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Preparation of silica gel supported metalloporphyrin compound and application method thereof

A metalloporphyrin, immobilized technology, applied in the preparation of organic compounds, the preparation of carbon-based compounds, catalyst activation/preparation, etc., can solve the problem that the catalyst cannot be reused, the catalytic performance lacks stability, and the yield of acetophenone Low problems, to achieve the effect of promoting catalytic performance, less catalyst dosage, and improving yield and selectivity

Inactive Publication Date: 2009-10-21
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method utilizes metalloporphyrin as a catalyst, and the selectivity is poor, the yield of acetophenone is low, and industrialization is difficult; in addition, the catalyst cannot be reused, and the catalytic performance lacks stability, and is easily oxidized and deactivated by itself.

Method used

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  • Preparation of silica gel supported metalloporphyrin compound and application method thereof
  • Preparation of silica gel supported metalloporphyrin compound and application method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Example 1: Weigh 2.0000 g of the silica gel-immobilized porphyrin prepared in any of the above Examples 1, Example 2, and Example 3, soak in 45ml DMF, add 0.40g cobalt chloride, and react at 130°C for 1.5h, and reduce pressure A certain amount of solvent was recovered by distillation, the reaction solution was filtered while it was hot, washed with DMF, water, ethanol in turn, and dried to obtain 2.0159g of silica gel-supported metalloporphyrin, the metallization degree was 99.8%, and the solid load of cobalt porphyrin was 0.0903 g / g.

Embodiment 2

[0022] Example 2: Weigh 2.0000g of the silica gel immobilized porphyrin prepared in any of the above Examples 1, Example 2, and Example 3, soak in 40ml DMF, add 0.29g ferric chloride, react at 120°C for 2h, and distill under reduced pressure A certain amount of solvent is recovered, the reaction solution is filtered while it is hot, washed with DMF, water, ethanol, and dried to obtain 2.0151g of silica gel-supported metalloporphyrin, the degree of metallization is 99.5%, and the solid load of iron porphyrin is 0.0898g / g.

Embodiment 3

[0023]Example 3: Weigh 2.0000 g of the silica gel-immobilized porphyrin prepared in any of the above Examples 1, Example 2, and Example 3, soak in 50ml DMF, add 0.15g manganese chloride, and react at 110°C for 2.5 hours. A certain amount of solvent was recovered by distillation, the reaction solution was filtered while it was hot, washed with DMF, water, ethanol in turn, and dried to obtain 2.0134g of silica gel-supported metalloporphyrin, with a metallization degree of 99.0% and a solid loading of manganese porphyrin of 0.0811 g / g.

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Abstract

The invention belongs to the technical field of supported metalloporphyrins, and in particular relates to preparation of a silica gel supported metalloporphyrin compound and an application method thereof so as to solve the problems of preparing the metalloporphyrin compound in the prior art. The preparation steps are that: tetraphenylporphyrin, Lewis acid and trichloromethane are added with a chloromethylation reagent dropwise for thermostatic reaction, and chloromethylation tetraphenylporphyrin is obtained after treatment; the chloromethylation tetraphenylporphyrin is dissolved into DMF, the mixture is added with silica gel for temperature reaction, and the silica gel supported porphyrin is obtained after treatment; and the silica gel supported porphyrin is dissolved into the DMF, the mixture is subjected to temperature rise and added with metal salt or oxide for reaction, and the silica gel supported metalloporphyrin compound is obtained after treatment. The application method comprises that: phenylethane and the silica gel supported metalloporphyrin compound are introduced with O2 for the temperature reaction, and a main product hypnone is obtained after treatment. The invention has the advantages that: the reaction is easier, and the supported degree of the porphyrin is high; and in the application, the activity of a catalyst is effectively protected, the activities of the catalyst are promoted, and the yield and the selectivity of the main product are improved.

Description

Technical field [0001] The invention belongs to the technical field of immobilized metal porphyrins, and specifically relates to a preparation and application method of a silica gel immobilized metal porphyrin compound. Background technique [0002] Metallophophines (MPs) are an important class of biomimetic catalysts, which can mimic biological oxidases and achieve the catalytic activation of molecular oxygen under mild conditions, thereby making hydrocarbons highly efficient, selective and environmentally friendly. Oxidation. However, expensive MPs-based catalysts have two outstanding shortcomings, which limit their application in organic synthesis: (1) They are difficult to separate and inconvenient to recycle; (2) The catalytic performance lacks stability and is prone to self-oxidation loss. live. An important way to overcome the above problems is to immobilize metalloporphyrins, such as using silica gel, zeolite, clay, and organic polymers as supports for heterogeneous catal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22B01J37/00C07C49/78C07C45/36
CPCY02P20/50
Inventor 王蕊欣焦纬洲高保娇
Owner ZHONGBEI UNIV
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