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Method for preparing high-purity natural benzaldehyde from cinnamyl aldehyde or cinnamon oil

A technology for cinnamaldehyde and benzaldehyde is applied in the field of preparing high-purity natural benzaldehyde, and achieves the effects of cost saving, mild reaction conditions and short reaction time

Inactive Publication Date: 2017-02-15
GUANGXI FORESTRY RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] For the above existing technical problems, the invention provides a kind of method for preparing high-purity natural benzaldehyde by cinnamaldehyde or cinnamon oil, this method not only solves the prior art how to separate with solvent after natural benzaldehyde is prepared problem, but also greatly improved the purity and yield of the product, with the prospect of industrial production

Method used

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  • Method for preparing high-purity natural benzaldehyde from cinnamyl aldehyde or cinnamon oil

Examples

Experimental program
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Embodiment 1

[0030] A kind of method of preparing high-purity natural benzaldehyde by cinnamaldehyde or cinnamon oil: take cinnamaldehyde or cinnamon oil as raw material, take n-butanol as solvent, the volume ratio of n-butanol and cinnamaldehyde or cinnamon oil is 10:1, Potassium carbonate or potassium bicarbonate is used as a catalyst, the molar ratio of the amount of catalyst added to cinnamaldehyde is 1:5, hydrogen peroxide aqueous solution is used as an oxidant, and the method of adding hydrogen peroxide is: the mass percentage concentration is 30% over Dilute the hydrogen peroxide to a mass percent concentration of 15% or a mass percent concentration of 10% and add in two times, adding half of the amount at the beginning of the reaction, and adding the other half when the reaction is halfway through;

[0031] Under the condition of 40 DEG C, stir and react for 1.5h, after standing still, obtain an organic solution that is naturally separated from the aqueous solution and contain benza...

Embodiment 2

[0033] A method for preparing high-purity natural benzaldehyde by cinnamaldehyde or cinnamon oil: take cinnamaldehyde or cinnamon oil as raw material, take n-butanol as solvent, and the volume ratio of n-butanol and cinnamaldehyde or cinnamon oil is 15:1, Potassium carbonate or potassium bicarbonate is used as a catalyst, the molar ratio of the amount of catalyst added to cinnamaldehyde is 1:10, and hydrogen peroxide aqueous solution is used as an oxidant, and the method of adding hydrogen peroxide is: the mass percentage concentration is 30% over The hydrogen peroxide is diluted to a mass percent concentration of 15% or a mass percent concentration of 10%, and is injected dropwise.

[0034]Under the condition of 45 DEG C, stir and react for 1.8h, after standing still, obtain an organic solution that is naturally separated from the aqueous solution and contain benzaldehyde, and then carry out vacuum distillation to the organic solution containing benzaldehyde (be about to put t...

Embodiment 3

[0036] A method for preparing high-purity natural benzaldehyde by cinnamaldehyde or cinnamon oil: taking cinnamaldehyde or cinnamon oil as raw material, using n-butanol as solvent, the volume ratio of n-butanol and cinnamaldehyde or cinnamon oil is 20:1, Potassium carbonate or potassium bicarbonate is used as the catalyst, the molar ratio of the amount of catalyst added to cinnamaldehyde is 1:15, and hydrogen peroxide aqueous solution is used as the oxidant, and the method of adding hydrogen peroxide is: the mass percentage concentration is 30% over Dilute the hydrogen peroxide to a mass percent concentration of 15% or a mass percent concentration of 10% and add in two times, adding half of the amount at the beginning of the reaction, and adding the other half when the reaction is halfway through;

[0037] Under the condition of 50 DEG C, stirring and reacting for 2 hours, after standing still, an organic solution that is naturally separated from the aqueous solution and contai...

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Abstract

The invention discloses a method for preparing high-purity natural benzaldehyde from cinnamyl aldehyde or cinnamon oil. The method comprises the steps of carrying out a stirred reaction on the cinnamyl aldehyde or cinnamon oil, which serves as a raw material, for 1.5 to 3.5 hours at the temperature of 40 DEG C to 65 DEG C in the presence of potassium carbonate or potassium bicarbonate, which serves as a catalyst, in a manner of taking n-butanol as a solvent and taking an aqueous hydrogen peroxide solution as an oxidant, carrying out standing so as to obtain a benzaldehyde containing organic solution which is naturally separated from an aqueous solution, and then, carrying out reduced-pressure distillation on the benzaldehyde containing organic solution, thereby preparing the high-purity natural benzaldehyde. According to the method, the problem in the prior art that how to separate the natural benzaldehyde from the solvent after the natural benzaldehyde is prepared is solved, and the purity and yield of the product are improved greatly, so that the method has an industrial production prospect.

Description

technical field [0001] The invention belongs to a preparation method of chemical products. Specifically, it is a method for preparing natural benzaldehyde from cinnamaldehyde or cinnamon oil, especially a method for preparing high-purity natural benzaldehyde from cinnamaldehyde or cinnamon oil. Background technique [0002] Benzaldehyde is a food spice with a wide range of applications, and it is also an important intermediate raw material for fine organic synthesis, widely used in pesticides, medicines, spices, dyes and other fields. The sources of benzaldehyde can be divided into two categories: one is obtained by oxidation of toluene as raw material; the other is obtained by hydrolysis or ozonation of natural products as raw materials. The aroma quality of benzaldehyde prepared from natural products is better than that prepared from toluene, so it has higher economic value. [0003] There are two main methods for preparing benzaldehyde from natural products: one is to u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C45/28C07C45/82C07C47/54
CPCC07C45/28C07C45/82C07C47/54
Inventor 陈海燕梁忠云李军集秦荣秀周丽珠李桂珍谷瑶孟中磊
Owner GUANGXI FORESTRY RES INST
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