Palladium / perovskite material for visible light catalytic ome reaction, and preparation method and application thereof
By loading palladium nanoparticles onto perovskite CsPbBr3 to form Pd/CsPbBr3 nanocomposite materials, the problems of high-temperature byproduct generation and rapid recombination of photogenerated electrons and holes in the traditional Suzuki reaction were solved, and a highly efficient and stable visible light-catalyzed Suzuki reaction was achieved.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-09-28
- Publication Date
- 2026-03-17
AI Technical Summary
Traditional Suzuki reactions require high temperatures, leading to the formation of byproducts. Furthermore, common catalysts exhibit rapid recombination of photogenerated electrons and holes and low catalytic efficiency under solar spectral conditions.
Palladium nanoparticles were loaded onto inorganic metal halide perovskite CsPbBr3 as a support to form a Pd/CsPbBr3 nanocomposite material, which was then used to catalyze the reaction by generating photocharge through visible light excitation.
Under mild visible light conditions, the Pd/CsPbBr3 nanocomposite material exhibits highly efficient catalytic performance, producing biphenyl and its derivatives in yields of 85-99%, and retains its activity after 5 cycles.
Smart Images

Figure CN117380227B_ABST
Abstract
Description
Technical Field
[0001] This invention belongs to the technical field of inorganic hybrid material synthesis and application, specifically relating to palladium / perovskite materials for visible light-catalyzed neighbor-wood reactions, their preparation methods, and applications. Background Technology
[0002] The Suzuki reaction, or neighbor-wood reaction, is considered an important part of modern synthetic chemistry and has been widely used in the preparation of various drugs and polymers (Reference 1. Dasa, et al. "Schiff base-derivedhomogeneous and heterogeneous palladium catalysts for the Suzuki-Miyaura reaction", Coordination Chemistry Reviews, 2016, 311, 1-23). In recent years, palladium catalysts have been widely used as catalysts in the Suzuki reaction due to their unique catalytic activity, good functional group tolerance, and high catalytic selectivity under mild conditions (Reference 2. García-Melchor et al. "Computational perspective on Pd-catalyzed CC cross-coupling reaction mechanisms", Accounts of Chemical Research, 2013, 46(11), 2626-2634). Typically, homogeneous palladium complexes or supported heterogeneous palladium catalysts are used in the Suzuki reaction [Reference 3. Oliveira et al. Pd nanoparticles simulated on graphene oxide / silica nanocomposite: efficient and recyclable catalysts for cross-coupling reactions”《Chemistry Select》, 2018, 3(2), 535-543. Reference 4. Kohlhler et al.“Genesis of coordinatively unsaturated palladium complexes dissolved from solid precursors during Heck coupling reactions and their role as catalytically active specie”《Inorganic Chemistry》, 2007, 46(6), 1876-1883].Traditional Suzuki reactions typically require high-temperature environments provided by energy combustion; however, high temperatures easily lead to the formation of byproducts (Reference 5. Chuentragool et al. "Catalysis with palladium complexes photoexcited by visible light", Angewandte International Edition Chemie, 2019, 58(34), 11586-11598). Therefore, developing green and clean energy sources and efficient heterogeneous catalytic materials are effective means to solve these problems.
