution into a beaker in sequence, stirring for 1h, and then adding NaBH 4 (0.1M) adding the above mixtureStanding the obtained solution at room temperature (3 h) until the color of the solution changes from light yellow to black, and washing with deionized water and ethanol for multiple times to obtain Pt 3 A Co gel precursor;
(2)SnS 2 /Pt 3 preparing a Co composite photocatalyst:
0.0877g SnCl was weighed out 4 ·5H 2 Placing O (stannic chloride pentahydrate) into a glass beaker, adding 10mL of deionized water and 20mL of ethylene glycol to completely dissolve the O, magnetically stirring, adding 0.2423g of L-cysteine and 0.5645g of sodium dodecyl benzene sulfonate to generate white precipitate, and continuously stirring for 0.5h; 3ml of Pt 3 A Co (2 mM) precursor was added thereto and mixed well, and the resulting suspension was poured into a 50ml reaction vessel and heated at 160 ℃ for 10 hours. Washing, centrifuging and drying to obtain SnS 2 /Pt 3 A Co composite photocatalyst;
(3) Taking 0.02g of catalyst and 100ml of deionized water from the sample in the step (2), adding the catalyst and the deionized water into a photoreactor, and introducing CO at a large flow rate 2 Injecting CO at a certain pressure after the gas in the kettle is exhausted 2 A gas. The custom xenon lamp illumination was turned on under magnetic stirring and samples were analyzed at 1h intervals. After 5h of irradiation, the CO2 gas reduction CO was calculated to be 40.4. Mu. Mol/g.
Example 3:
(1)Pt 3 preparation of Co gel precursor:
adding 1g/L platinum chloride solution and 1g/L cobalt chloride solution into a beaker in sequence, stirring for 1h, and then adding NaBH 4 (0.1M) adding into the above mixed solution until the color of the solution changes from light yellow to black, standing the obtained solution at room temperature (3 h), washing with deionized water and ethanol for multiple times to obtain Pt 3 A Co gel precursor;
(2)SnS 2 /Pt 3 preparing a Co composite photocatalyst:
0.0877g of SnCl was weighed out 4 ·5H 2 Placing O (stannic chloride pentahydrate) into a glass beaker, adding 10mL of deionized water and 20mL of ethylene glycol to completely dissolve the O, magnetically stirring, adding 0.2423g of L-cysteine and 0.5645g of sodium dodecyl benzene sulfonate to generate white precipitate,continuously stirring for 0.5h; mixing 5ml of Pt 3 Co (2 mM) precursor was added thereto and mixed well, and the resulting suspension was poured into a 50ml reaction vessel and heated at 160 ℃ for 10 hours. Washing, centrifuging and drying to obtain SnS 2 /Pt 3 A Co composite photocatalyst;
(3) Taking 0.02g of catalyst and 100ml of deionized water from the sample in the step (2), adding the catalyst and the deionized water into a photoreactor, and introducing CO at a large flow rate 2 After the gas in the kettle is exhausted, CO with a certain pressure is injected 2 A gas. The custom xenon lamp was turned on under magnetic stirring and samples were analyzed at 1h intervals. After 5h of irradiation, CO was calculated 2 The gas reduced CO was 92.3. Mu. Mol/g.
Example 4:
(1)Pt 3 preparing a Co gel precursor:
adding 1g/L platinum chloride solution and 1g/L cobalt chloride solution into a beaker in sequence, stirring for 1h, and then adding NaBH 4 (0.1M) is added into the mixed solution until the color of the solution is changed from light yellow to black, the obtained solution is stood at room temperature (3 h), and is washed by deionized water and ethanol for a plurality of times to obtain Pt 3 A Co gel precursor;
(2)SnS 2 /Pt 3 preparing a Co composite photocatalyst:
0.0877g of SnCl was weighed out 4 ·5H 2 Placing O (stannic chloride pentahydrate) into a glass beaker, adding 10mL of deionized water and 20mL of ethylene glycol to completely dissolve the O, magnetically stirring, adding 0.2423g of L-cysteine and 0.5645g of sodium dodecyl benzene sulfonate to generate white precipitate, and continuously stirring for 0.5h; mixing 7ml of Pt 3 Co (2 mM) precursor was added thereto and mixed well, and the resulting suspension was poured into a 50ml reaction vessel and heated at 160 ℃ for 10 hours. Washing, centrifuging and drying to obtain SnS 2 /Pt 3 A Co composite photocatalyst;
(3) Taking 0.02g of catalyst and 100ml of deionized water from the sample in the step (2), adding the catalyst and the deionized water into a photoreactor, and introducing CO at a large flow rate 2 Injecting CO at a certain pressure after the gas in the kettle is exhausted 2 A gas. The custom xenon lamp was turned on under magnetic stirring and samples were analyzed at 1h intervals. After 5h of irradiation, CO was calculated 2 The gas reduced CO was 52.6. Mu. Mol/g.
