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Method for preparing butyl butyrate through direct catalytic conversion of n-butyraldehyde

A technology of butyl butyrate and n-butyraldehyde, which is applied in the field of direct catalytic conversion of n-butyraldehyde to butyl butyrate, can solve the problems of long preparation route of butyl butyrate, many side reactions, equipment corrosion, etc., and achieve raw material conversion High efficiency and product selectivity, good atom economy, and mild reaction conditions

Active Publication Date: 2020-06-02
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

[0020] In order to solve the current problems such as long preparation route of butyl butyrate, severe equipment corrosion, many side reactions, dark product color, complex post-treatment process, large discharge of "three wastes" and high production cost, the purpose of the present invention is to develop a A method for preparing butyl butyrate by direct catalytic conversion of n-butyraldehyde has the advantages of short route, good atom economy, mild reaction conditions, recyclable catalyst, high conversion rate of raw materials and high product selectivity

Method used

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  • Method for preparing butyl butyrate through direct catalytic conversion of n-butyraldehyde
  • Method for preparing butyl butyrate through direct catalytic conversion of n-butyraldehyde
  • Method for preparing butyl butyrate through direct catalytic conversion of n-butyraldehyde

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Add 20 grams of n-butyraldehyde and 0.2 g of aluminum oxalate (1% of the mass of n-butyraldehyde) into a 100 ml two-necked round-bottomed flask equipped with a condenser, stir evenly, control the reaction temperature to 10°C by a refrigerator, and react for 2 hours After the reaction, the mixture is qualitatively and quantitatively analyzed by gas chromatography-mass spectrometry, and the conversion rate of n-butyraldehyde and the selectivity of butyl butyrate are both above 99%.

Embodiment 2～7

[0030] The specific methods of Examples 2-7 are similar to those of Example 1, and the specific reaction conditions and results are shown in Table 1. Use aluminum citrate, aluminum tartrate, aluminum malate, aluminum adipate, aluminum pimelate, aluminum dodecanoate and other organic dibasic acid aluminum or organic tribasic acid aluminum as the catalyst, and the catalyst dosage is n-butyraldehyde 0.2-1.0% of the mass, the reaction temperature is 0-20 DEG C, and the reaction time is 0.5-2 hours, the conversion rate of n-butyraldehyde and the selectivity of butyl butyrate can reach more than 99%.

[0031] Table 1. Direct catalytic conversion of n-butyraldehyde to butyl butyrate

[0032]

Embodiment 8

[0034] Catalyst recycling. After the reaction in Example 1, the product was distilled and separated, the catalyst was left in the reaction flask, and 20 grams of n-butyraldehyde was added to repeat the reaction, and the reaction was carried out at 10°C for 2 hours. The conversion rate of n-butyraldehyde and the selectivity of butyl butyrate both reached more than 99%. .

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Abstract

The invention relates to a method for preparing butyl butyrate by directly converting n-butyraldehyde. According to the method, n-butyraldehyde is used as a raw material, one or more than two of organic dibasic acid aluminum or organic tribasic acid aluminum such as aluminum oxalate, aluminum citrate, aluminum tartrate, aluminum malate, aluminum adipate, aluminum heptanedioate, aluminum dodecanedioate and the like are used as catalysts, the use amount of the catalyst is 0.2-1.0% of the mass of the n-butyraldehyde, the reaction temperature is 0-20 DEG C, the reaction time is 0.5-2 hours, and the n-butyraldehyde conversion rate and the butyl butyrate selectivity can reach more than 99%. The method has the advantages of short route, good atom economy, mild reaction conditions, catalyst recyclability, high raw material conversion rate, high product selectivity and the like.

Description

technical field [0001] The invention belongs to the field of organic chemical industry, in particular to a method for preparing butyl butyrate through direct catalytic conversion of n-butyraldehyde. Background technique [0002] Butyl butyrate, also known as n-butyl butyrate, is a colorless transparent liquid with banana and pineapple aroma, which exists in fruits such as apples, bananas, grapes, pears, strawberries and plums. Butyl butyrate is an edible spice that is allowed to be used in my country's "National Food Safety Standard Food Additive Use Standard" (GB 2760). It is widely used in foods such as candy, biscuits, bread, ice cream and soft drinks, and can also be used as Solvent for shellac, coumarone resins and paints, etc. Industrially used butyl butyrate is produced by the esterification reaction of n-butyric acid and n-butanol under the action of a catalyst. The catalyst used is mainly concentrated sulfuric acid. Due to the strong acidity and strong oxidizing p...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/44C07C69/24
CPCC07C67/44C07C69/24Y02P20/584
Inventor 黄义争徐杰高进杜文强苗虹孙颖郑玺石松
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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