[0003] Metal halide perovskites are a class of hybrid materials that possess advantages unmatched by other inorganic hybrid materials, such as high absorption coefficients, wide visible light absorption, high carrier mobility, and long carrier diffusion lengths (Reference 6. Seoetal. "Efficient flexible organic / inorganic hybrid perovskite light-emitting diodes based on graphene anode" Advance Materials, 2017, 29(12), 1605587). These characteristics give perovskite materials great potential and application prospects in photochemistry, especially in heterogeneous photocatalysis. In addition, the tunable structure and physicochemical properties of metal halide perovskites allow for the rational design of the structure and composition of perovskites according to the expected functions. Among them, the inorganic metal halide perovskite CsPbBr3 possesses rich chemical composition, excellent chemical stability, and good photoactivity, making it beneficial as a photocatalyst for achieving efficient photochemical reactions (Reference 7. Nedelcu et al. "Fast anion-exchange in equally luminescent nanocrystals of cesium lead halide perovskites (CsPbX3, X=Cl,Br,I)", *Nano Letters*, 2015, 15(8), 5635-5640. Reference 8. Hou et al. "Inorganic colloidal perovskite quantum dots for robust solar CO2 reduction", *Chemistry-A European Journal*, 2017, 23(100), 9481-9485). Based on the above discussion, we synthesized the inorganic metal halide perovskite CsPbBr3 and its nanocomposite material Pd / CsPbBr3, and applied it to the photocatalytic Suzuki reaction. Experimental results show that the prepared Pd / CsPbBr3 nanocomposite material exhibits excellent catalytic performance and broad applicability in the photocatalytic Suzuki reaction, with yields of biphenyl and its series derivatives ranging from 85% to 99%. Furthermore, the Pd / CsPbBr3 nanocomposite material retains its catalytic activity even after five cycles. Summary of the Invention
[0004] The purpose of this invention is to overcome the problems of rapid recombination of photogenerated electrons and holes and low catalytic efficiency of common catalysts under solar spectral conditions, and to provide a palladium / perovskite material with wide visible light absorption and high catalytic efficiency for visible light catalytic neighbor-wood reactions, as well as its preparation method and application.
[0005] To achieve the above objectives, the technical solution of the present invention is as follows:
[0006] The present invention first provides a palladium / perovskite material for visible light catalyzing the neighboring wood reaction. The palladium / perovskite material has the chemical formula Pd / CsPbBr3, wherein the particle size of CsPbBr3 is 40-300 nm and the size of palladium nanoparticles is 2-5 nm.
[0007] This invention also provides a method for preparing the above-mentioned palladium / perovskite material for visible light-catalyzed neighbor-wood reaction, specifically including the following steps:
[0008] (1) Preparation of perovskite nanomaterials: CsBr was ultrasonically dissolved in pure water and PbBr2 was ultrasonically dissolved in N,N-dimethylformamide to prepare a precursor solution. The precursor solution was then added dropwise to a mixed solution of oleic acid, n-octylamine and n-hexane at a certain rate. The mixture was then continuously stirred in an oil bath at 25-50°C for 2-6 hours to form an emulsion. Acetone was then added to break the emulsion. The mixture was then centrifuged, washed and dried in a vacuum drying oven at 50-80°C for 2-8 hours to obtain perovskite nanomaterials.
[0009] (2) Preparation of Pd / perovskite nanocomposite material: The perovskite nanomaterial prepared in step (1) was dried and dispersed in anhydrous ethanol. It was sonicated for 30-120 min to make it uniformly dispersed. Then, palladium acetate solution was added and the mixture was irradiated under a blue LED lamp for 5-30 min. After centrifugation, washing and drying in a vacuum drying oven at 50-80℃ for 2-8 hours, Pd / CsPbBr3 nanocomposite material was obtained.
[0010] Furthermore, in the mixed system described in step (1), the concentration of CsBr is 5:6 mg / L and the concentration of PbBr2 is 11:14 mg / L.
[0011] Further, in step (1), the volume ratio of oleic acid, n-octylamine, n-hexane, and acetone is 3-5 mL oleic acid : 1-3 mL n-octylamine : 2-3 mL n-hexane : 3-5 mL acetone.
[0012] Furthermore, in step (1), the dropping rate of the CsBr and PbBr2 precursor solutions is 2s to 10s / drop.
[0013] Furthermore, in the reaction system of step (2), the concentration of the perovskite nanomaterial is 1:4 mg / mL, and the concentration of palladium acetate is 1:3 mg / mL.
[0014] Furthermore, in step (2), the power of the blue LED light is 7-28W.
