CN114985004A - Cadmium indium sulfide/PDDA/NiFe-LDH photocatalytic composite material and preparation method and application thereof - Google Patents
Cadmium indium sulfide/PDDA/NiFe-LDH photocatalytic composite material and preparation method and application thereof Download PDFInfo
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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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/06—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides containing polymers
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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
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/043—Sulfides with iron group metals or platinum group metals
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- B01J35/39—
-
- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/02—Impregnation, coating or precipitation
- B01J37/03—Precipitation; Co-precipitation
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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
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- 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 invention discloses two-dimensional CdIn 2 S 4 The two-dimensional CdIn is prepared by a simple low-temperature reflux method, a coprecipitation method and a direct stirring method 2 S 4 PDDA/two-dimensional NiFe-LDH photocatalytic composite material and prepared two-dimensional CdIn 2 S 4 the/PDDA/two-dimensional NiFe-LDH photocatalytic composite materials have specific two-dimensional CdIn 2 S 4 The material has higher carbon dioxide reduction performance. In addition, the prepared two-dimensional CdIn 2 S 4 the/PDDA/two-dimensional NiFe-LDH photocatalytic composite material is prepared in visible light (lambda)>420 nm) illuminationHas higher stability when irradiated.
Description
Technical Field
The invention belongs to the technical field of photocatalysis, and particularly relates to two-dimensional CdIn 2 S 4 A PDDA/two-dimensional NiFe-LDH photocatalytic composite material, a preparation method and application thereof.
Background
With the drastic change of climate, a series of serious consequences such as melting of glaciers, rising of sea level, drought and massive whitening of coral reefs appear, indicating that global warming is in progress and will have a great influence on environmental problems. From an energy perspective, this dangerous climate change is largely due to global energy imbalances caused by the large carbon dioxide emissions of fossil fuels that are continuously consumed by humans. One of the best approaches to address the growing energy demand and climate change problems is the reduction of artificial photocatalytic carbon dioxide to valuable chemical feedstocks. Since pioneering work in 1979 by Inoue et al, 1979, efforts have been directed to the development of photocatalytic materials for the photoreduction of carbon dioxide to chemical fuels, such as CO, methane, methanol, or formic acid. To date, various photocatalytic materials have proven useful for the photocatalytic conversion of carbon dioxide, including various metal oxides, sulfides, phosphides, titanium-containing molecular sieves, metal organic frameworks, and polymeric semiconductors. As AB 2 X 4 One-member, ternary sulfide CdIn of group semiconductors 2 S 4 Has a proper band gap (2.00-2.37 eV), and is a potential photocatalyst candidate material under the irradiation of visible light. Previous studies have shown that CdIn 2 S 4 In the photocatalysis of hydrogen evolution, bacterial inactivation, pollutant degradation and CO 2 Reduction, etc. The LDHs have unique layered structure, flexible chemical composition, adjustable electronic band structure and stronger CO 2 The adsorption capacity provides an ideal platform for developing various heterostructure photocatalysts. In view of scarcity of noble metals and their high price, development of a new preparation method to achieve synthesis of a sample with high catalytic activity while minimizing the amount of noble metal promoter used, or development of an alternative non-noble metal promoter has been forced in the eyebrowAnd (5) eyelash beating. Meanwhile, the problem of how to inhibit the photo-corrosion of the cadmium indium sulfide and how to inhibit the photo-generated carriers from being rapidly compounded also becomes the difficulty and challenge of important research work.
Disclosure of Invention
The invention aims to provide the two-dimensional CdIn with the regular shape and the simple and environment-friendly production process 2 S 4 A PDDA/two-dimensional NiFe-LDH photocatalytic composite material, a preparation method thereof and application of the photocatalytic composite material in carbon dioxide reduction.
