Method for preparing natural benzaldehyde

A benzaldehyde, natural technology, applied in the field of preparation of natural benzaldehyde, can solve the problems of unstable ozonide intermediates, reduce the natural degree of benzaldehyde, and low ozone utilization rate, and achieve easy continuous scale production, low cost, easily controlled effects

Inactive Publication Date: 2011-09-21
SUN YAT SEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reaction system of this method must be anhydrous, the ozonide intermediate is unstable, the reaction temperature needs to be strictly controlled, the equipment requirements are high, and the utilization rate of ozone is not high, so there are certain environmental problems
[0006] 3, near critical water method, people such as Lv Xiuyang (CN

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0017] Example 1

[0018] Add 0.1656 g of cinnamon oil (containing 82% cinnamaldehyde) into the autoclave, add hydrogen peroxide, the molar ratio of raw material to hydrogen peroxide is 1:1, and then add carbon dioxide to a pressure of 20MPa, stir at 50°C, and react. After 2 hours, quickly put the reaction kettle in ice water to complete the reaction, and slowly release the pressure, and dilute the reactants and products in the discharged gas with ethyl acetate during the venting process. After testing, 0.0306 g of benzaldehyde product can be obtained. The yield of benzaldehyde was 23.1%.

Example Embodiment

[0019] Example 2

[0020] Add 0.2484 grams of substrate cinnamon oil (containing 82% cinnamaldehyde) into the autoclave, and introduce oxygen. The molar ratio of raw material to oxygen is 2:1, and then introduce carbon dioxide to a pressure of 6.5MPa at 30°C. After stirring for 1 hour, the reaction kettle was quickly placed in ice water to complete the reaction, and the pressure was slowly relieved, and the reactants and products in the discharged gas were diluted with ethyl acetate during the emptying process. After testing, benzene can be obtained. The formaldehyde product was 0.0379 g, and the benzaldehyde yield was 19.1%.

Example Embodiment

[0021] Example 3

[0022] Add 0.3312 grams of substrate cinnamon oil (containing 82% cinnamaldehyde) into the autoclave, add hydrogen peroxide, the molar ratio of raw material to hydrogen peroxide is 1:3, and then add carbon dioxide to a pressure of 10MPa, and stir at 60°C After reacting for 1.5 hours, quickly put the reaction kettle in ice water to complete the reaction, and slowly release the pressure, and dilute the reactants and products in the discharged gas with ethyl acetate during the emptying process. The benzaldehyde product can be obtained by testing. 0.0660 g, the yield of benzaldehyde was 24.9%.

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PUM

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Abstract

The invention discloses a method for preparing natural benzaldehyde from cinnamon oil without catalytic oxidation. In the method, natural cinnamon oil is taken as a raw material, supercritical or subcritical carbon dioxide is taken as a reaction medium, air, oxygen or hydrogen peroxide is taken as an oxidant, and the cinnamon oil is oxidized under mild reaction conditions to form the natural benzaldehyde. Solvents and catalysts are not used, and the method has the advantages of simple technical route, mild reaction conditions, environmental friendliness, low cost and the like.

Description

technical field [0001] The present invention relates to a kind of preparation method of natural benzaldehyde, specifically, relate to a kind of method that oxidizes natural cinnamaldehyde in supercritical or subcritical carbon dioxide medium to prepare natural benzaldehyde. Background technique [0002] Natural benzaldehyde has the aroma of bitter almonds and is an important spice with the second largest consumption in the world. Compared with synthetic benzaldehyde, natural benzaldehyde has the advantages of high naturalness, high aroma quality, and no solvent residue. Natural benzaldehyde is widely used in high-grade cosmetics and food as a high-grade fragrance. According to statistics, at present, the natural benzaldehyde used in food flavors and fragrances in the world is as high as 7,000 tons a year, and the demand is still increasing year by year. my country is rich in cinnamon oil resources, and the use of cinnamon oil (natural cinnamaldehyde content 70-80%) to prod...

Claims

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Application Information

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IPC IPC(8): C07C47/54C07C45/67C07C45/54
CPCY02P20/54
Inventor 纪红兵姚煜东关西文周贤太
Owner SUN YAT SEN UNIV
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