[0015] Furthermore, in step (2), the mass fraction of palladium in the synthesized Pd / CsPbBr3 nanocomposite is 1.2–1.6 wt%.
[0016] The present invention also provides an application of the above-mentioned palladium / perovskite material for visible light catalytic neighbor-wood reaction, wherein the visible light absorption range of the palladium / perovskite material for visible light catalytic neighbor-wood reaction can be extended to 532 nm, and photogenerated charge is generated by visible light excitation, and a visible light catalytic Suzuki reaction is carried out to produce a series of biphenyl compounds with different substituents.
[0017] This invention tested the photocatalytic Suzuki reaction capability of the Pd / perovskite nanocomposite material. The specific test steps and results were as follows: (a) Sampling: The prepared Pd / CsPbBr3 nanocomposite material, alkali, iodobenzene or its derivatives, and phenylboronic acid or its derivatives were added to a solvent; (b) Photocatalysis: The mixture was irradiated under visible light for 4 hours, and then the biphenyl series products were separated and purified. NMR detection results showed that the Pd / CsPbBr3 nanocomposite material exhibited excellent photocatalytic Suzuki reaction performance under visible light.
[0018] Furthermore, in the mixed system described in step (b), the mass ratio of the Pd / CsPbBr3 nanocomposite material is 3:7 mg.
[0019] Further, the alkali mentioned in step (a) includes sodium carbonate, potassium carbonate, and cesium carbonate.
[0020] Further, the solvents mentioned in step (a) include ethanol, distilled water, N,N-dimethylformamide, and mixtures thereof.
[0021] Further, the iodobenzene derivatives mentioned in step (a) include 2-methyliodobenzene, 2-fluoroiodobenzene, 3-methyliodobenzene, 3-fluoroiodobenzene and 4-methyliodobenzene.
[0022] Further, the phenylboronic acid derivatives mentioned in step (a) include 2-methylphenylboronic acid, 2-fluorophenylboronic acid, 2-methoxyphenylboronic acid, 3-methylphenylboronic acid, and 4-methylphenylboronic acid.
[0023] Further, the molar ratio of iodobenzene and phenylboronic acid in step (a) is 1:1.5 to 1:2 mol.
[0024] The beneficial effects of this invention are as follows:
[0025] 1. This synthetic route is simple to operate, with mild reaction conditions and high efficiency, which is beneficial for the rapid and efficient synthesis of Pd / CsPbBr3 nanocomposites.
[0026] 2. Pd / CsPbBr3 nanocomposites have good chemical and water stability, large specific surface area, and wide visible light absorption range.
[0027] 3. This invention utilizes inorganic metal perovskite CsPbBr3 as a support to load palladium nanoparticles, preparing a Pd / CsPbBr3 nanocomposite material, which exhibits excellent catalytic performance in the photocatalytic Suzuki reaction and shows good general applicability to iodobenzene derivatives and phenylboronic acid derivatives with different substituents. Attached Figure Description
[0028] Figure 1 Transmission electron microscopy image of perovskite CsPbBr3 nanomaterials.
[0029] Figure 2 This is a schematic diagram of the structure of perovskite CsPbBr3 nanomaterials.
[0030] Figure 3 The image shows the powder X-ray diffraction (PXRD) pattern of the Pd / CsPbBr3 nanocomposite material.
[0031] Figure 4 The infrared spectrum of the Pd / CsPbBr3 nanocomposite material is shown.
[0032] Figure 5 The image shows the UV-Vis absorption spectrum of the perovskite CsPbBr3 nanomaterial.
[0033] Figure 6 The 1H NMR spectrum of the biphenyl product obtained by photocatalytic Suzuki reaction of Pd / CsPbBr3 nanocomposite material.
[0034] Figure 7 The 1H NMR spectrum of the 2-methylbiphenyl product obtained by photocatalytic Suzuki reaction of Pd / CsPbBr3 nanocomposite material.