In order to achieve the purpose, the invention adopts the following technical scheme:
two-dimensional CdIn 2 S 4 The preparation method of the/PDDA/two-dimensional NiFe-LDH photocatalytic composite material comprises the following steps:
(1) simple low-temperature reflux method for preparing two-dimensional CdIn 2 S 4 Nanosheet: adding Cd (CH) 3 COO) 2 ·2H 2 O and InCl 3 Mixing, adding deionized water, and stirring for 30min (rotation speed of 800 rmp) to obtain a mixed solution. Subsequently, an excess amount of Thioacetamide (TAA) was added to the above mixed solution, and further stirred for 30min (rotation speed 800 rmp). The solution was then heated to a certain temperature by a water bath and incubated for a certain period of time with vigorous stirring (1000 rmp). Centrifuging (rotation speed of 10000 rmp, time of 5 min), collecting precipitate, washing with deionized water, and repeating the centrifuging and washing steps for 3 times to remove excessive impurities. Finally, placing the collected yellow precipitate in a vacuum drying oven at 60 ℃ for 12 hours to obtain the two-dimensional CdIn 2 S 4 Nanosheets (CIS NSs);
(2) preparation of two-dimensional CdIn by direct stirring method 2 S 4 PDDA nanosheet: CISNSs (100 mg) was added to 10mL of PDDA solution at a concentration of x (x =2, 5, 7, 10, 12 mg/mL) and stirred vigorously (1000 rmp) for 1 hour. Then, the mixture was centrifuged (rotation speed: 10000 rmp for 5 min), and thus obtained PDDA-modified cissns (CP-x) were thoroughly washed with deionized water to remove residual free PDDA adsorbed on the surface. Finally, the powder obtained is placed under vacuum at 60 ℃Drying for 12 hours to obtain the two-dimensional CdIn 2 S 4 a/PDDA nanosheet (CP-x);
(3) preparing a two-dimensional NiFe-LDH nano sheet by a direct coprecipitation method: mixing Ni (NO) 3 ) 2 ·6H 2 O and Fe (NO) 3 ) 3 ·9H 2 O, mixing and adding deionized water; the pH of the mixed solution was adjusted to 9.0 with 0.5M NaOH solution at room temperature, and a tan precipitate appeared. Then, vigorously stirring the yellow brown precipitate at room temperature for 24 hours; then filtering the generated precipitate, and washing with distilled water for multiple times to remove redundant soluble ions; finally, drying the washed precipitate in an oven at 80 ℃ overnight, and grinding the precipitate into powder to obtain two-dimensional NiFe-LDH nano sheets;
(4) CdIn preparation by direct stirring method 2 S 4 The composite material of/PDDA/NiFe-LDH: mixing 50 mg of CP-x powder with y mg of NiFe-LDH powder, and adding 30 mL of deionized water; stirring the mixed solution at room temperature for 1 h; centrifuging the stirred mixed solution, then putting the mixed solution into an oven for drying, and finally grinding the dried mixed solution into powder to obtain the CdIn 2 S 4 the/PDDA/NiFe-LDH powder sample.
Further, step (1), mixing Cd (CH) in the solution 3 COO) 2 ·2H 2 O、InCl 3 And Thioacetamide (TAA) at concentrations of 0.006 mol/L, 0.012 mol/L, and 0.032mol/L, respectively.
Further, in the step (1), the temperature of the mixed solution is heated to 100 ℃, and the mixed solution is kept for 12 hours.
Further, in step (2), the PDDA solution is prepared by using 0.5M NaCl solution, and the PH is 10.
Further, in the step (3), Ni (NO) 3 ) 2 ·6H 2 O and Fe (NO) 3 ) 3 ·9H 2 The concentrations of O were 1.6 mol/L and 0.33 mol/L, [ Ni ] 2+ + Fe 3+ ]= 0.2M (Ni in preparation of NiFe-LDH) 2+ And Fe 3+ Total ion concentration).
Further, in step (3), the titration solution is washed with distilled water several times to remove excess soluble ions until the pH of the titration solution reaches 7.
Further, in step (4), y is 2, 5, 7, 10, 15, preferably not more than 50% of CP-x mass, i.e. y ≦ 50% M CP-x . A preferred value is y = 7.
As the loading of LDH is increased, on one hand, the light absorption performance of CIS can be enhanced, and on the other hand, more CO can be provided 2 Adsorption sites, but when the loading of LDH is too high, the light absorption properties of CIS are covered, thereby decreasing its carbon dioxide reduction properties. While at a preferred value of 7, CdIn 2 S 4 the/PDDA/NiFe-LDH photocatalytic composite material has the highest carbon dioxide reduction performance.
The two-dimensional CdIn prepared by the invention 2 S 4 the/PDDA/two-dimensional NiFe-LDH photocatalytic composite material is used for visible light (lambda)>420 nm) for 2h for carbon dioxide reduction.
The carbon dioxide reduction comprises the following specific steps:
5 mL of acetonitrile, 3 mL of water and 2 mL of triethanolamine are placed in a reactor, and 10 mg of CdIn is added 2 S 4 The composite photocatalyst is prepared by performing vacuum pumping on a/PDDA/NiFe-LDH composite photocatalyst for 2 min, and introducing CO 2 Gas is sealed for 5 min, and is exposed to visible light (lambda)>420 nm) for 2 hours, taking 1 mL of gas for gas chromatography, and performing qualitative and quantitative analysis through retention time and peak area.
