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Heteropolyacid-doped Schiff base macrocyclic dinuclear manganese complex catalyst and its synthesis and application

A technology of a binuclear manganese complex and a Schiff base macrocycle is applied to a heteropolyacid-doped Schiff base macrocyclic binuclear manganese complex catalyst and the fields of synthesis and application thereof, and can solve the problem of waste acid discharge, large consumption, high consumption, etc. of corrosion equipment. Pollution of the environment and other problems, to achieve the effect of easy regeneration, easy recovery and high conversion rate

Inactive Publication Date: 2016-03-02
WUHAN INSTITUTE OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although sulfuric acid can make the esterification reaction go smoothly, there are a series of problems such as large dosage, corrosion of equipment and waste acid discharge to pollute the environment.

Method used

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  • Heteropolyacid-doped Schiff base macrocyclic dinuclear manganese complex catalyst and its synthesis and application

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The preparation of catalyst 1 (substituent R=F on the benzene ring):

[0016] 1) Sodium hydroxide (12g, 0.3mol) was placed in a 250mL three-necked flask, and 40mL of distilled water was added to dissolve it. 4-Fluoro-phenol (33.63 g, 0.3 mol) was added to the sodium hydroxide solution under cooling in an ice bath. Stir to make it all dissolve (it can be observed that the solution is clear and transparent). Add 37%-40.0% formaldehyde solution (60mL) dropwise to the above mixed solution, and complete the dropwise addition within 15-20min (the phenomenon of temperature rise will occur during the dropping process, keep the reaction temperature below 5°C), Stirring was continued for 30 min. The solution is light yellow, change the condition of the ice bath to heating in an oil bath, control the temperature of the solution at about 45°C and react for 8 hours (after 60 minutes, the color becomes darker and gradually changes from colorless to a red transparent solution), cool...

Embodiment 2

[0024] Catalyst 2 (substituent R=CH on the benzene ring 3 When) preparation is identical with the preparation method of catalyst 1;

Embodiment 3

[0026] The preparation of catalyst 3 (when the substituent on the benzene ring is R=Cl) is the same as that of catalyst 1.

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Abstract

The invention relates to a heteropoly acid-doped Schiff base macrocyclic binuclear manganese complex catalyst and synthesis and application thereof. The catalyst is prepared by the following steps: adding 4-R-phenol into a solution of sodium hydroxide under an ice bath cooling condition; adding formaldehyde, stirring, heating, cooling, regulating the pH, filtering, washing, recrystallizing and drying to obtain 2,6-dihydroxytoluene-4-R-phenol; mixing manganese dioxide and trichloromethane; performing heating reflux; filtering and washing a product on manganese dioxide by using trichloromethane; evaporating a solvent to obtain a crude product; recrystallizing, purifying and drying to obtain 2,6-diformyl-4-R-phenol; dropwise adding an ethanol solution of ethanediamine into manganese chloride tetrahydrate; stirring, filtering obtained precipitate, washing, dissolving into methyl alcohol, adding silicotungstic acid, stirring the solution, filtering, washing and drying. The catalyst is easy to prepare, noncorrosive to equipment, environment-friendly, high in transformation rate in a catalytic esterification reaction, and easy to recycle.

Description

technical field [0001] The invention relates to a class of catalysts, in particular to a class of heteropolyacid-doped Schiff base macrocyclic dinuclear manganese complex catalysts and their synthesis and application. technical background [0002] For a long time, the synthesis of esters has always followed the method of direct esterification of alkyds using inorganic acids, especially sulfuric acid, as a catalyst. Although sulfuric acid can make the esterification reaction go smoothly, there are a series of problems such as large dosage, corrosion of equipment and pollution of waste acid discharge to the environment. At home and abroad, we have been exploring the use of alternative acidic catalysts and non-acidic catalysts as catalysts for ester synthesis, solid acid catalysts, including molecular screening catalysts, solid superacid catalysts, composite solid superacid catalysts and solid heteropolyacid catalysts. Among them, the heteropoly acid type catalyst has the char...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22C07C67/08C07C69/63
Inventor 程清蓉潘志权周红
Owner WUHAN INSTITUTE OF TECHNOLOGY