[0035] Figure 8 The 1H NMR spectrum of the 3-methylbiphenyl product obtained by photocatalytic Suzuki reaction of Pd / CsPbBr3 nanocomposite material.
[0036] Figure 9 The graph shows the cycle performance of the photocatalytic Suzuki reaction of Pd / CsPbBr3 nanocomposite materials. Detailed Implementation
[0037] The present invention will be further illustrated below with reference to the accompanying drawings and specific embodiments. It should be understood that the following specific embodiments are for illustrative purposes only and are not intended to limit the scope of the invention.
[0038] Example 1
[0039] Preparation of Pd / CsPbBr3 nanocomposites:
[0040] (1) Take 2 mmol of cesium bromide solution in 2 mL of distilled water, and dissolve 2 mmol of lead bromide in 3 mL of N,N-dimethylformamide. After sonication for 30 min, add the two solutions dropwise at a rate of 5 s / drop to a mixed solution containing 8 mL of oleic acid, 1.5 mL of n-octylamine and 500 mL of cyclohexane. Stir the mixed solution in an oil bath at 50 °C for 3 hours to form an emulsion. Then add 500 mL of acetone to break the emulsion. Finally, wash with anhydrous ethanol and dry in a vacuum drying oven at 50 °C for 3 hours to obtain a yellow powdery solid CsPbBr3.
[0041] (2) 20 mg of dried perovskite CsPbBr3 powder was ultrasonically dispersed in 2 mL of anhydrous ethanol to prepare a 10 mg / mL suspension. 0.2 mL of palladium acetate solution (5 mg / mL) was added to this suspension. The resulting mixture was stirred under a blue LED light for 5 min, then washed by centrifugation with anhydrous ethanol, and dried in a vacuum drying oven at 50 °C for 2 hours to obtain a brownish-yellow powdery Pd / CsPbBr3 nanocomposite material. Test results showed that the size of the palladium nanoparticles was approximately 3 nm, and the mass fraction of the palladium nanoparticles was 1.42 wt%.
[0042] Basic representation
[0043] The CsPbBr3 material described in Example 1 has a blocky morphology with a size of approximately 40 nm. Figure 1 As shown. Figure 2 The diagram shown is a schematic of its structure. The center of the structure is a cesium atom, and the octahedron is composed of bromine and lead atoms.
[0044] like Figure 3 The PXRD spectra are shown below. (a) is the XRD spectrum of the CsPbBr3 compound simulated using standard data exported from Jade 6 software; (b) is the PXRD spectrum of the CsPbBr3 compound synthesized in Example 1. The peak positions of the two XRD spectra (a) and (b) are completely consistent, indicating that the synthesized CsPbBr3 compound is a pure phase without impurities. (c) corresponds to the PXRD spectrum of Pd / CsPbBr3 in Example 1, indicating that the original structure of CsPbBr3 was not changed after loading palladium nanoparticles.
[0045] like Figure 4The infrared spectra are shown in (a) and (b) respectively. (a) is the infrared spectrum of the CsPbBr3 compound in Example 1. The presence of protective agents such as n-octylamine and oleic acid was determined by the characteristic peaks of the spectrum. These protective agents modified the surface of CsPbBr3. (b) is the infrared spectrum of Pd / CsPbBr3 in Example 1, which further illustrates that the palladium nanoparticles did not change the original structure of CsPbBr3.
[0046] Figure 5 The image shows the UV-Vis absorption spectrum of CsPbBr3 described in Example 1. The spectral peaks indicate that the material can absorb visible light, and its absorption range in the visible light region is from 400 nm to 532 nm.