The invention adopts the method to prepare the two-dimensional CdIn 2 S 4 The material can enable CdIn to be under the conditions of simulating solar irradiation and adding a sacrificial agent 2 S 4 The photogenerated electrons on the NiFe-LDH are combined with the photogenerated holes of the NiFe-LDH in a Type-II charge mode in a transmission mode, and the photogenerated holes on the NiFe-LDH are captured by a sacrificial agent, namely CdIn 2 S 4 The photoproduction electrons are further transmitted to NiFe-LDH, the effective separation of the photoproduction electron-hole pairs and the introduction of PDDA prevent CdIn on the one hand 2 S 4 Of the photogenerated hole pairs CdIn 2 S 4 Self-oxidation to inhibit CdIn 2 S 4 For the purpose of photo-etching, on the other hand, the introduction of a promoter NiFe-LDH not only provides more CO 2 The adsorption sites also improve the reduction performance of carbon dioxide, and finally the two-dimensional CdIn is obtained 2 S 4 the/PDDA/two-dimensional NiFe-LDH photocatalytic composite material has more excellent carbon dioxide reduction performance and stability. In addition, the invention also has the following beneficial effects:
(1) the invention relates to two-dimensional CdIn 2 S 4 the/PDDA/two-dimensional NiFe-LDH photocatalytic composite material is used for a carbon dioxide reduction system, has higher catalytic efficiency, and the prepared two-dimensional CdIn 2 S 4 the/PDDA/two-dimensional NiFe-LDH photocatalytic composite material has specific two-dimensional CdIn 2 S 4 The material has higher carbon dioxide reduction performance and is easy to recover, which is beneficial to the sustainable development of environment and energy,
(2) two-dimensional CdIn 2 S 4 the/PDDA/two-dimensional NiFe-LDH photocatalytic composite material has the advantages of good cycle performance, simple production process, environmental friendliness and easiness in recovery.
Drawings
Fig. 1 is SEM images of different materials, respectively: (A) CdIn 2 S 4 SEM picture of (1); (B) CdIn 2 S 4 SEM image of/PDDA composite material; (C) CdIn 2 S 4 SEM picture of/PDDA/NiFe-LDH composite material;
FIG. 2 is an X-ray diffraction pattern of different materials; c is CdIn 2 S 4 CP is CdIn 2 S 4 the/PDDA composite material has CPL of CdIn 2 S 4 a/PDDA/NiFe-LDH composite material;
FIG. 3 is an ultraviolet-visible diffuse reflectance spectrum of different materials; c is CdIn 2 S 4 CP is CdIn 2 S 4 The CPL of the/PDDA composite material is CdIn 2 S 4 a/PDDA/NiFe-LDH composite material;
FIG. 4 is a graph of carbon dioxide reduction activity of different materials;
c is CdIn 2 S 4 (ii) a CP is CdIn 2 S 4 the/PDDA composite material, CP-7, represents: 100 mg CdIn 2 S 4 Preparing a binary composite sample with 20 mL of 7 mg/mL PDDA solution, and so on; CPL is CdIn 2 S 4 /PDDA/NiFe-LDH composite materialCPL-7 denotes: a ternary composite sample prepared from 50 mg of CP-x and 7 mg of NiFe-LDH, and the like;
FIG. 5 is a comparison graph of cycle experiments of different materials under simulated sunlight irradiation;
c is CdIn 2 S 4 CP is CdIn 2 S 4 the/PDDA composite material has CPL of CdIn 2 S 4 The composite material of/PDDA/NiFe-LDH, CPL-0.06 shows: LDH/CP =0.14, and so on.
