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A kind of metal-bipyridylium photocatalyst, preparation method and application thereof

A bipyridinium salt and catalyst technology, applied in the field of photocatalysis, can solve the problems of complicated catalyst preparation and high cost, and achieve the effects of high selectivity, cost reduction and simple synthesis process

Active Publication Date: 2020-07-10
BEIJING INSTITUTE OF TECHNOLOGYGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, titanium dioxide and sulfide nanosheets are used as photocatalysts, but the preparation of these catalysts is cumbersome, and expensive metals are often used, resulting in high cost

Method used

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  • A kind of metal-bipyridylium photocatalyst, preparation method and application thereof
  • A kind of metal-bipyridylium photocatalyst, preparation method and application thereof
  • A kind of metal-bipyridylium photocatalyst, preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] Preparation of metal-bipyridylium photocatalyst Zn 2 C 48 N 8 Cl 6 h 52 o 8 : Add ligand bipyridylium salt (0.05mmol) and 2mL mixed solvent into a small glass bottle of 20mL, stir and dissolve to obtain an onium salt solution; in addition, add ZnCl to a small glass bottle of 20mL 2 ·xH 2 O (0.025mmol) and 2mL mixed solvent, stirring and dissolving to obtain a metal salt solution; drop the metal salt solution into the ligand solution, mix the two evenly, stir until a precipitate is produced, filter the precipitate, and acetone Washing, drying in an oven at 70 degrees under normal pressure for 1 hour to obtain a metal-bipyridylium photocatalyst;

[0047] Wherein, the structure of ligand onium salt is:

[0048] Wherein, the mixed solvent is: a mixed solvent of N,N-dimethylformamide and ethanol (1:1 by volume).

[0049] The IR of the final product (KBr, cm –1 ) characterization results such as figure 1 As shown, the results show that the final product is Zn 2 C...

Embodiment 2

[0052] Preparation of metal-bipyridylium photocatalyst Cd 4.5 C 66 N 3 Cl 11 o 37 h 55 : add bipyridylium salt (0.05mmol) and 2mL water in the vial of 20mL, stir and dissolve, adjust pH=7 with the NaOH solution of 2mol / L, obtain ligand solution; In addition, take trimesic acid ( 0.05mmol) in a 10mL beaker, add 1mL water in the beaker, stir and dissolve, adjust pH=7 with 2mol / L NaOH solution to obtain a trimesic acid solution; the trimesic acid solution is dripped into the formulation In the body solution, the two are uniformly mixed to obtain a mixed solution, and 2 mL of 0.01mol / L CdCl is added to the mixed solution 2 aqueous solution, and then add 1 mL of ethanol to adjust the polarity, and after stirring for 15 min, an orange columnar solid is produced. The obtained solid was filtered, washed with acetone, and dried in an oven at 70° C. under normal pressure for 1 hour to obtain a metal-bipyridylium photocatalyst.

[0053] Wherein, the structure of ligand onium salt ...

Embodiment 3

[0057] The preparation of aldehyde: add the metal-bipyridylium photocatalyst Zn that embodiment 1 prepares in 10ml quartz centrifuge tube 2 C 48 N 8 Cl 6 h 52 o 8 (2mg) and 2mL acetone, then add 0.2mmol of different aromatic alcohols, turn on the LED light source, and irradiate the reaction under the condition of uniform stirring. After the reaction, the photocatalyst was separated from the solution, and the upper layer solution was taken by centrifugation, and the conversion rate of the reactant was detected by GC-2014C gas chromatography. The reaction products, illumination time, conversion rate and selectivity of different aromatic alcohols are shown in Table 1.

[0058] Conversion rate and selectivity of different aromatic alcohols in table 1 embodiment 1

[0059]

[0060] It can be seen from Table 1 that the selectivity of the catalytic reaction system is relatively high. Among them, the yield of the aromatic alcohol of the electron-donating group is higher than...

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Abstract

The invention belongs to the field of photocatalysis, and specifically relates to a metal-bipyridinium photocatalyst, a preparation method and its application. The catalyst is a compound composed of a bipyridinium salt and a metal salt; the bipyridinium salt is composed of a ligand and an anion. The method is as follows: dissolving bipyridinium salt in a solvent to obtain a ligand solution; dissolving a metal salt in a solvent to obtain a metal salt solution; mixing the ligand solution and the metal salt solution, stirring until precipitation occurs, and The precipitate is obtained after filtration, washing and drying. The photocatalyst can catalyze the oxidation of alcohol to aldehyde. Specifically, the reactant alcohol is dissolved in an organic solvent, a metal-bipyridinium photocatalyst is added, and a light source is used to irradiate the reaction for 0.5 to 30 hours while stirring. The photocatalyst is simple to prepare, does not use precious metals, has good recyclability, and has mild reaction conditions. Used in alcohol oxidation reactions, it has the characteristics of high activity, high selectivity and easy recovery.

Description

technical field [0001] The invention belongs to the field of photocatalysis, and in particular relates to a metal-bipyridylium photocatalyst, a preparation method and an application thereof. Background technique [0002] Aldehydes are an important class of fine chemical raw materials, widely used in the production and research and development of chemicals. Alcohols are a class of organic compounds with a wide range of sources and low prices, so the selective oxidation of alcohols to aldehydes has attracted the attention of chemical researchers for many years. The traditional oxidation of alcohols to aldehydes usually requires the use of a large number of oxidants, such as chromium oxide, manganese dioxide, periodic salt, and hydrogen peroxide. Disadvantages such as recycling. With people's increasing concern about the environment and energy, researchers began to explore the selective oxidation of alcohols using noble metal complexes such as palladium (Pd), ruthenium (Ru) a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D213/22
CPCC07C45/002C07F3/00C07F3/003C07F3/06B01J31/1815B01J2231/763B01J2531/26B01J2531/27B01J35/39C07C47/575C07C47/54C07C47/55
Inventor 张杰郭瑞云
Owner BEIJING INSTITUTE OF TECHNOLOGYGY
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