[0047] Example 2
[0048] Preparation of Pd / CsPbBr3 nanocomposites:
[0049] (1) Take 2 mmol of cesium bromide solution in 2 mL of distilled water, and dissolve 2 mmol of lead bromide in 3 mL of N,N-dimethylformamide. Add the two solutions dropwise at a rate of 2 s / drop to a mixed solution containing 10 mL of oleic acid, 3 mL of n-octylamine and 600 mL of cyclohexane. Stir the mixed solution in an oil bath at 50 °C for 3 hours to form an emulsion. Then add 500 mL of acetone to break the emulsion. Finally, wash with anhydrous ethanol and dry in a vacuum drying oven at 50 °C for 3 hours to obtain yellow powdered CsPbBr3 with a size of approximately 300 nm.
[0050] (2) 20 mg of dried perovskite CsPbBr3 powder was ultrasonically dispersed in 2 mL of anhydrous ethanol to prepare a suspension with a concentration of 10 mg / mL. 0.2 mL of palladium acetate solution (7.5 mg / mL) was added dropwise to this suspension. The resulting mixture was stirred under a blue LED light for 5 min, then washed by centrifugation with anhydrous ethanol, and dried in a vacuum drying oven at 50 °C for 2 hours to obtain a brown powdery Pd / CsPbBr3 nanocomposite material. Test results showed that the size of the palladium nanoparticles was approximately 5 nm, and the mass fraction of the palladium nanoparticles was 1.65 wt%.
[0051] Example 3
[0052] Take 2 mmol of cesium bromide solution in 2 mL of distilled water, and dissolve 2 mmol of lead bromide in 3 mL of N,N-dimethylformamide. Add the two solutions dropwise at a rate of 8 s / drop to a mixed solution containing 6 mL of oleic acid, 1.0 mL of n-octylamine, and 400 mL of cyclohexane. Stir the mixed solution in an oil bath at 50 °C for 3 hours to form an emulsion. Then add 500 mL of acetone to break the emulsion. Finally, wash with anhydrous ethanol and dry in a vacuum drying oven at 50 °C for 3 hours to obtain a yellow powder of CsPbBr3 with a size of approximately 80 nm.
[0053] (2) 20 mg of dried perovskite CsPbBr3 powder was ultrasonically dispersed in 2 mL of anhydrous ethanol to prepare a suspension with a concentration of 10 mg / mL. 0.2 mL of palladium acetate solution (2.5 mg / mL) was added dropwise to this suspension. The resulting mixture was stirred under a blue LED light for 5 min, then washed by centrifugation with anhydrous ethanol, and dried in a vacuum drying oven at 50 °C for 2 hours to obtain a brownish-yellow powdery Pd / CsPbBr3 nanocomposite material. Test results showed that the size of the palladium nanoparticles was approximately 3 nm, and the mass fraction of the palladium nanoparticles was 1.21 wt%.
[0054] Example 4
[0055] Photocatalytic Suzuki reaction: 5 mg of the Pd / CsPbBr3 nanocomposite material obtained in Example 1, 0.1 mmol of iodobenzene, 0.15 mmol of phenylboronic acid, and 0.1 mmol of potassium carbonate were weighed into a 4 mL glass vial. 1 mL of ethanol was added, and the mixture was irradiated under a 28 W LED lamp for 4 hours. The biphenyl product was then separated and purified. NMR detection results showed that the Pd / CsPbBr3 nanocomposite material exhibited excellent photocatalytic Suzuki reaction performance under visible light. Figure 6 As shown, the yield of biphenyl products reached 96% after 4 hours.
[0056] The reaction formula is as follows:
[0057]
[0058] Example 5
[0059] The experiment in Example 4 was repeated by replacing the ethanol solvent in Example 4 with 1 mL of distilled water, and the yield of biphenyl product was 23%.
[0060] Example 6
[0061] The experiment in Example 4 was repeated by replacing the ethanol solvent in Example 4 with 1 mL of N,N-dimethylformamide, and the yield of biphenyl product was 84%.
[0062] Example 7
[0063] The experiment in Example 4 was repeated with a 1 / 1 volume ratio of ethanol / water mixed solvent (1 mL) instead of the ethanol solvent in Example 4, and the yield of biphenyl product was 83%.