Detailed Description
Two-dimensional CdIn 2 S 4 The preparation method of the/PDDA/two-dimensional NiFe-LDH photocatalytic composite material comprises the following steps:
(1) simple low-temperature reflux method for preparing two-dimensional CdIn 2 S 4 Nanosheet: adding Cd (CH) 3 COO) 2 ·2H 2 O and InCl 3 Mixing, adding deionized water, and stirring for 30min (rotation speed of 800 rmp) to obtain a mixed solution. Subsequently, an excess amount of Thioacetamide (TAA) was added to the above mixed solution, and further stirred for 30min (rotation speed 800 rmp). The solution was then heated to a certain temperature by a water bath and incubated for a certain period of time with vigorous stirring (1000 rmp). Centrifuging (rotation speed of 10000 rmp, time of 5 min), collecting precipitate, washing with deionized water, and repeating the centrifuging and washing steps for 3 times to remove excessive impurities. Finally, placing the collected yellow precipitate in a vacuum drying oven at 60 ℃ for 12 hours to obtain the two-dimensional CdIn 2 S 4 Nanosheets (CIS NSs);
(2) preparation of two-dimensional CdIn by direct stirring method 2 S 4 PDDA nanosheet: CISNSs (100 mg) was added to 10mL of PDDA solution at a concentration of x (x =2, 5, 7, 10, 12 mg/mL) and stirred vigorously (1000 rmp) for 1 hour. Then, the mixture was centrifuged (rotation speed: 10000 rmp for 5 min), and thus obtained PDDA-modified cissns (CP-x) were thoroughly washed with deionized water to remove residual free PDDA adsorbed on the surface. Finally, the obtained powder is dried in vacuum at 60 ℃ for 12 hours to obtain the two-dimensional CdIn 2 S 4 a/PDDA nanosheet (CP-x);
(3) preparing a two-dimensional NiFe-LDH nano sheet by a direct coprecipitation method: mixing Ni (NO) 3 ) 2 ·6H 2 O and Fe (NO) 3 ) 3 ·9H 2 O, mixing and adding deionized water; the pH of the mixed solution was adjusted to 9.0 with 0.5M NaOH solution at room temperature, and a tan precipitate appeared. Then, vigorously stirring the yellow brown precipitate at room temperature for 24 hours; then filtering the generated precipitate, and washing the precipitate for multiple times by using distilled water to remove redundant soluble ions; finally, drying the washed precipitate in an oven at 80 ℃ overnight, and grinding the precipitate into powder to obtain two-dimensional NiFe-LDH nano sheets;
(4) CdIn preparation by direct stirring method 2 S 4 The composite material of/PDDA/NiFe-LDH: mixing 50 mg of CP-x powder with y mg of NiFe-LDH powder, and adding 30 mL of deionized water; stirring the mixed solution at room temperature for 1 h; centrifuging the stirred mixed solution, then putting the mixed solution into an oven for drying, and finally grinding the dried mixed solution into powder to obtain the CdIn 2 S 4 Powder sample of/PDDA/NiFe-LDH (CPL-y).
Wherein the dosage ratio of the CP-x to the NiFe-LDH is as follows: NiFe-LDH/CP-x =0.04-0.3 (e.g. 0.04, 0.1, 0.14, 0.2, 0.3), preferably NiFe-LDH/CP-x = 0.14.
The present invention is further illustrated by the following specific examples, but the scope of the present invention is not limited to the following examples.
Example 1
Preparation of two-dimensional CdIn 2 S 4 Nano meter
1.5 mmol of Cd (CH) 3 COO) 2 ·2H 2 O and 3 mmol InCl 3 After mixing, 250 mL of deionized water was added and stirred for 30min (rotation speed 800 rmp) to obtain a mixed solution. Subsequently, an excess of thioacetamide (TAA, 8 mmol) was added to the above mixed solution, and further stirred for 30min (rotation speed 800 rmp). The solution was then heated to 100 ℃ by means of a water bath and incubated for 12h with vigorous stirring (1000 rmp). Centrifuging (rotation speed 10000 rmp for 5 min), collecting precipitate, washing with deionized water, and repeating the centrifuging and washing steps for 3 times to remove excessive impurities. Finally collecting yellowPlacing the color precipitate in a vacuum drying oven at 60 ℃ for 12 hours to obtain the two-dimensional CdIn 2 S 4 Nanometer Slice (CISNSs)
Taking 10 mg of prepared CdIn 2 S 4 The sample was placed in a reactor containing a mixed solution of 5 mL acetonitrile, 3 mL water and 2 mL triethanolamine, followed by evacuation for 2 min, followed by CO introduction 2 The gas is sealed and placed under visible light for 2 hours, and the yield of carbon dioxide reduced into carbon monoxide and the yield of competing product hydrogen are respectively 1.593 mu mol.L -1 ·h -1 And 0.595 mmol.L -1 ·h -1 。
Example 2
Preparation of two-dimensional CdIn 2 S 4 /PDDA composite material
CIS NSs (100 mg) was added to 10mL of PDDA solution at a concentration of x (x =2, 5, 7, 10, 12 mg/mL) and vigorously stirred (1000 rmp rpm) for 1 hour. Then, the mixture was centrifuged (rotation speed: 10000 rmp for 5 min), and thus obtained PDDA-modified cissns (CP-x) were thoroughly washed with deionized water to remove residual free PDDA adsorbed on the surface. Finally, the obtained powder is dried in vacuum at 60 ℃ for 12 hours to obtain the two-dimensional CdIn 2 S 4 a/PDDA nanosheet (CP-x).
