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Method for preparing acetal or ketal under catalytic action of metal-organic frameworks

A metal-organic framework, catalytic preparation technology, applied in organic compound/hydride/coordination complex catalysts, organic chemistry, chemical instruments and methods, etc., can solve the problem that catalysts cannot be recycled, product separation is difficult, and reaction conditions are harsh. problem, to achieve the effect of high conversion rate and selectivity, simple process and easy separation

Inactive Publication Date: 2013-05-22
ANHUI UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to overcome the disadvantages of serious environmental pollution, harsh reaction conditions, difficult product separation and non-recyclable catalysts in the prior art, and provide a method for preparing acetal or ketal by metal-organic framework compound catalysis

Method used

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  • Method for preparing acetal or ketal under catalytic action of metal-organic frameworks

Examples

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Effect test

Embodiment 1

[0022] Example 1: Add 10mmol of n-butyraldehyde, 10mmol of 1,3-propanediol and 20mg of IRMOF-3-1 into a 25ml one-necked bottle with a stirring bar and a reflux condenser. Vigorously stirred at 80°C for 1 hour, cooled to room temperature and filtered, the filtrate was detected by gas chromatography with a conversion rate of 98%, a selectivity of 100%, and a yield of 98%. The filter residue was vacuum dried at 120°C for 8 hours to remove water and then recycled.

Embodiment 2

[0023] Example 2: 10mmol 1-butanone, 10mmol 2,2-dimethylpropanediol and 20mg IRMOF-3-1 were respectively added to a 25ml one-necked bottle with a stirring bar and a condenser. Vigorously stirred at 90°C for 2 hours, cooled to room temperature and filtered, the filtrate was detected by gas chromatography with a conversion rate of 97%, a selectivity of 100%, and a yield of 97%. The filter residue was vacuum-dried at 120°C for 8 hours to remove water and then recycled.

Embodiment 3

[0024] Example 3: 10mmol cyclohexanone, 10mmol 2,2-dimethylpropanediol and 22mg IRMOF-3-2 were respectively added to a 25ml one-necked bottle with a stirring bar and a condenser tube. The reaction was vigorously stirred at 100°C for 2 hours, cooled to room temperature and filtered. The filtrate was detected by gas chromatography with a conversion rate of 93%, a selectivity of 100%, and a yield of 93%. The filter residue was vacuum-dried at 120°C for 8 hours to remove water and then recycled.

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Abstract

The invention provides a method for preparing acetal or ketal under the catalytic action of metal-organic frameworks, belonging to the technical field of organic chemistry synthesis. In the acetal or ketal reaction, the mol ratio of aldehyde or ketone to alcohol is 1:(1-6), the molar weight of the metal-organic frameworks calculated on the basis of -SO3H is 10% of the aldehyde or ketone, the reaction temperature is 80-100 DEG C, the reaction time is 1-3 hours, and the reaction pressure is one atmosphere; the temperature is reduced to room temperature after the reaction; and the metal-organic framework catalyst obtained by filtration can be recycled after being subjected to vacuum dehydration at 120 DEG C. The method provided by the invention is environment-friendly; and the catalyst has the advantages of high conversion rate and high selectivity, and can be recycled many times while the catalytic activity is not obviously lowered.

Description

technical field [0001] The invention belongs to the technical field of organic chemical synthesis, and in particular relates to a method for preparing acetal or ketal by catalyzing a metal organic framework compound. Background technique [0002] Metal-organic frameworks (MOFs) are a new type of functional material that has received widespread attention, also known as porous coordination polymers, usually referring to metal ions or metal clusters and organic ligands that form a periodic infinite network structure through a self-assembly process. crystalline material. As a heterogeneous solid catalyst, it is similar to molecular sieves, with special topological structure, regularity of internal arrangement and pores of specific size and shape. However, in terms of chemical properties, metal-organic framework compounds are different from inorganic molecular sieves. Their pores are composed of metal and organic components, and they have greater activity and selectivity for org...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D319/06C07D319/08B01J31/22
Inventor 岳彩波伊廷锋
Owner ANHUI UNIVERSITY OF TECHNOLOGY
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