[0064] Example 8
[0065] The experiment in Example 4 was repeated with a 1 / 3 volume ratio of ethanol / water mixed solvent (1 mL) instead of the ethanol solvent in Example 4, and the yield of biphenyl product was 44%.
[0066] Example 9
[0067] The experiment in Example 4 was repeated with a 3 / 1 volume ratio of ethanol / water mixed solvent (1 mL) instead of the ethanol solvent in Example 4, and the yield of biphenyl product was 85%.
[0068] Example 10
[0069] The experiment of Example 4 was repeated by replacing the Pd / CsPbBr3 nanocomposite material obtained in Example 1 with 3 mg of the Pd / CsPbBr3 nanocomposite material obtained in Example 1. The yield of biphenyl product was 81%.
[0070] Example 11
[0071] The experiment in Example 4 was repeated with 0.1 mmol sodium carbonate instead of potassium carbonate, and the yield of biphenyl product was 45%.
[0072] Example 12
[0073] The experiment in Example 4 was repeated with 0.1 mmol of phenylboronic acid instead of 0.15 mmol of phenylboronic acid. The yield of biphenyl product was 74%.
[0074] Example 13
[0075] The experiment in Example 4 was repeated with 0.2 mmol of phenylboronic acid instead of 0.15 mmol of phenylboronic acid. The yield of biphenyl product was 87%.
[0076] Example 14
[0077] Weigh 5 mg of the Pd / CsPbBr3 nanocomposite material obtained in Example 1, 0.1 mmol of 2-methyliodobenzene, 0.15 mmol of phenylboronic acid, and 0.1 mmol of potassium carbonate into a 4 mL glass vial. Add 1 mL of ethanol solvent. Irradiate the system under a 28 W LED lamp for 4 hours. Then, separate and purify to obtain the biphenyl derivative. NMR detection results show that the Pd / CsPbBr3 nanocomposite material exhibits excellent photocatalytic Suzuki reaction performance under visible light. Figure 7 As shown, the product yield reached 86% after 4 hours.
[0078] Example 15
[0079] The experiment in Example 14 was repeated by replacing 2-methyliodobenzene with 0.1 mmol of 2-fluoroiodobenzene, and the yield of biphenyl derivatives was 66%.
[0080] Example 16
[0081] The experiment in Example 14 was repeated by replacing 2-methyliodobenzene with 0.1 mmol of 3-methyliodobenzene, and the yield of biphenyl derivatives was 93%.
[0082] Example 17
[0083] The experiment in Example 14 was repeated by replacing 2-methyliodobenzene with 0.1 mmol of 3-fluoroiodobenzene, and the yield of biphenyl derivatives was 85%.
[0084] Example 18
[0085] The experiment in Example 14 was repeated by replacing 2-methyliodobenzene with 0.1 mmol of 4-methyliodobenzene, and the yield of the biphenyl derivative was 79%.
[0086] Example 19
[0087] Weigh 5 mg of the Pd / CsPbBr3 nanocomposite material obtained in Example 1, 0.1 mmol of iodobenzene, 0.15 mmol of 3-methylphenylboronic acid, and 0.1 mmol of potassium carbonate into a 4 mL glass vial. Add 1 mL of ethanol solvent. Irradiate the system under a 28 W LED lamp for 4 hours. Then, separate and purify to obtain the biphenyl derivative. NMR detection results show that the Pd / CsPbBr3 nanocomposite material exhibits excellent photocatalytic Suzuki reaction performance under visible light. Figure 8 As shown, the product yield reached 78% after 4 hours.
[0088] Example 20
[0089] The experiment in Example 19 was repeated by replacing 3-methylphenylboronic acid with 0.15 mmol of 2-methylphenylboronic acid, and the yield of biphenyl derivatives was 88%.