10 mg of the prepared CP-7 sample was placed in a reactor containing a mixed solution of 5 mL of acetonitrile, 3 mL of water and 2 mL of triethanolamine, followed by evacuation for 2 min and subsequent CO introduction 2 The gas is sealed and placed under visible light for 2 hours, and the yield of carbon dioxide reduced into carbon monoxide and the yield of competing product hydrogen are 3.984 mu mol.L respectively -1 ·h -1 And 0.399 mmol. multidot.L -1 ·h -1 。
Example 3
Preparation of two-dimensional NiFe-LDH
0.16M Ni (NO) 3 ) 2 ·6 H 2 O and 0.033M Fe (NO) 3 ) 3 ·9 H 2 O, mixing, and adding 100mL of deionized water; the pH of the mixed solution was adjusted to 9.0 with 0.5M NaOH solution at room temperature, and a tan precipitate appeared. Then, the yellow brown precipitate is placed in a chamberStirring strongly for 24 h at the temperature; then filtering the generated precipitate, and washing with distilled water for multiple times to remove redundant soluble ions until the pH value of the titration solution reaches 7; and finally, drying the washed precipitate in an oven at 80 ℃ overnight, and grinding the precipitate into powder to obtain the two-dimensional NiFe-LDH nanosheet.
Example 4
Preparation of two-dimensional CdIn 2 S 4 /PDDA/NiFe-LDH composite material
Mixing 50 mg of CP-x powder with y mg of NiFe-LDH powder, and adding 30 mL of deionized water; stirring the mixed solution at room temperature for 1 h; centrifuging the stirred mixed solution, then putting the mixed solution into an oven for drying, and finally grinding the dried mixed solution into powder to obtain the CdIn 2 S 4 Powder sample of/PDDA/NiFe-LDH (CPL-y). .
A10 mg sample of the prepared CPL-7 (wherein CP-x is CP-7) was placed in a reactor containing a mixed solution of 5 mL acetonitrile, 3 mL water and 2 mL triethanolamine, and then evacuated for 2 min, followed by introduction of CO 2 The gas is sealed and placed under simulated sunlight for 2 hours, and the yield of carbon dioxide reduced into carbon monoxide and the yield of competing product hydrogen are 12.400 mu mol.L respectively -1 ·h -1 And 0.960 mmol. multidot.L -1 ·h -1 。
The results of the experiments relating to the materials prepared according to the present invention are shown in one of figures 1 to 5.
As can be seen from the SEM image of fig. 1, by comparing the a and B images, the surface of the CIS becomes significantly rough and the degree of agglomeration of the overall morphology is greater, which demonstrates that the PDDA can be successfully loaded on the CIS; by comparing the three diagrams of B, C and D, the CP and the NiFe-LDH with two flaky structures with different thicknesses are stacked together, and the success of material synthesis is also proved.
FIG. 2, X-ray diffraction patterns of different materials show that the synthesized CIS nanosheet has a strong (002) peak, and in addition, the (101) peak of the CIS can be seen after PDDA and NiFe-LDH are loaded, which further proves the success of material synthesis.
FIG. 3, ultraviolet-visible diffuse reflectance spectra of different materials show that PDDA and NiFe-LDH loading can effectively enhance the visible light absorption performance of CIS.
FIG. 4, a graph showing the carbon dioxide reduction activity of different materials, shows that PDDA and NiFe-LDH were loaded to effectively enhance the carbon dioxide reduction performance of CIS.
Fig. 5 is a comparison of carbon dioxide reduction cycle experiments of different materials under visible light irradiation, which illustrates that the composite material has higher carbon dioxide reduction activity and cycle stability under the visible light irradiation of different materials.
