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Preparation method of anisic aldehyde

A technology of anisaldehyde and anethole, which is applied in the field of preparation of anisaldehyde, can solve the problems of high cost and price, pollution of three wastes, and low yield, and achieve the effects of large-scale industrial production, less pollution, and less corrosion

Active Publication Date: 2014-01-08
ZITONG HUIQUAN PERFUME CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The first method is the anethole oxidation method, which is rarely used due to the limitation of natural resources and high cost price.
The second is the oxidation method (Sommelet reaction method) using anisole (sodium red alum) as the raw material. This method will produce a large amount of acidic wastewater and cause serious corrosion to the equipment.
The third is the cresol synthesis method, which has the problems of serious pollution of three wastes and low yield

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] The raw material natural Artemisinin with a purity of 50% is put into a rectification tower for purification. The temperature of the bottom of the rectification tower is 160°C and the temperature at the top of the tower is 120°C to obtain purified Artemisinin with a purity of About 98%.

[0043] Put the purified wormwood into the isomerization pot, then add catalyst potassium hydroxide to the isomerization pot, control the temperature in the isomerization pot to 180°C, and react for 4 hours. After the reaction, stop the isomerization pot. Heated to get anethole. Wherein, the quality of the potassium hydroxide added is 5% of the quality of the purified Artemisinin.

[0044] Freeze the anethole at minus 20°C, and centrifuge the anethole under the freezing condition for 20 minutes to obtain high-purity anethole.

[0045] Put 1000kg of high-purity anethole into the reactor, and add 200kg of dilute sulfuric acid, 300kg of MnO 2 , control the temperature in the reactor to ...

Embodiment 2

[0050] The raw material natural wormwood is put into a rectification tower for purification, the temperature of the bottom of the rectification tower is 150° C., and the temperature of the top of the tower is 110° C. to obtain the purified wormwood.

[0051] Put the purified wormwood into the heterogeneous pot, then add potassium hydroxide into the heterogeneous pot, control the temperature in the heterogeneous pot to 185°C, and react for 3 hours. After the reaction is over, stop heating the heterogeneous pot , get anethole. Wherein, the quality of the potassium hydroxide added is 3% of the quality of the purified Artemisinin.

[0052] The anethole is frozen below -20°C, and the anethole is centrifuged under the freezing condition for 50 minutes to obtain high-purity anethole.

[0053] Put 1000kg of high-purity anethole into the reactor, and add 100kg of dilute sulfuric acid, 400kg of MnO 2 , control the temperature in the reactor to 100°C, react for 4 hours, and obtain the ...

Embodiment 3

[0058] The raw material natural wormwood is put into a rectification tower for purification, the temperature of the bottom of the rectification tower is 155° C., and the temperature of the top of the tower is 115° C. to obtain the purified wormwood.

[0059] Put the purified wormwood into the heterogeneous pot, then add potassium hydroxide into the heterogeneous pot, control the temperature in the heterogeneous pot to 175°C, and react for 5 hours. After the reaction, stop heating the heterogeneous pot , get anethole. Wherein, the quality of the potassium hydroxide added is 8% of the quality of the purified Artemisinin.

[0060] The anethole is frozen below -25° C., and the anethole is centrifuged under freezing conditions for 15 minutes to obtain high-purity anethole.

[0061] Put 1000kg of high-purity anethole into the reactor, and add 300kg of dilute sulfuric acid, 250kg of MnO 2 , Control the temperature in the reactor to 105°C, and react for 3h to obtain crude anisaldehy...

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PUM

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Abstract

The invention discloses a preparation method of anisic aldehyde and aims to provide a novel preparation method of anisic aldehyde in order to reduce the production cost of the anisic aldehyde and the environment pollution. The method comprises the following steps: isomerizing; carrying out refrigerated centrifugation; oxidizing; centrifuging; washing; and neutralizing. Estragole is subjected to steps such as isomerization, centrifugation and oxidization in the presence of a catalyst so that electrons in estragole molecules are rearranged, and foreign matters generate required anethole. The anethole is subjected to oxidization reaction under an acidic condition of manganese dioxide and transformed from ketone to aldehyde so that anisic aldehyde is obtained finally. According to the invention, the estragole is used as the raw material, the purification content of the estragole for preparing the anisic aldehyde can be up to over 97% and is about 13% higher than that of the traditional process. The preparation method is capable of remarkably increasing the yield of the anisic aldehyde and meeting the requirement for large-scale industrial production, easier to purify as well as little in equipment corrosion and environment pollution.

Description

technical field [0001] The invention relates to the field of perfume production, in particular to a preparation method of anisaldehyde. Background technique [0002] The chemical name of anisaldehyde is p-methoxybenzaldehyde, which has a wide range of applications. It has a long-lasting hawthorn aroma and is attractive in aroma, so it is widely used in the preparation of various flavors such as sweet flower, hawthorn and clove flavors, as well as the preparation of food, sugar and beverage flavors; in medicine, its It is an important intermediate for the preparation of anti-vitamin drugs (such as hydroxybenzyl penicillin, porphyrin photosensitizers, etc.); in the electroplating industry, it can be used as an excellent brightener for cyanide-free galvanizing DE additives; in agriculture In the field, anisaldehyde can be used as insecticide, insecticide additive, biological growth inhibitor, etc. Due to its excellent properties, anisaldehyde has been widely used. [0003] A...

Claims

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Application Information

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IPC IPC(8): C07C47/575C07C45/28
CPCC07C41/32C07C45/28C07C47/575C07C43/215
Inventor 钟利明
Owner ZITONG HUIQUAN PERFUME CHEM
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