[0090] Example 21
[0091] The experiment in Example 19 was repeated by replacing 3-methylphenylboronic acid with 0.15 mmol of 2-fluorophenylboronic acid, and the yield of biphenyl derivatives was 72%.
[0092] Example 22
[0093] The experiment in Example 19 was repeated by replacing 3-methylphenylboronic acid with 0.15 mmol of 2-methoxyphenylboronic acid, and the yield of biphenyl derivatives was 51%.
[0094] Example 23
[0095] The experiment in Example 19 was repeated by replacing 3-methylphenylboronic acid with 0.15 mmol of 4-methylphenylboronic acid, and the yield of biphenyl derivatives was 77%.
[0096] Example 24
[0097] Photocatalytic cycling experiment: The Pd / CsPbBr3 nanocomposite material after photocatalysis in Example 4 was centrifuged, washed twice with anhydrous ethanol, and dried in a vacuum drying oven at 85°C. The recovered Pd / CsPbBr3 nanocomposite material was then used as a photocatalyst to repeat the experiment in Example 4. The results showed that the Pd / CsPbBr3 nanocomposite material could withstand 5 cycles. Figure 9 As shown.
[0098] It should be noted that the above content merely illustrates the technical concept of the present invention and should not be construed as limiting the scope of protection of the present invention. For those skilled in the art, corresponding changes and substitutions can be made based on the technical solution and inventive concept of the present invention, and those with the same performance or use should also be considered within the scope of protection of the present invention.
Claims
1. Use of a palladium / perovskite material catalyzing the o-iodo reaction with visible light, characterized in that, The chemical formula of the palladium / perovskite material is Pd / CsPbBr3, wherein the particle size of CsPbBr3 is 40-300 nm, and the size of the palladium nanoparticle is 2-5 nm; The preparation method of the palladium / perovskite material specifically comprises the following steps: (1) perovskite nanomaterial preparation: CsBr is ultrasonically dissolved in pure water, PbBr2 is ultrasonically dissolved in N,N-dimethylformamide to prepare a precursor solution, and the precursor solution is added dropwise to a mixed solution of oleic acid, n-octylamine and n-hexane at a certain speed, then the mixed system is continuously stirred at 25-50 DEG C in an oil bath for 2-6 hours to form an emulsion, then acetone is added to break the emulsion, and the emulsion is dried by centrifugation, washing and drying in a 50-80 DEG C vacuum drying oven for 2-8 hours to obtain a perovskite nanomaterial; (2) palladium / perovskite material preparation: the dried perovskite nanomaterial prepared in step (1) is dispersed in anhydrous ethanol, ultrasonically dispersed for 30-120 min, then palladium acetate solution is added, and the system is irradiated under a blue LED lamp for 5-30 min, and then the system is dried by centrifugation, washing and drying in a 50-80 DEG C vacuum drying oven for 2-8 hours to obtain a palladium / perovskite material; In step (1), the concentration of CsBr in the mixed system is 5:6 mg / L, and the concentration of PbBr2 is 11:14 mg / L, In step (1), the volume ratio of the amounts of oleic acid, n-octylamine, n-hexane and acetone is 3-5 mL of oleic acid: 1-3 mL of n-octylamine: 2-3 mL of n-hexane: 3-5 mL of acetone; In the reaction system of step (2), the concentration of the perovskite nanomaterial is 1:4 mg / mL, and the concentration of palladium acetate is 1:3 mg / mL; In step (2), the power of the blue LED lamp is 7-28 W; In step (2), the mass fraction of palladium in the synthesized palladium / perovskite material is 1.2-1.6 wt%, The visible light absorption range of the palladium / perovskite material for visible light catalysis of o-wood reaction can be extended to 532 nm, photo-generated charges are generated by visible light excitation, and a series of diphenyl compounds connected with different substituents are generated by visible light catalysis of Suzuki reaction.
Citation Information
Patent Citations
Preparation method of flexible nano piezoelectric generator based on CsPbBr3 nanocrystals
CN115173738A