FIG. 1 is an XRD pattern of the photocatalyst, showing SnS clearly 2 All diffraction peaks matched well with the standard card, indicating that the desired material was successfully prepared.
FIG. 2 is a DRS plot of a photocatalyst showing, with clarity, alloy-modified SnS 2 The photocatalyst widens the light absorption range. SnS 2 At Pt 3 The absorption range of light under the modification effect of the Co alloy is 385-720 nm, which shows that Pt 3 The Co alloy can broaden the light absorption range of the semiconductor.
FIG. 3 shows SnS 2 /Pt 3 TEM image of Co composite photocatalyst, from which SnS can be seen 2 /Pt 3 The morphology of Co is a sheet-particle structure, and the size of Co is 2-3nm.
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 (5)

1. Pt 3 Atomic layer SnS modified by Co alloy 2 The preparation method of the composite photocatalyst is characterized in that,
(1) Preparation of Pt 3 Co precursor:
adding the platinum chloride solution and the cobalt chloride solution into a beaker in sequence, stirring, and then adding NaBH 4 Standing the obtained solution at room temperature until the color of the solution changes from light yellow to black, and washing the solution with deionized water and ethanol for multiple times after standing to obtain Pt 3 A Co gel precursor; then diluting with deionized water to obtain Pt 3 The Co gel solution is reserved;
wherein the concentration of the platinum chloride solution is 1g/L, the concentration of the cobalt chloride solution is 1g/L, and NaBH is added 4 The concentration of the solution is 0.1M, the stirring time is 1h, the standing time is 3h, and Pt 3 The concentration of the Co gel solution is 2 mM;
（2）SnS 2 /Pt 3 preparing a Co composite photocatalyst:
SnCl pentahydrate 4 •5H 2 Dissolving O in a mixed solution of ethylene glycol and deionized water, then adding L-cysteine and sodium dodecyl benzene sulfonate, and uniformly stirring to prepare tin disulfide; adding a certain amount of Pt 3 Co gel solution to form mixed solution, the tin disulfide and Pt 3 Pt in Co gel solution 3 The mass ratio of Co is 1: (0.5 to 4); adding the mixed solution into a reaction kettle for hydrothermal reaction at 150-180 ℃ for 10h, naturally cooling to room temperature, washing, centrifuging and drying a product after the reaction to obtain SnS 2 /Pt 3 And (3) a Co composite photocatalyst.
2. The method according to claim 1, wherein in the step (2), the tin chloride pentahydrate, the ethylene glycol, the deionized water, the L-cysteine, and the sodium dodecylbenzenesulfonate are used in a ratio of 0.0877g:15 15mL, 0.2423g:0.5645g.
3. The method of claim 1, wherein in step (2), the tin disulfide is reacted with Pt 3 Pt in Co gel solution 3 The mass ratio of Co is 1:3.2.
4. pt 3 Co alloy modified atomic layer SnS 2 The composite photocatalyst is characterized by being prepared by the preparation method of any one of claims 1 to 3, having a flake-added particle structure and a size of 2 to 3nm.
5. Subjecting the Pt of claim 4 to 3 Co alloy modified atomic layer SnS 2 Use of a composite photocatalyst for the reduction of carbon dioxide.
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CN104923263A (en) * 2015-05-20 2015-09-23 湖北大学 Composite photocatalytic water splitting catalyst and preparation method thereof
CN110252346A (en) * 2019-05-29 2019-09-20 江苏大学 A kind of MoS2/SnS2The preparation method and purposes of/r-GO composite photo-catalyst
CN111203256A (en) * 2020-02-18 2020-05-29 江苏大学 SnS2/Au/g-C3N4Preparation method and application of composite photocatalyst

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