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A kind of n-butyraldehyde one-step conversion method for preparing butyl butyrate

A technology of butyl butyrate and n-butyraldehyde, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve the problems of large discharge of "three wastes", equipment corrosion, and many side reactions, and achieve raw material High conversion rate and product selectivity, mild reaction conditions, and good atom economy

Active Publication Date: 2021-04-13
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0024] In order to solve the outstanding problems such as long preparation route of butyl butyrate, many side reactions, complex post-treatment process, large discharge of "three wastes", serious equipment corrosion and high production cost, the purpose of the present invention is to develop a one-step n-butyraldehyde The conversion method to produce butyl butyrate has the advantages of short route, good atom economy, mild reaction conditions, high conversion rate of raw materials and high product selectivity, and recyclable catalyst.

Method used

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  • A kind of n-butyraldehyde one-step conversion method for preparing butyl butyrate
  • A kind of n-butyraldehyde one-step conversion method for preparing butyl butyrate
  • A kind of n-butyraldehyde one-step conversion method for preparing butyl butyrate

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Add 20 grams of n-butyraldehyde and 0.1 gram of aluminum glycinate (0.5% of the quality of n-butyraldehyde) into 100 ml of two-necked round-bottomed flasks equipped with condenser tubes, control the reaction temperature by a refrigerator to be 10° C., stir 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 2～5

[0034] The specific method of Examples 2-5 is similar to that of Example 1, and the specific reaction conditions and results are shown in Table 1. Using aluminum lysine, aluminum alanine, aluminum trimethyl tryptophan, aluminum glutamate and other amino acid aluminum as catalysts, the amount of catalyst is 0.2-1.0% of the mass of n-butyraldehyde, the reaction temperature is 0-20°C, the reaction The time is 0.5-2 hours, and the conversion rate of n-butyraldehyde and the selectivity of butyl butyrate can reach more than 99%.

[0035] Table 1. One-step conversion of n-butyraldehyde to prepare butyl butyrate

[0036]

Embodiment 6

[0038] Catalyst recycling. After the reaction in Example 1, the product was distilled and separated, the catalyst was left in the reaction flask, and 20 g of n-butyraldehyde was added to repeat the reaction at 10° C. for 2 hours. The catalyst was recycled three times, the conversion rates of n-butyraldehyde were 99%, 98%, 98%, and the selectivities of butyl butyrate were 99%, 99%, 98%.

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Abstract

The invention relates to a method for preparing butyl butyrate by one-step conversion of n-butyraldehyde, using n-butyraldehyde as raw material and amino acid aluminum as catalyst, preferably aluminum glycinate, aluminum lysine, aluminum alanine and trimethyl tryptophan One or two or more of amino acid aluminum such as aluminum acid and aluminum glutamate are catalysts, the amount of catalyst is 0.2-1.0% of the mass of n-butyraldehyde, the reaction temperature is 0-20°C, the reaction time is 0.5-2 hours, n-butyraldehyde Aldehyde conversion rate and butyl butyrate selectivity can reach more than 99%. The invention has the advantages of short route, good atom economy, mild reaction conditions, recyclable catalyst, high conversion rate of raw materials and high product selectivity.

Description

technical field [0001] The invention belongs to the field of organic chemical industry, in particular to a method for preparing butyl butyrate through one-step conversion of n-butyraldehyde. Background technique [0002] Butyl butyrate is a liquid with banana and pineapple flavors. It is an edible spice that is allowed to be used in my country's "National Food Safety Standard Food Additives Use Standard" (GB 2760). It is mainly used in candy, biscuits, bread, ice cream and soda It can also be used as a solvent for paint, nitrocellulose, etc. Industrially, butyl butyrate is produced by the esterification reaction of n-butyric acid and n-butanol under the action of concentrated sulfuric acid and other catalysts. The catalyst severely corrodes the equipment and is prone to side reactions such as oxidation and dehydration. The product has a deep color and requires a post-treatment process Complicated, the "three wastes" discharge a large amount, and the production cost is high. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C67/00C07C69/24
CPCC07C67/00C07C69/24Y02P20/584
Inventor 黄义争徐杰高进杜文强苗虹孙颖石松郑玺
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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