Method for preparing anisaldehyde through micro-channel continuous ozone oxidation

A technology of ozone oxidation and anisaldehyde, applied in the field of chemical application, can solve the problems such as unreported production of anisaldehyde, achieve the effects of low cost, few by-products, and avoiding energy consumption and human consumption

Active Publication Date: 2020-06-19
FUDAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Production of anisaldehyde by microchannel ozonation technology has not been reported so far

Method used

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  • Method for preparing anisaldehyde through micro-channel continuous ozone oxidation
  • Method for preparing anisaldehyde through micro-channel continuous ozone oxidation
  • Method for preparing anisaldehyde through micro-channel continuous ozone oxidation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1: Take 3.08g of fennel oil (90% anethole content) and dissolve it in 10g of cyclohexane; the fennel oil solution is passed into the sampling pump 1 and sent to the preheating module 1 in the microchannel reactor; ozone The generator uses oxygen as the gas source to prepare ozone, and the concentration of the ozone generator is set to 60%. The ozone generated by the ozone generator is passed into the sampling pump 2 and sent to the preheating module 2 in the first microchannel reactor; the control of the sampling pump 1 and the flow rate of the injection pump 2 is 1mL / min, the microchannel oil bath temperature is room temperature; the fennel oil solution in the preheating module 1 enters the mixing module 1 through the pipeline after preheating, and the ozone in the preheating module 2 is preheated. After heating, it enters the mixing module 1 through the pipeline, and the two are mixed to start the oxidation reaction; the time for mixing to flow through the m...

Embodiment 2

[0031] Embodiment 2: Get 3.08g of fennel oil (90% anethole content) and dissolve it in 10g of cyclohexane; the fennel oil solution is passed into the sampling pump 1 and sent to the preheating module 1 in the microchannel reactor; ozone The generator uses oxygen as the gas source to prepare ozone, and the concentration of the ozone generator is set to 60%. The ozone generated by the ozone generator is passed into the sampling pump 2 and sent to the preheating module 2 in the first microchannel reactor; the control of the sampling pump 1 and the flow rate of the injection pump 2 is 1mL / min, the temperature of the microchannel oil bath is -20°C; the fennel oil solution in the preheating module 1 enters the mixing module 1 through the pipeline after preheating; After ozone is preheated, it enters the mixing module 1 through the pipeline, and the two are mixed to start the reaction; the time for mixing to flow through the microchannel reactor is about 20 minutes; the reacted mixed ...

Embodiment 3

[0032] Embodiment 3: Control the flow rate of the sampling pump 1 and the sampling pump 2 to be 0.5mL / min, and the other conditions and procedures are the same as in the embodiment 1. 2.26 g of anisaldehyde was obtained with a yield of 88.7% (calculated by anethole).

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Abstract

The invention belongs to the technical field of chemical application, and particularly relates to a method for preparing anisaldehyde through micro-channel continuous ozone oxidation. According to themethod, anethole is used as a raw material, ozone is used as an oxidizing agent, sodium hydrogen sulfite is used as a reducing agent, micro-channel equipment is adopted for mixing, a continuous reaction is carried out, anise oil is oxidized by ozone in the presence of a solvent or in the absence of a solvent, oxydol is reduced by sodium hydrogen sulfite, and the target product anisaldehyde is obtained. Compared with the present synthesis technology in the prior art, the method has the advantages of realization of continuous reaction, easiness in automatic control, simplicity, convenience andsafety in operation, mild reaction conditions, few byproducts, low cost and less pollution and is suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of chemical applications, and in particular relates to a method for preparing anisaldehyde through continuous ozone oxidation in a microchannel. Background technique [0002] Star anise, also known as star anise, star anise, aniseed, scientific name Illiciumverum, is an important economic tree species with "medicine and food from the same source" in southern China. Yunnan, southern Fujian, western Guangdong. China's star anise exports account for more than 80% of the world market and has great economic value. Star anise fruit can be used as seasoning, leaves and fruit can be steamed with aromatic oil, called star anise oil, and its content is generally 5% to 12%. Fennel oil can be used in the food industry such as making liqueur; it is also a spice for making toothpaste, soap, perfume, and cosmetics; Anethole in anise oil can be directly oxidized to produce anisaldehyde without separation. Anisaldehyde is...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/41C07C47/575B01J19/00
CPCC07C45/41B01J19/0093C07C47/575
Inventor 戴惠芳朱猷律
Owner FUDAN UNIV
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