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Preparation method and application of nano Cu-organic complex/Ag composite

A technology of organic complexes and composite materials, which is applied in the field of preparation of nano-Cu-organic complexes/Ag composite materials, can solve the problems of energy consumption and time consumption in the preparation of composite materials, achieve good industrial application prospects, reduce costs, and reduce poisoning Effect

Inactive Publication Date: 2016-02-17
SHANDONG NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This patent has the following deficiencies: (1) in the preparation of Cu-MOFSiO 2 At 50-70°C and 100W ultrasonic conditions, ethyl orthosilicate needs to be added dropwise in 40-70min, which shows that the preparation of the composite material consumes energy and time; (2) the metal-organic complex prepared by the invention Cu-MOF needs to be coated with shell silica on its surface to be used for catalytic reduction of 4-nitrophenol to 4-aminophenol in aqueous medium

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  • Preparation method and application of nano Cu-organic complex/Ag composite
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  • Preparation method and application of nano Cu-organic complex/Ag composite

Examples

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Embodiment 1

[0055] Example 1 Preparation of Ligand H 6 L

[0056] Ligand H 6 L is prepared by heating and reacting 5-aminoisophthalic acid and cyanuric chloride under alkaline conditions. The preparation steps are as follows:

[0057] Add 0.073mol of 5-aminoisophthalic acid, 0.117mol of sodium hydroxide and 0.085mol of sodium bicarbonate into 120mL of water; stir at room temperature for 30min, add 24mL of 1,4-cyanuric chloride containing 3.68g of cyanuric chloride dropwise within 5min Dioxane solution; heat the mixture to 100°C and continue to stir for 24 hours; after cooling to room temperature, neutralize the reaction solution to pH 5 with hydrochloric acid, filter with suction and wash with distilled water for 3 times, and dry to obtain the ligand H 6 L, the productive rate is 95%;

[0058] The ligand H 6 L, the construction formula is as follows:

[0059]

Embodiment 2

[0060] Example 2 Preparation of Cu-organic complex crystals by solvothermal method

[0061] 0.030g of H 6 L and 2 mL DMF, 2 mL DMSO and 100 μL H 2 O shaking and blending, adding 0.164g of Cu(NO 3 ) 2 ·3H 2 O After shaking and blending, add 0.9mL HBF 4 , the mixed solution was sealed in a reaction kettle, heated at 85°C for 3 days, and after natural cooling, the product was centrifuged and washed three times with anhydrous EtOH to obtain blue Cu-organic complex crystals, which were observed under a scanning electron microscope as regular octagonal crystals. Hedral crystal, the average particle size is about 20um;

[0062] Single crystal diffraction analysis shows that the Cu-organic complex crystal has the chemical formula [Cu 3 L(H 2 O) 3 ]·10H 2 O·5DMF is a 3D porous metal-organic framework, one of which consists of three Cu 2+ , a L 6- , three H 2 O molecular composition; its XRD pattern as attached figure 1 As shown, its 2θ has characteristic absorption at 4.1,...

Embodiment 3

[0063] Embodiment 3 A kind of preparation method of nanometer Cu-organic complex / Ag composite material

[0064] 0.17gCu(NO 3 ) 2 and 0.02g Ligand H 6 L was added to a mixed solvent of 0.4mL DMF and 0.4mL DMSO, and the two mixtures were blended and shaken for 6 seconds to obtain a Cu-organic complex gel; the Cu-organic complex gel was aged at 100°C 2 days, cooled to room temperature, washed 3 times with ethanol, dried to obtain nano Cu-organic complex crystals;

[0065] Described nanometer Cu-organic complex crystal, the XRD comparison of the Cu-organic complex crystal that obtains with solvent method sees attached figure 1 , the XRD pattern shows that the characteristic absorption peaks of the nano-Cu-organic complex crystal and the Cu-organic complex crystal prepared by the solvothermal method are the same, and 2θ has characteristic absorption at 4.1, 6.6, 81, 10.4, 12.1 and 16.0, This shows that the nano-Cu-organic complex crystal has the chemical formula [Cu 3 L(H 2 O...

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Abstract

The invention relates to a preparation method and application of a nano Cu-organic complex / Ag composite and belongs to the technical field of metal organic complexes, material science, nano materials, chemical industry, catalyzing and the like. Nano Cu-organic complex crystals with the grain size of 40 nm to 50 nm are adopted for loading nano-silver, due to the fact that the nano Cu-organic complex crystals comprise a large number of unsaturated loca, Ag+ can be selectively adsorbed, during UV-irradiation, Ag particles generated by in-situ reduction of Ag+ are anchored in the nano Cu-organic complex crystals, and therefore the composite is prepared. The cost of preparation raw materials is low, the process is simple and easy to operate, and reaction energy consumption is low. The composite can efficiently catalyze and reduce an aromatic nitrocompound into aromatic amine, and can catalyze phenylethylene oxide into styrene oxide.

Description

technical field [0001] The invention relates to a preparation method and application of a nano Cu-organic complex / Ag composite material, and belongs to the technical fields of metal organic complexes, material science, nanomaterials, chemical industry, catalysis and the like. Background technique [0002] Nanocrystals generally refer to ultrafine crystals with a particle size in the range of 1-100nm. Due to their fine grains and the presence of a large number of atoms in the grain boundaries and defect centers in the grains, it shows the characteristics that ordinary large particles do not have. Characteristics, that is, small size effect, surface effect, quantum size effect and macroscopic quantum tunneling effect, which lead to significant differences between the properties of light, magnetism, electricity, heat, force and chemical activity of nanocrystals and their bulk properties. [0003] Nano-noble metal particles have become an indispensable catalyst in the field of c...

Claims

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Application Information

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IPC IPC(8): B01J31/22C07C211/52C07C209/18C07D303/04C07D301/12B01D53/02
Inventor 匡芮石敬民郑鲁沂迟颜辉陈雪雪张程程
Owner SHANDONG NORMAL UNIV
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