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Preparation method and application of a functional coordination polymer

A coordination polymer and functionalization technology, applied in the preparation of organic compounds, preparation of amino hydroxyl compounds, organic compound/hydride/coordination complex catalysts, etc., can solve the problem of large specific surface energy, easy agglomeration, catalytic Reduced activity and other issues, to achieve uniform crystal size, reduce production costs, and high catalytic activity

Inactive Publication Date: 2017-03-01
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to improve the catalytic activity of nano-silver, the purpose of its preparation is to obtain monodisperse and shape-controllable particles, but because of its large specific surface energy, it is easy to agglomerate during the synthesis and catalytic process, resulting in a decrease in its catalytic activity.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] A preparation method of 3-ethyl-1,2,4-triazole: to 54ml of propionic acid, add 50ml of hydrazine hydrate with a mass fraction of 80%, stir to release heat, heat and reflux for 8h; after cooling slightly, Start heating and distillation. When the temperature reaches above 220°C, stop the distillation and continue to reflux for 2 hours. The temperature is stable at 170±1°C; cool and filter to obtain colorless crystals of 4-amino-3-ethyl-1,2,4- Triazole, the productive rate is 77%;

[0028] Take 11g of 4-amino-3-ethyl-1,2,4-triazole, add 20ml of 6mol / L dilute HCl, add 150ml of aqueous solution containing 13g of sodium nitrite, stir at 25°C for 2h, and use a rotating Evaporate to dryness with an evaporator, add 60ml of absolute ethanol and heat to reflux for 30min, cool to room temperature, and evaporate to dryness with a rotary evaporator to obtain a yellow crystal substance, which is dissolved by heating with 100ml of toluene and recrystallized to obtain a colorless needle...

Embodiment 2

[0030]A preparation method of 3-ethyl-1,2,4-triazole: to 54ml of propionic acid, add 56ml of hydrazine hydrate with a mass fraction of 80%, stir to exotherm, heat to reflux for 10h; after cooling slightly, Start heating and distilling, when the temperature reaches above 220°C, stop the distillation, continue to reflux for 3h, the temperature is stable at 170±1°C; cool and filter to obtain colorless crystal 4-amino-3-ethyl-1,2,4- Triazole, the productive rate is 80%;

[0031] Take 11g of 4-amino-3-ethyl-1,2,4-triazole, add 25ml of 6mol / L dilute HCl, add 150ml of an aqueous solution containing 15g of sodium nitrite, stir at 28°C for 2h, and use a rotating Evaporate to dryness with an evaporator, add 60ml of absolute ethanol and heat to reflux for 30min, cool to room temperature, and evaporate to dryness with a rotary evaporator to obtain a yellow crystal substance, which is dissolved by heating with 100ml of toluene and recrystallized to obtain a colorless needle-shaped crystal,...

Embodiment 3

[0033] A preparation method of 3-ethyl-1,2,4-triazole: to 54ml of propionic acid, add 54ml of hydrazine hydrate with a mass fraction of 80%, stir to exotherm, heat to reflux for 9h; after cooling slightly, Start heating and distillation. When the temperature reaches above 220°C, stop the distillation and continue to reflux for 2-3h, the temperature is stable at 170±1°C; cool and filter to obtain colorless crystals of 4-amino-3-ethyl-1,2, 4-triazole, the productive rate is 78%;

[0034] Take 11g of 4-amino-3-ethyl-1,2,4-triazole, add 23ml of 6mol / L dilute HCl, add 150ml of an aqueous solution containing 14g of sodium nitrite, stir at 26°C for 2h, and use a rotating Evaporate to dryness with an evaporator, add 60ml of absolute ethanol and heat to reflux for 30min, cool to room temperature, and evaporate to dryness with a rotary evaporator to obtain a yellow crystal substance, which is dissolved by heating with 100ml of toluene and recrystallized to obtain a colorless needle-shap...

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Abstract

The present invention relates to a preparation method and applications of a functional coordination polymer, and belongs to the technical fields of material science, nanometer materials, catalysis and the like. According to the present invention, polyvinylpyrrolidone, silver nitrate and 3-ethyl-1,2,4-triazole are adopted as main raw materials to prepare Ag@MOF, and a porous titanium dioxide shell layer is coated on the surface to prepare the functional coordination polymer Ag@MOF@TiO2. The polymer has the excellent performance of catalytic reduction of 4-nitrophenol into 4-aminophenol and catalytic oxidation of styrene into styrene oxide, and has good application prospects in heterogeneous catalytic reduction and oxidation reactions.

Description

technical field [0001] The invention relates to a preparation method and application of a functionalized coordination polymer, in particular to an Ag@MOF @TiO 2 The preparation method and the application of catalytic reduction of 4-nitrophenol to 4-aminophenol and catalytic oxidation of styrene to phenyloxirane belong to the technical fields of material science, nanomaterials, metal-organic complexes, chemical industry, and catalysis . Background technique [0002] Metal-organic frameworks (MOFs) are currently a hot field in materials science, metal-organic complexes, chemical engineering, and catalysis research. It is an organic ligand that connects inorganic metal ions or metal ion clusters through coordination bonds. A crystalline material that forms an infinitely extending network. The biggest feature of MOFs is that it is a crystalline material, but it has high porosity and large internal specific surface area. The structure of inorganic metal ions or metal ion clust...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/38C07F1/10C07C215/76C07C213/02C07D303/04C07D301/19
Inventor 王志玲于洋洋张书香郑鲁沂
Owner UNIV OF JINAN
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