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Application of sea urchin-shaped cobalt-based photocatalyst in synthesis of benzoazacycle by converting CO2

A photocatalyst, sea urchin-shaped technology, applied in the field of photocatalysis, can solve the problems of low catalytic efficiency, complex preparation, poor economy, etc., and achieve the effect of high photocatalytic efficiency, low preparation difficulty, and few reaction components

Active Publication Date: 2020-11-03
HANGZHOU NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] The present invention is to overcome prior art with CO 2 In the synthesis reaction of benzazepine heterocycle, high temperature activation of CO 2 The energy consumption of the reaction is too high and the economy is poor, the specific surface area of ​​the existing photocatalyst is small, which leads to the shortcomings of low catalytic efficiency, complicated preparation, and high cost. A sea urchin-like cobalt-based photocatalyst is provided to convert CO 2 The application in the synthesis of benzazepine heterocycles can effectively reduce CO 2 The reaction activation energy can reduce the reaction temperature and improve the economy of the reaction; and the sea urchin-like cobalt-based photocatalyst has a large specific surface area and high catalytic efficiency, and is simple to prepare and low in cost

Method used

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  • Application of sea urchin-shaped cobalt-based photocatalyst in synthesis of benzoazacycle by converting CO2
  • Application of sea urchin-shaped cobalt-based photocatalyst in synthesis of benzoazacycle by converting CO2
  • Application of sea urchin-shaped cobalt-based photocatalyst in synthesis of benzoazacycle by converting CO2

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preparation example Construction

[0032] A sea urchin-like cobalt-based photocatalyst provided by the invention is effective in converting CO 2 The application in the synthesis of benzazepine rings, wherein the preparation method of the catalyst specifically comprises the following steps:

[0033] (1) Put 1 to 2 mol of p-aminobenzoic acid into 10 to 20 mL of a mixed solution containing equal volumes of DMF and ethanol, and stir for 10 to 30 minutes to obtain the organic ligand L;

[0034] (2) Add 1.5mol Co(NO 3 ) 2 ·6H 2 O, stirring for 10 to 30 minutes to form a mixed solution;

[0035] (3) Transfer the mixed solution to a stainless steel autoclave with a Teflon liner, put it into a drying oven at 150-230° C. and heat it for 10-20 hours, and after cooling to 20-30° C., filter to obtain the primary product of the catalyst;

[0036] (4) Wash the catalyst primary product with 5-10mL DMF and 5-10mL ethanol respectively until its weight no longer changes, then dry the catalyst primary product in a vacuum oven ...

Embodiment 1

[0041] A sea urchin-like cobalt-based photocatalyst in the conversion of CO 2 The application in the synthesis of benzazepine rings, wherein the preparation method of the catalyst specifically comprises the following steps:

[0042] (1) Put 1mol p-aminobenzoic acid into 10mL mixed solution containing equal volume of DMF and ethanol, stir for 10 minutes to obtain organic ligand L;

[0043] (2) Add 1.5mol Co(NO 3 ) 2 ·6H 2 O, stirred for 10 minutes to form a mixed solution;

[0044] (3) Transfer the mixed solution to a stainless steel autoclave with Teflon lining, put it into a drying oven at 150° C. and heat it for 10 hours, and after cooling to 25° C., filter to obtain the catalyst primary product;

[0045] (4) Wash the primary catalyst product 3 times with 5mL DMF and 5mL ethanol, until its weight no longer changes, then dry the primary catalyst product in a vacuum oven at 70°C for 10 hours to obtain the final product of sea urchin-like cobalt-based photocatalyst .

[0...

Embodiment 2

[0050] A sea urchin-like cobalt-based photocatalyst in the conversion of CO 2The application in the synthesis of benzazepine rings, wherein the preparation method of the catalyst specifically comprises the following steps:

[0051] (1) Put 1.5mol p-aminobenzoic acid into 15mL mixed solution containing equal volume of DMF and ethanol, stir for 20 minutes to obtain organic ligand L;

[0052] (2) Add 1.5mol Co(NO 3 ) 2 ·6H 2 O, stirred for 20 minutes to form a mixed solution;

[0053] (3) Transfer the mixed solution to a stainless steel autoclave with Teflon lining, put it into a drying oven at 200° C. and heat it for 15 hours, and after cooling to 25° C., filter to obtain the catalyst primary product;

[0054] (4) Wash the primary catalyst product 3 times with 7mL DMF and 7mL ethanol, until its weight no longer changes, then dry the primary catalyst product in a vacuum oven at 80°C for 12 hours to obtain the final product of sea urchin-like cobalt-based photocatalyst .

[...

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Abstract

The invention relates to the technical field of photocatalysis, in particular to application of a sea urchin-shaped cobalt-based photocatalyst to synthesis of benzoazacycle by converting CO2. A complex is of a sea urchin-shaped microsphere structure, which is composed of an organic ligand L and cobalt nitrate hexahydrate and is formed by arranging a plurality of nano needle-shaped complex crystals. The main body of the organic ligand L is p-aminobenzoic acid; the application comprises the following steps: introducing CO2 into a solution containing o-phenylenediamine compounds, carrying out carbonylation reaction and cyclization with o-phenylenediamine compounds under the action of the urchin-shaped cobalt-based catalyst to generate the benzoazacycle compounds. The sea urchin-shaped microsphere structure cobalt-based catalyst formed by the obtained nano needle-shaped complex crystal has a very large specific surface area and high photocatalytic efficiency; when the photocatalyst is adopted to catalyze and activate CO2, the reaction for synthesizing the benzoazacycle by converting CO2 can be carried out at room temperature, so that the energy consumption is greatly reduced, and the cost is reduced.

Description

technical field [0001] The invention relates to the technical field of photocatalysis, in particular to a sea urchin-like cobalt-based photocatalyst in the conversion of CO 2 Applications in the synthesis of benzazepine rings. Background technique [0002] Benzazine heterocyclic compounds are a class of substances widely used in plastics, inks and other industries. For example, benzopyrazolone organic pigments are high-grade organic pigments with excellent application performance, high coloring strength, and good Heat resistance and solubility resistance; as a renewable and abundant greenhouse gas, how to recover and utilize carbon dioxide has gradually become a major topic in chemical synthesis reactions, such as in "Chemistry World" 2012 S1 8-9 in the article "Carbon Dioxide as Carbonylating Reagent for the Synthesis of Benzimidazolones", the CO 2 As a carbonylation reagent, it can be condensed with o-phenylenediamine under alkaline conditions to synthesize benzimidazolo...

Claims

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Application Information

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IPC IPC(8): C07D235/26B01J31/22B01J35/00B01J35/02B01J35/10
CPCC07D235/26B01J31/2226B01J2531/845B01J2540/40B01J2540/68B01J35/50B01J35/60B01J35/39
Inventor 郑辉杨思炜沈圆芳屠雪薇胡安康
Owner HANGZHOU NORMAL UNIVERSITY
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