Example 5
Two-dimensional CdIn 2 S 4 Preparing a/PDDA/two-dimensional NiFe-LDH photocatalytic composite material:
(1) simple low-temperature reflux method for preparing two-dimensional CdIn 2 S 4 Nanosheet: adding Cd (CH) 3 COO) 2 ·2H 2 O and InCl 3 Mixing, adding deionized water, and stirring for 30min (rotation speed of 800 rmp) to obtain a mixed solution. Subsequently, an excess amount of Thioacetamide (TAA) was added to the above mixed solution, and further stirred for 30min (rotation speed 800 rmp). The solution was then heated to a certain temperature by a water bath and incubated for a certain period of time with vigorous stirring (1000 rmp). Centrifuging (rotation speed of 10000 rmp, time of 5 min), collecting precipitate, washing with deionized water, and repeating the centrifuging and washing steps for 3 times to remove excessive impurities. Finally, placing the collected yellow precipitate in a vacuum drying oven at 60 ℃ for 12 hours to obtain the two-dimensional CdIn 2 S 4 Nanosheets (CIS NSs);
(2) preparation of two-dimensional CdIn by direct stirring method 2 S 4 PDDA nano-sheet: CISNSs (100 mg) was added to 10mL of PDDA solution at a concentration of x (x =2, 5, 7, 10, 12 mg/mL) and stirred vigorously (1000 rmp) for 1 hour. Then, the mixture was centrifuged (rotation speed: 10000 rmp for 5 min), and the PDDA-modified CIS NSs (CP-x) thus obtained were thoroughly washed with deionized water to remove residual free PDDA adsorbed on the surface. Finally, the obtained powder is dried in vacuum at 60 ℃ for 12 hours to obtain the two-dimensional CdIn 2 S 4 a/PDDA nanosheet (CP-x);
(3) preparation of two-dimensional NiFe-LDH nano-grade by direct coprecipitation methodSheet: mixing Ni (NO) 3 ) 2 ·6H 2 O and Fe (NO) 3 ) 3 ·9H 2 O, mixing and adding deionized water; the pH of the mixed solution was adjusted to 9.0 with 0.5M NaOH solution at room temperature, and a tan precipitate appeared. Then, vigorously stirring the yellow brown precipitate at room temperature for 24 hours; then filtering the generated precipitate, and washing the precipitate for multiple times by using distilled water to remove redundant soluble ions; finally, drying the washed precipitate in an oven at 80 ℃ overnight, and grinding the precipitate into powder to obtain two-dimensional NiFe-LDH nano sheets;
(4) CdIn preparation by direct stirring method 2 S 4 The composite material of/PDDA/NiFe-LDH: mixing 50 mg of CP-x powder with y mg of NiFe-LDH powder, and adding 30 mL of deionized water; stirring the mixed solution at room temperature for 1 h; centrifuging the stirred mixed solution, then putting the mixed solution into an oven for drying, and finally grinding the dried mixed solution into powder to obtain the CdIn 2 S 4 the/PDDA/NiFe-LDH powder sample.
Wherein, the dosage ratio of the NiFe-LDH to the CP-x is 0.14.
Example 6
Two-dimensional CdIn 2 S 4 Preparing a/PDDA/two-dimensional NiFe-LDH photocatalytic composite material:
(1) simple low-temperature reflux method for preparing two-dimensional CdIn 2 S 4 Nanosheet: adding Cd (CH) 3 COO) 2 ·2H 2 O and InCl 3 Mixing, adding deionized water, and stirring for 30min (rotation speed of 800 rmp) to obtain a mixed solution. Subsequently, an excess amount of Thioacetamide (TAA) was added to the above mixed solution, and further stirred for 30min (rotation speed 800 rmp). Then heating the solution to a certain temperature by a water bath, and keeping the temperature for a certain time under the condition of vigorous stirring (the rotating speed is 1000 rmp). Centrifuging (rotation speed 10000 rmp for 5 min), collecting precipitate, washing with deionized water, and repeating the centrifuging and washing steps for 3 times to remove excessive impurities. Finally, placing the collected yellow precipitate in a vacuum drying oven at 60 ℃ for 12 hours to obtain the two-dimensional CdIn 2 S 4 Nanosheets (CIS NSs);
(2) preparation of two-dimensional by direct stirring methodCdIn 2 S 4 PDDA nano-sheet: CIS NSs (100 mg) was added to 10mL of PDDA solution at a concentration of x (x =2, 5, 7, 10, 12 mg/mL) and vigorously stirred (1000 rmp rpm) for 1 hour. Then, the mixture was centrifuged (rotation speed: 10000 rmp for 5 min), and thus obtained PDDA-modified cissns (CP-x) were thoroughly washed with deionized water to remove residual free PDDA adsorbed on the surface. Finally, the obtained powder is dried in vacuum at 60 ℃ for 12 hours to obtain the two-dimensional CdIn 2 S 4 a/PDDA nanosheet (CP-x);
(3) preparing a two-dimensional NiFe-LDH nano sheet by a direct coprecipitation method: mixing Ni (NO) 3 ) 2 ·6H 2 O and Fe (NO) 3 ) 3 ·9H 2 O, mixing and adding deionized water; the pH of the mixed solution was adjusted to 9.0 with 0.5M NaOH solution at room temperature, and a tan precipitate appeared. Then, the yellow brown precipitate is stirred strongly for 24 hours at room temperature; then filtering the generated precipitate, and washing with distilled water for multiple times to remove redundant soluble ions; finally, drying the washed precipitate in an oven at 80 ℃ overnight, and grinding the precipitate into powder to obtain two-dimensional NiFe-LDH nano sheets;
(4) CdIn preparation by direct stirring method 2 S 4 The composite material of/PDDA/NiFe-LDH: mixing 50 mg of CP-x powder with y mg of NiFe-LDH powder, and adding 30 mL of deionized water; stirring the mixed solution at room temperature for 1 h; centrifuging the stirred mixed solution, drying in a drying oven, and grinding into powder to obtain CdIn 2 S 4 the/PDDA/NiFe-LDH powder sample.
