Sandwiched Zr-MOFs (Metal-organic Frameworks)/graphene composite photocatalyst as well as preparation method and application thereof

A graphene composite and photocatalyst technology, applied in the direction of organic compound/hydride/coordination complex catalyst, physical/chemical process catalyst, organic compound preparation, etc., can solve the problem of graphene composite and reduce the conductivity of graphene efficiency and other issues, to achieve excellent photocatalytic performance, improve photocatalytic efficiency, and inhibit the effect of recombination

Inactive Publication Date: 2014-12-10
FUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] The preparation methods of MOFs / graphene composite materials reported in the above documents and invention patents have the following two problems: (1) The raw materials (metal salts and organic ligands) for the synthesis of MOFs are directly synthesized by using unmodified graphene. In-situ recombination, due to the strong coordination between metal ions and organic ligands, it is easy to cause unsatisfactory recombination with graphene
(2) Use chemically modified graphene with a certain amount of functional groups on the surface that can bond and coordinate with metal ions as a precursor, and further combine it with the raw materials for synthesizing MOFs (metal salts and organic ligands). In-situ recombination, although graphene and MOFs materials can be grafted through the coordination between metal ions and ligands on the graphene surface, more defects will inevitably be introduced during the chemical modification of graphene , greatly reducing the conductivity of graphene

Method used

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  • Sandwiched Zr-MOFs (Metal-organic Frameworks)/graphene composite photocatalyst as well as preparation method and application thereof
  • Sandwiched Zr-MOFs (Metal-organic Frameworks)/graphene composite photocatalyst as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Weigh 318 mg zirconium tetrachloride (ZrCl 4 ) and 245.2 mg of 2-aminoterephthalic acid (2-NH 2 -H 2 BDC), added to 150 ml of DMF (N,N'-dimethylformamide), stirred at room temperature at a stirring rate of 700 rpm for 60 minutes, and the solution obtained after stirring was transferred to a 50 ml autoclave in batches reaction in an oven at 120°C for 48 hours, after the time was up, take it out and cool it in the air to room temperature, centrifuge, exchange methanol for 5 days, and dry it in a vacuum oven at 80°C to obtain an amino group-containing Zr-MOF material. Weigh 25 mg of the prepared Zr-MOF material into a glass reactor, add 2.5 ml of pre-saturated benzotrifluoride and 0.5 mmol (50 microliters) of benzyl alcohol, seal it, and use a xenon lamp light source with a wavelength ≥ 420 nm 8 hours of light.

Embodiment 2

[0031] Take 1 milliliter of the aqueous phase dispersion of graphite oxide with a concentration of about 1.6 mg per milliliter in 150 milliliters of DMF (N,N'-dimethylformamide), and sonicate for 30-40 minutes to obtain a brown-yellow solution A; Add 14.3 mg of trimethyl-(2-oxo-2-pyrene-1-yl-ethyl)-ammonium bromide (pyrene + ), and then sonicated for 30-40 minutes to obtain a bright yellow solution B; add 245.2 mg of 2-aminoterephthalic acid (2-NH 2 -H 2 BDC), stirred overnight at room temperature; then added 318 mg of zirconium tetrachloride (ZrCl 4 ) and 245.2 mg of 2-aminoterephthalic acid (2-NH 2 -H 2 BDC), and then stirred at room temperature for 60 minutes at a stirring rate of 700 rpm; the solution obtained after stirring was transferred to a 50 ml high-pressure reactor in batches, and reacted in an oven at 120 ° C for 48 hours, and was taken out after the time was up. Cool to room temperature in the air, centrifuge, exchange methanol for 5 days, and dry in a vacuum...

Embodiment 3

[0033] Take 4 ml of the aqueous dispersion of graphite oxide with a concentration of about 1.6 mg per ml in 150 ml of DMF (N,N'-dimethylformamide), and sonicate for 30-40 minutes to obtain a brownish yellow solution A; Add 14.3 mg of 3-methyl(2-oxo-2-pyrene-1-yl-ethyl)ammonium bromide (pyrene + ), and then sonicated for 30-40 minutes to obtain a bright yellow solution B; add 245.2 mg of 2-aminoterephthalic acid (2-NH 2 -H 2 BDC), stirred overnight at room temperature; then added 318 mg of zirconium tetrachloride (ZrCl 4 ) and 245.2 mg of 2-aminoterephthalic acid (2-NH 2 -H 2 BDC), and then stirred at room temperature for 60 minutes at a stirring rate of 700 rpm; the solution obtained after stirring was transferred to a 50 ml high-pressure reactor in batches, and reacted in an oven at 120 ° C for 48 hours, and was taken out after the time was up. Cool to room temperature in the air, centrifuge, exchange methanol for 5 days, and dry in a vacuum oven at 80 °C to obtain a Zr-M...

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Abstract

The invention provides a sandwiched Zr-MOFs (Metal-organic Frameworks) / graphene composite photocatalyst as well as a preparation method and an application of the photocatalyst. The composite photocatalyst is a material with a sandwich-like structure, formed by a zirconium-containing metal-organic framework compound Zr-BDC-NH2 and graphene through compounding, wherein the graphene is 0.5-5.0% in mass fraction, the modified oxidized graphene is used as a graphene precursor, and a non-covalent self-assembly in-situ solvent thermal method is adopted for preparation; compared with the Zr-MOFs which is not loaded with graphene, the sandwiched Zr-MOFs / graphene composite photocatalyst has the photocatalytic performance improved remarkably, and can transform aromatic alcohol organic matters into the corresponding aromatic aldehyde substances in a high-selectivity manner under the excitation of visible light with 420-800 nanometers, the selectivity is 100% and the primary conversion rate can reach 70%. The non-covalent self-assembly in-situ solvent thermal method is simple and is easy to operate, and the prepared sandwiched Zr-MOFs / graphene composite photocatalyst has excellent capability of selectively oxidizing aromatic alcohol substances under a photocatalytic condition, and has important promotion significance on clean and high-efficiency industrial production of fine chemicals.

Description

technical field [0001] The invention belongs to the field of photocatalysts, and in particular relates to a sandwich structure Zr-MOFs / graphene composite photocatalyst, its preparation and its application in the synthesis of aromatic aldehyde chemicals. Background technique [0002] Aromatic aldehydes are a class of important chemicals widely used in spices, food additives, medicines, dyes, pesticides, coatings and liquid crystal materials. Its synthesis and preparation play a pivotal role in the chemical industry. Generally, aromatic aldehyde compounds can be prepared by chemical synthesis, electrolytic synthesis and phase transfer catalysis. The chemical synthesis is mainly divided into direct chemical reaction synthesis and indirect chemical reaction synthesis in terms of raw materials and routes. The direct chemical reaction is to directly introduce a formyl group into the benzene ring or introduce other groups and then convert it into a formyl group through a chemical ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07C45/29C07C47/54C07C47/55C07C205/44C07C201/12
Inventor 龙金林徐洁王绪绪张子重林华香
Owner FUZHOU UNIV
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