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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 (CN1597653A, CN1834080A) reported the method for preparing benzaldehyde in near critical water, realized the greening of process, but side reaction is many, and selectivity is poor, and the temperature of reaction (200~350 ℃ ) high, high temperature not only has high requirements on equipment, but also reduces the natural degree of benzaldehyde

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 0.1656 grams of cinnamon oil (containing 82% cinnamaldehyde) in the autoclave, add hydrogen peroxide, the mol ratio of raw material and hydrogen peroxide is 1: 1, then feed carbon dioxide to a pressure of 20MPa, stir at 50°C, and react After 2 hours, the reaction kettle was quickly placed in ice water to end the reaction, and the pressure was released slowly, and the reactants and products in the discharged gas were diluted with ethyl acetate during the venting process, and 0.0306 grams of benzaldehyde product could be obtained after testing , the yield of benzaldehyde was 23.1%.

Embodiment 2

[0020] Add 0.2484 grams of substrate cinnamon oil (containing 82% cinnamaldehyde) in the autoclave, feed oxygen, the mol ratio of raw material and oxygen is 2: 1, then feed carbon dioxide to a pressure of 6.5MPa, at 30 ° C Under stirring, after reacting for 1 hour, quickly place the reaction kettle in ice water to end the reaction, and slowly release the pressure, and dilute with ethyl acetate to receive the reactants and products in the discharged gas during the venting process. After testing, you can get benzene The formaldehyde product is 0.0379 grams, and the yield of benzaldehyde is 19.1%.

Embodiment 3

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

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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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