Wherein the dosage ratio of the NiFe-LDH to the CP-x is 0.14.
Example 7
Two-dimensional CdIn 2 S 4 Preparing a/PDDA/two-dimensional NiFe-LDH photocatalytic composite material:
(1) simple low-temperature reflux method for preparing two-dimensional CdIn 2 S 4 Nanosheet: adding Cd (CH) 3 COO) 2 ·2H 2 O and InCl 3 Mixing, adding deionized water, and stirring for 30min (rotation speed of 800 rmp) to obtain a mixed solution. Then, as described aboveThe mixed solution was added with an excess of Thioacetamide (TAA) and stirred for another 30min (rotation speed 800 rmp). The solution was then heated to a certain temperature by a water bath and incubated for a certain period of time with vigorous stirring (1000 rmp). Centrifuging (rotation speed of 10000 rmp, time of 5 min), collecting precipitate, washing with deionized water, and repeating the centrifuging and washing steps for 3 times to remove excessive impurities. Finally, placing the collected yellow precipitate in a vacuum drying oven at 60 ℃ for 12 hours to obtain the two-dimensional CdIn 2 S 4 Nanosheets (CIS NSs);
(2) preparation of two-dimensional CdIn by direct stirring method 2 S 4 PDDA nanosheet: CISNSs (100 mg) was added to 10mL of PDDA solution at a concentration of x (x =2, 5, 7, 10, 12 mg/mL) and stirred vigorously (1000 rmp) for 1 hour. Then, the mixture was centrifuged (rotation speed: 10000 rmp for 5 min), and thus obtained PDDA-modified cissns (CP-x) were thoroughly washed with deionized water to remove residual free PDDA adsorbed on the surface. Finally, the obtained powder is dried in vacuum at 60 ℃ for 12 hours to obtain the two-dimensional CdIn 2 S 4 PDDA nanosheets (CP-x);
(3) preparing a two-dimensional NiFe-LDH nano sheet by a direct coprecipitation method: mixing Ni (NO) 3 ) 2 ·6H 2 O and Fe (NO) 3 ) 3 ·9H 2 O, mixing and adding deionized water; the pH of the mixed solution was adjusted to 9.0 with 0.5M NaOH solution at room temperature, and a tan precipitate appeared. Then, the yellow brown precipitate is stirred strongly for 24 hours at room temperature; then filtering the generated precipitate, and washing with distilled water for multiple times to remove redundant soluble ions; finally, drying the washed precipitate in an oven at 80 ℃ overnight, and grinding the precipitate into powder to obtain two-dimensional NiFe-LDH nano sheets;
(4) CdIn preparation by direct stirring method 2 S 4 The composite material of/PDDA/NiFe-LDH: mixing 50 mg of CP-x powder with y mg of NiFe-LDH powder, and adding 30 mL of deionized water; stirring the mixed solution at room temperature for 1 h; centrifuging the stirred mixed solution, then putting the mixed solution into an oven for drying, and finally grinding the dried mixed solution into powder to obtain the CdIn 2 S 4 Powder sample of/PDDA/NiFe-LDH (CPL-y).
Wherein, the dosage ratio of the NiFe-LDH to the CP-x is 0.14.
The above description is only a preferred embodiment of the present invention, and all the equivalent changes and modifications made according to the claims of the present invention should be covered by the present invention.
