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Production method of natural equivalent anisic aldehyde

An anisaldehyde and production method technology, applied in the field of spice production, can solve the problems of increasing equipment cost and raw material cost, difficult disposal of waste acid, large amount of sulfuric acid, etc., and achieve low production cost, high degree of naturalness, and less waste acid Effect

Active Publication Date: 2012-02-01
GUANGXI WANSHAN SPICE
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Though this method has improved yield, avoids using toxic toluene to carry out extraction, has increased equipment cost and raw material cost (polymerization inhibitor is more expensive), and the amount of sulfuric acid that uses is big, and the waste acid that produces is many, waste acid in industrial production Difficult to handle

Method used

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  • Production method of natural equivalent anisic aldehyde
  • Production method of natural equivalent anisic aldehyde

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Put 20kg of anethole, 120kg of dilute sulfuric acid, 60kg of manganese dioxide and 80kg of water into the reactor while stirring, slowly raise the temperature to 120°C within 10 minutes, and react at a constant temperature for 120 minutes. After the reaction is over, the reaction materials are put into a pressure filter tank while it is hot for pressure filtration. It takes about 90 minutes, the filtrate is discharged from the bottom of the tank, and the filter residue is taken out from the top of the tank. The filtrate discharged from the bottom of the pressure filter tank enters the liquid separation tank through the pipeline to stand for stratification, and the sinking water is drained regularly, and the intermediate product anisealdehyde crude product enters the neutralization tank through the pipeline from the bottom of the liquid separation tank. Since the obtained crude anisaldehyde is acidic because it contains part of sulfuric acid, the pH value of the solution ...

Embodiment 2

[0029] Put 20kg of anethole, 115kg of dilute sulfuric acid, 59kg of manganese dioxide and 80kg of water into the reactor while stirring, slowly raise the temperature to 120°C within 10 minutes, and react at a constant temperature for 110 minutes. After the reaction is over, the reaction materials are put into a pressure filter tank while it is hot for pressure filtration. It takes about 100 minutes, the filtrate is discharged from the bottom of the tank, and the filter residue is taken out from the top of the tank. The filtrate discharged from the bottom of the pressure filter tank enters the liquid separation tank through the pipeline to stand for stratification, and the sinking water is drained regularly, and the intermediate product anisealdehyde crude product enters the neutralization tank through the pipeline from the bottom of the liquid separation tank. Since the obtained crude anisaldehyde is acidic because it contains part of sulfuric acid, the pH value of the solution...

Embodiment 3

[0031] Put 20kg of anethole, 114kg of dilute sulfuric acid, 58kg of manganese dioxide and 80kg of water into the reactor while stirring, slowly raise the temperature to 130°C within 10 minutes, and react at a constant temperature for 120 minutes. After the reaction is over, the reaction materials are put into a pressure filter tank while it is hot for pressure filtration. It takes about 90 minutes, the filtrate is discharged from the bottom of the tank, and the filter residue is taken out from the top of the tank. The filtrate discharged from the bottom of the pressure filter tank enters the liquid separation tank through the pipeline to stand for stratification, and the sinking water is drained regularly, and the intermediate product anisealdehyde crude product enters the neutralization tank through the pipeline from the bottom of the liquid separation tank. Since the obtained crude anisaldehyde is acidic because it contains part of sulfuric acid, the pH value of the solution ...

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Abstract

The invention discloses a production method of natural equivalent anisic aldehyde, which is characterized in that natural anise camphor is used as raw materials, manganese dioxide is adopted as oxidizing agents, the oxidation reaction is generated in dilute sulphuric acid media with the concentration being 40 percent to 45 percent, the natural equivalent anise camphor, the manganese dioxide, water and the dilute sulphuric acid are put into a reaction kettle for reaction according to an addition ratio of 1 to 3 / 2 to 4 / 3 to 5 / 5 to 7, and the natural equivalent anisic aldehyde is obtained through press filtering separation, still standing delamination, neutralization reaction and pressure reduction distillation after the reaction. The process is simple, the reaction condition is mild, the cost is low, the obtained anisic aldehyde has pure perfume, the concentration is higher than 98.0 percent, and the natural abundance can reach higher than 95 percent.

Description

technical field [0001] The invention relates to the field of perfume production, in particular to a synthesis method for synthesizing anisaldehyde by oxidation of anethole. Background technique [0002] Natural equivalents refer to substances produced by synthetic methods, or substances processed from natural raw materials by chemical methods, whose chemical structure and properties are equivalent to those existing in natural products. [0003] Anisaldehyde, the chemical name is 4-methoxybenzaldehyde (4-methoxybenzaldehyde), it has a strong aroma of anise and hawthorn, attractive fragrance, long-lasting fragrance, and strong antioxidant properties, widely used Used in food and fragrance industry. Anisaldehyde is the raw material for the synthesis of anisyl alcohol and its esters, anisic acid and its esters, and anisonitrile, and is also the raw material for the synthesis of amoxicillin. It is an extremely important synthetic fragrance and pharmaceutical intermediate. The m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/28C07C47/575
Inventor 杨少凡刘新伟赖积南黄江涛文天寿胡林刚
Owner GUANGXI WANSHAN SPICE
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