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A kind of ruthenium complex photocatalyst, preparation method and application thereof
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A technology of photocatalyst and ruthenium complex, applied in the field of preparation of new ruthenium complex photocatalytic materials
Active Publication Date: 2021-01-26
CHINA THREE GORGES UNIV
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[0004] According to literature reports, C 34 h 28 N 8 RuP 2 f 16 As a photocatalyst, it has not been reported yet
Method used
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Embodiment 1
[0034] The preparation scheme that the present invention adopts comprises the following steps
[0035] Step 1: Divide 1.00 x 10 -4 mol of Ru(2,2'-bipyridine) 2 Cl 2 Dissolve in N,N-dimethylformamide solution (5ml), stir until dissolved;
[0036] Step 2: Place the 1.05×10 -4 mol of 1-benzyl-4-phenyl-1H-1,2,3-triazole was added to the solution in step 1, stirred until dissolved, in which Ru(2,2'-bipyridine) 2 Cl 2 , The molar ratio of 1-benzyl-4-phenyl-1H-1,2,3-triazole is 1:1.05;
[0037] Step 3: Heat the solution obtained in step 2 to 160°C and react for 24 hours.
[0038] Step 4: After the reaction is completed and cooled to room temperature, the saturated NH 4 PF 6 Aqueous solution (5ml) was slowly added to the solution from step 3 and stirred for an additional 2 hours. At this time, a large amount of solid will appear in the system.
[0039] Step 5: After the reaction is completed, filter with suction, and the residue is dried to obtain compound C 34 h 28 N 8 R...
Embodiment 2
[0044] The application of the novel ruthenium complex photocatalyst obtained in Example 1 of the present invention in the degradation of phenylboronic acid.
[0045] Including the following steps:
[0046]
[0047] Step 1: Divide the 5.00 x 10 -4 mol of phenylboronic acid was dissolved in N,N-dimethylformamide solution (2ml), stirred until dissolved;
[0048] Step 2: Convert 1.00×10 -5 mol of the new photocatalyst is added to the reaction system, and at the same time 1.00×10 -3 The triethylamine of mol adds in the reaction system;
[0049] Step 3: Turn on the visible light source in the photochemical reaction instrument (irradiated by a 36W fluorescent lamp), so that phenylboronic acid is photocatalytically degraded into phenol under the action of the new photocatalyst 1;
[0050] Step 4: After the photocatalytic reaction started, samples were taken from the reaction every 30 minutes for nuclear magnetic spectrum to detect the degradation of phenylboronic acid. Final yie...
Embodiment 3
[0054] The application of the novel ruthenium complex photocatalyst obtained in Example 1 of the present invention in catalyzing the coupling reaction of terminal alkynes and diazonium salts. Including the following steps:
[0055]
[0056] Step 1: Divide 2.00 x 10 -3 mol of phenylacetylene (2) was dissolved in N,N-dimethylformamide solution (2ml), stirred until dissolved;
[0057] Step 2: Convert 1.00×10 -5 mol of novel photocatalysts and 5.00×10 -5 Triphenyl phosphogold chloride is added to the reaction system, and at the same time, 5.00×10 -4 The phenylacetylene (2) of mol adds in the reaction system;
[0058] Step 3: Turn on the blue light source (irradiated by 23W fluorescent lamp) in the photochemical reaction apparatus, let phenylacetylene (2) and diazonium tetrafluoroborate p-methoxybenzene salt (3) start to react in the new photocatalyst 1 and triphenylphosphine chloride Oxidative coupling reaction occurs under the action of gold.
[0059] Step 4: After the p...
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Abstract
The invention provides a novel photocatalyst which has a chemical structural formula as shown in the specification, and the chemical formula is C34H28N8RuP2F16, and a molecular weight is 940.07. A synthesis method comprises the following step: by taking Ru(2,2'-bipridine)2Cl2 and 1-benzyl-4-phenyl-1H-1,2,3-triazole as raw materials in a mole ratio of 1:1.05, carrying out anion exchange with NH4PF6, thereby obtaining the novel photocatalyst. Catalysis performance tests show that the catalyst has a good capability of degrading borophenylic acid under a white light radiation condition, and in addition, the double-metal photocatalyst consisting of a ruthenium compound and Ph3AuCl has a good coupling reaction of catalysis tail end alkyne and diazonium salt under a blue light radiation condition. The process provided by the invention is simple in method and high in efficiency; the obtained novel photocatalyst is high in purity, regular in single crystal morphology and uniform in size; discovery and study on C34H28N8RuP2F16 are beneficial to widening of study fields of ruthenium series photocatalytic material materials, and novel ideas are provided for design and synthesis of novel visible light photocatalysts.
Description
technical field [0001] The invention belongs to the field of functional materials, in particular to a preparation method and application of a novel ruthenium complex photocatalytic material. Background technique [0002] [Ru(bpy) 3 ] 2+ , three [2,2' bipyridyl] ruthenium ion, as a commercial photosensitizer, has good water solubility, stable chemical, electrochemical and photochemical properties, redox reversible, high luminous efficiency, wide application pH range, can be Electrochemical regeneration, long excited state lifetime and other characteristics have been widely used in organic photocatalytic reactions. [Ru(bpy) 3 ] 2+ It is expensive and is consumed in large quantities in organic reactions, resulting in environmental pollution and high production costs, while the new ruthenium complex catalyst C 34 h 28 N 8 RuP 2 f 16 The discovery and research will help to further broaden the research field of ruthenium series photocatalytic materials, and will also prov...
Claims
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