Claims (10)
1. Two-dimensional CdIn 2 S 4 The preparation method of the/PDDA/two-dimensional NiFe-LDH photocatalytic composite material is characterized by comprising the following steps: the method comprises the following steps:
(1) preparation of two-dimensional CdIn by low-temperature reflux method 2 S 4 Nanosheet: adding Cd (CH) 3 COO) 2 ·2H 2 O and InCl 3 Mixing, adding deionized water, stirring for 30min to obtain a mixed solution, adding excessive thioacetamide into the mixed solution, stirring for 30min, heating in water bath, carrying out hydrothermal reaction under vigorous stirring, centrifuging after the reaction is finished, collecting a precipitate, washing with deionized water to obtain a yellow precipitate, and vacuum drying to obtain the two-dimensional CdIn 2 S 4 A nanosheet;
(2) two-dimensional CdIn prepared by stirring method 2 S 4 PDDA nanosheet: the two-dimensional CdIn prepared in the step (1) is 2 S 4 Adding the nanosheet into a PDDA solution, stirring for 1h, and centrifuging the mixture to obtain the PDDA modified CdIn 2 S 4 Thoroughly cleaning the nanosheets with deionized water to remove residual free PDDA adsorbed on the surface, and finally, vacuum drying the obtained powder to obtain the two-dimensional CdIn 2 S 4 a/PDDA nanosheet;
(3) preparing a two-dimensional NiFe-LDH nanosheet by a coprecipitation method: mixing Ni (NO) 3 ) 2 ·6H 2 O and Fe (NO) 3 ) 3 ·9H 2 O, mixing and adding deionized water; adjusting the pH value of the mixed solution to 9.0 by using 0.5M NaOH solution at room temperature to obtain a tawny precipitate, and then stirring the tawny precipitate at room temperature for 24 hours; the resulting precipitate was then filtered and washed with distilled water several times to remove muchThe remaining soluble ions; finally, drying the washed precipitate, and grinding the precipitate into powder to obtain a two-dimensional NiFe-LDH nano sheet;
(4) stirring method for preparing CdIn 2 S 4 The composite material of/PDDA/NiFe-LDH: mixing the two-dimensional CdIn obtained in the step (1) 2 S 4 Adding deionized water into the PDDA nanosheets and the NiFe-LDH nanosheets obtained in the step (2), and stirring at room temperature; centrifuging, drying and grinding to obtain the two-dimensional CdIn 2 S 4 The composite material comprises/PDDA/two-dimensional NiFe-LDH photocatalysis.
2. The two-dimensional CdIn of claim 1 2 S 4 The preparation method of the/PDDA/two-dimensional NiFe-LDH photocatalytic composite material is characterized by comprising the following steps: step (1), mixing Cd (CH) in the solution 3 COO) 2 ·2H 2 O、InCl 3 And the concentration of thioacetamide is 0.006 mol/L, 0.012 mol/L and 0.032mol/L respectively.
3. The two-dimensional CdIn of claim 1 2 S 4 The preparation method of the/PDDA/two-dimensional NiFe-LDH photocatalytic composite material is characterized by comprising the following steps: and (1) performing hydrothermal reaction at 100 ℃ for 12 h.
4. The two-dimensional CdIn of claim 1 2 S 4 The preparation method of the/PDDA/two-dimensional NiFe-LDH photocatalytic composite material is characterized by comprising the following steps: step (2), preparing the PDDA solution by using a 0.5M NaCl solution, wherein the pH value is 10, and the concentration is 2-12 mg/mL; the two-dimensional CdIn 2 S 4 The mass ratio of the nano-sheets to the PDDA is 10: 4-24.
5. The two-dimensional CdIn of claim 1 2 S 4 The preparation method of the/PDDA/two-dimensional NiFe-LDH photocatalytic composite material is characterized by comprising the following steps: in the mixed solution of the step (3), Ni (NO) 3 ) 2 · 6H 2 O and Fe (NO) 3 ) 3 · 9H 2 The O concentrations were 1.6 mol/L and 0.33 mol/L, respectively.
6. The two-dimensional CdIn of claim 5 2 S 4 The preparation method of the/PDDA/two-dimensional NiFe-LDH photocatalytic composite material is characterized by comprising the following steps: ni in NiFe-LDH preparation process 2+ And Fe 3+ The total ion concentration of (2) was 0.2M.
7. The two-dimensional CdIn of claim 1 2 S 4 The preparation method of the/PDDA/two-dimensional NiFe-LDH photocatalytic composite material is characterized by comprising the following steps: in step (3), the titration solution is washed with distilled water for a plurality of times to remove excessive soluble ions until the pH value of the titration solution reaches 7.
8. The two-dimensional CdIn of claim 1 2 S 4 The preparation method of the/PDDA/two-dimensional NiFe-LDH photocatalytic composite material is characterized by comprising the following steps: two-dimensional CdIn in step (4) 2 S 4 The mass ratio of the PDDA nano sheet to the NiFe-LDH nano sheet is 50: 2-15.
9. Two-dimensional CdIn prepared by the preparation method of any of claims 1-8 2 S 4 The composite material is a/PDDA/two-dimensional NiFe-LDH photocatalysis composite material.
10. The two-dimensional CdIn of claim 9 2 S 4 The application of the/PDDA/two-dimensional NiFe-LDH photocatalytic composite material is characterized in that: the carbon dioxide reduction device is used for carrying out carbon dioxide reduction under the irradiation of visible light or simulated sunlight.
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