A method for preparing acetal (ketone) catalyzed by an acidic magnetic material containing -so3h

A technology of -SO3H and magnetic materials, applied in the preparation of organic compounds, chemical instruments and methods, organic compound/hydride/coordination complex catalysts, etc., can solve the problem of high catalyst preparation price, large catalyst usage, post-treatment Complex process and other issues, to achieve the effect of easy industrialized large-scale production, poor miscibility, and high reaction selectivity

Active Publication Date: 2016-04-27
ANHUI UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to overcome the disadvantages of the existing catalytic preparation of acetal (ketone) technology that the amount of catalyst used is large, the amount of loss in recycling is large, the price of catalyst preparation is high, and the post-treatment process is complicated, etc., and provide a kind of acidity higher, Inexpensive and easy to prepare containing -SO 3 Acidic magnetic material of H catalyzes the method for preparing acetal (ketone)

Method used

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  • A method for preparing acetal (ketone) catalyzed by an acidic magnetic material containing -so3h
  • A method for preparing acetal (ketone) catalyzed by an acidic magnetic material containing -so3h
  • A method for preparing acetal (ketone) catalyzed by an acidic magnetic material containing -so3h

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Example 1: 10 mmol of n-butyraldehyde, 10 mmol of 1,3-propanediol and 2.72 g of acidic magnetic material were added to a 25 ml single-necked bottle with a stirring bar and a condenser. The reaction was vigorously stirred at 110° C. for 0.75 h, cooled to room temperature after the reaction, and the catalyst was sucked out with a magnet. The conversion rate of n-butyraldehyde was 97% as detected by the gas chromatography of the reaction liquid, the selectivity of the product n-butyraldehyde 1,3-propanediol acetal was 100%, and the calculated yield was 97%. The catalyst was recycled without treatment.

Embodiment 2

[0024] Example 2: 10mmol of benzaldehyde, 15mmol of 1,3-propanediol and 3.04g of acidic magnetic material were added to a 50ml single-necked bottle with a stirring bar and a condenser. The reaction was vigorously stirred at 110° C. for 1.5 h, cooled to room temperature after the reaction, and the catalyst was sucked out with a magnet. The conversion rate of benzaldehyde was 93% as detected by the gas chromatography of the reaction liquid, the selectivity of the product benzaldehyde 1,3-propanediol acetal was 100%, and the calculated yield was 93%. The catalyst was recycled without treatment.

Embodiment 3

[0025] Example 3: 10mmol of p-nitrobenzaldehyde, 25mmol of ethylene glycol and 2.41g of acidic magnetic material were added to a 50ml single-necked bottle with a stirring bar and a condenser. The reaction was vigorously stirred at 110° C. for 2 h, cooled to room temperature after the reaction, and the catalyst was sucked out with a magnet. Reaction liquid gas chromatography detects that the conversion rate of p-nitrobenzaldehyde is 96%, and the selectivity of product p-nitrobenzaldehyde-ethylene glycol acetal is 100%, and its productive rate is calculated as 96%, and the catalyzer is circulated without treatment use.

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Abstract

The invention discloses a method for preparing acetal (ketone) by catalyzing an acidic magnetic material containing -SO3H, which belongs to the technical field of chemical material and preparation thereof. According to the invention, mol ratio of aldehyde or ketone to alcohol used in the preparation method is 1: (1-5), mole of the acidic magnetic material catalyst accounts for 8-10% of that of the used aldehyde or ketone by calculating -SO3H, reaction temperature is 110 DEG C, the reaction time is 0.5-3 hours, the reaction pressure is one atmospheric pressure, a cooling step is carried out to room temperature after reaction is completed, the catalyst is sucked by a magnet, and the conversion rate, selectivity and acetal(ketone) yield of the reaction raw material are detected by a reaction solution through a gas chromatograph. Compared with the preparation method of other catalysts, the method has the advantages of high reaction selectivity, simple separation of the catalyst and the product, the catalyst enables cycle usage without any treatment, the operation of whole preparation process is simple, the economic benefit is high, and the method is convenient for industrial large scale production.

Description

technical field [0001] The invention belongs to the technical field of chemical materials and their preparation, in particular to a 3 The acidic magnetic material of H catalyzes the method for preparing acetal (ketone). Background technique [0002] Acetal (ketone) is an important intermediate in the chemical industry, often used for the protection of aldehydes or ketones, and even as a special reaction solvent. The traditional method of preparing acetal (ketone) is carried out under the catalysis of inorganic acid (sulfuric acid, hydrochloric acid, phosphoric acid, etc.), but this method has many side reactions, serious equipment corrosion, low product purity, cumbersome post-treatment, and produces three wastes pollute. Therefore, the development of new catalysts for acetals (ketones) that are green, efficient, recyclable, and easily separated from products has aroused great interest among chemists. [0003] In recent years, acidic ionic liquids, especially Bronster aci...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D319/06C07D317/16C07D319/08C07C43/303C07C41/56B01J31/28
CPCC07C41/56C07C43/303C07D317/16C07D319/06C07D319/08
Inventor 岳彩波粱莹吴胜华查荣轩叶晨廖凯储昭莲
Owner ANHUI UNIVERSITY OF TECHNOLOGY
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