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Carbazolyl porous organic polymer-carried transition metal oxide catalyst and application thereof

A transition metal and carbazole-based technology, applied in 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 repeated use performance, high activity and stability, and long service life

Active Publication Date: 2019-03-12
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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  • Carbazolyl porous organic polymer-carried transition metal oxide catalyst and application thereof
  • Carbazolyl porous organic polymer-carried transition metal oxide catalyst and application thereof
  • Carbazolyl porous organic polymer-carried transition metal oxide catalyst and application thereof

Examples

Experimental program
Comparison scheme
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

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 carbazolyl porous organic polymer-carried transition metal oxide catalyst and a method for preparing p-methoxybenzaldehyde by oxidizing p-methoxytoluene. The carbazolyl porous organic polymer-carried transition metal oxide catalyst is prepared by taking carbazolyl porous organic polymers as the carrier, carrying transition metal oxides on the carrier and performing calcination. The skeleton of the carbazolyl porous organic polymers is provided with uniformly-distributed nitrogen atoms, which can to some extent interact with metal, so that the uniformly-distributed nitrogen atoms can activate the active sites of the metal oxides on the one hand and reduce loss of active components during reaction on the other hand. The carbazolyl porous organic polymer-carried transition metal oxide catalyst can efficiently catalyze p-methoxytoluene to prepare p-methoxybenzaldehyde and achieve a conversion rate and selectivity up to higher than 70%. Compared with traditional heterogeneous catalysts, the carbazolyl porous organic polymer-carried transition metal oxide catalyst is high in thermal stability, better in catalytic activity, less prone to loss of active componentsand longer in service life.

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 Applications(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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