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Catalysis and Application of Carbazole-Based Porous Organic Polymer Supported Transition Metal Oxide

A transition metal and carbazole-based technology, which is applied in the direction of organic compound/hydride/coordination complex catalysts, preparation of organic compounds, physical/chemical process catalysts, etc., can solve the problem of insufficient activity of active centers and loss of active components and other problems, to achieve the effect of good reusability, high activity and stability, and high specific surface area

Active Publication Date: 2021-06-01
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Supported catalyst is a commonly used recyclable catalyst, but it often faces problems such as the loss of active components to varying degrees, and the activity of the active center is not high enough, and the choice of carrier is very important to solve the above problems

Method used

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  • Catalysis and Application of Carbazole-Based Porous Organic Polymer Supported Transition Metal Oxide
  • Catalysis and Application of Carbazole-Based Porous Organic Polymer Supported Transition Metal Oxide
  • Catalysis and Application of Carbazole-Based Porous Organic Polymer Supported Transition Metal Oxide

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Experimental program
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Effect test

Embodiment 1

[0023] The preparation of embodiment 1 material A

[0024] 1) Weigh 2.0g of ferric chloride, replace it with nitrogen, add 70ml of anhydrous chloroform, then add dropwise 0.8g of 1,3,5-tris(9-carbazolyl)benzene dissolved in 70ml of anhydrous chloroform, Stirring at room temperature for 36 hours, washing, suction filtration, concentrated hydrochloric acid washing, Soxhlet extraction, and vacuum drying to obtain a carbazole-based porous organic polymer.

[0025] 2) Weigh 0.2g of carbazole-based porous organic polymer, add 40mg of cobalt acetate tetrahydrate, add 5ml of ethanol, and stir at 40°C for 24h;

[0026] 3) After impregnation, ethanol was removed by a rotary steamer, dried in an oven at 80°C for 12h, and calcined in a muffle furnace at 300°C for 3h to obtain material A.

Embodiment 2

[0027] The preparation of embodiment 2 material B-E

[0028] The preparation method of material B-E is the same as that of material A, the difference lies in the selection of metal salt, loading and calcination temperature. The obtained materials are listed in Table 1.

[0029] Table 1 Metal salts, loads and calcination temperatures used in materials B-E

[0030] Material metal salt Loading capacity (wt%) Calcination temperature (℃) B CoCl 2 ·6H 2 o

Embodiment 3

[0031] The preparation of embodiment 3 material F

[0032] 1) Weigh 2.0g of ferric chloride, replace it with nitrogen, add 70ml of anhydrous chloroform, then add dropwise 0.8g of 1,3,5-tris(9-carbazolyl)benzene dissolved in 70ml of anhydrous chloroform, Stirring at room temperature for 36 hours, washing, suction filtration, concentrated hydrochloric acid washing, Soxhlet extraction, and vacuum drying to obtain a carbazole-based porous organic polymer.

[0033] 2) Weigh 0.2g of carbazole-based porous organic polymer, add 80mg of manganese acetate tetrahydrate, add 5ml of ethanol, and stir at 40°C for 24h;

[0034] 3) After the impregnation, ethanol was removed by a rotary steamer, dried in an oven at 80°C for 12h, and calcined in a muffle furnace at 400°C for 3h to obtain material F.

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Abstract

The invention discloses a method for preparing p-methoxybenzaldehyde by catalyzing p-methoxytoluene oxidation with carbazole-based porous organic polymer supported transition metal oxide. The catalyst uses a carbazole-based porous organic polymer as a carrier, and after loading a transition metal salt, obtains a transition metal oxide catalyst supported by a carbazole-based porous organic polymer through calcining. Since there are evenly distributed nitrogen atoms on the skeleton of the carbazole-based porous organic polymer, the nitrogen atoms have certain interactions with metals. Therefore, the uniformly distributed nitrogen atoms on the one hand activate the metal oxide active sites; on the other hand, reduce the loss of active components during the reaction. The catalyst can efficiently catalyze p-methoxytoluene to prepare p-methoxybenzaldehyde, and both the conversion rate and selectivity can reach more than 70%. Compared with traditional heterogeneous catalysts, the catalyst has high thermal stability, good catalytic activity, active components are not easily lost, and the service life of the catalyst is long.

Description

technical field [0001] The invention relates to the field of chemistry and chemical engineering, in particular to a carbazole-based porous organic polymer material post-supported cobalt manganese oxide catalyst and its application in the preparation of p-methoxybenzaldehyde by oxidation of p-methoxytoluene. Background technique [0002] P-methoxybenzaldehyde, also known as anisaldehyde, is generally a colorless or light yellow liquid at room temperature, with a long-lasting hawthorn aroma. It is a spice with high economic value and an important organic chemical synthesis intermediate. It is also an intermediate for the preparation of porphyrin-type photosensitizers, aminocarbyl penicillins, etc. At present, the methods for synthesizing p-methoxybenzaldehyde can be mainly divided into the synthesis of p-propenyl anisole, methoxybenzyl alcohol, phenol, p-hydroxybenzaldehyde, anisole, p-methoxytoluene, etc. route. [0003] In the process of preparing p-methoxybenzaldehyde fro...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/28B01J31/32C07C45/36C07C47/575
CPCB01J31/06B01J31/28B01J31/32B01J2231/70C07C45/36C07C47/575
Inventor 徐杰刘梦石松赵丽杜文强高进苗虹
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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