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Preparation method of benzaldehyde from cinnamaldehyde by continuous catalytic ozone oxidation

A technology of ozonation and cinnamaldehyde, applied in the field of continuous catalytic ozone oxidation of cinnamaldehyde to benzaldehyde, achieving the effects of high yield, high ozone utilization rate and simple process

Active Publication Date: 2015-06-17
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the method for preparing natural benzaldehyde by ozone selective oxidation of cinnamaldehyde or cinnamon oil has broad application prospects, the above-mentioned methods are batch processes, and there is still room for further improvement for industrial applications.

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  • Preparation method of benzaldehyde from cinnamaldehyde by continuous catalytic ozone oxidation

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Embodiment 1

[0029] A kind of continuous catalytic ozone oxidation cinnamaldehyde is the preparation method of benzaldehyde

[0030] Taking cinnamaldehyde as raw material, the mixed solution of loading 50g cinnamaldehyde and dehydrated alcohol is in the continuous ozonation reactor (attached figure 1 ), adding 0.5% MnO 2 Catalyst, at -5°C, pass 0.05g of ozone per hour per gram of cinnamaldehyde to carry out ozonation reaction, after 10 minutes of reaction, use 50g·h -1 g cat -1 Continuously feed the mixed solution of cinnamaldehyde and dehydrated alcohol, their mass ratio is cinnamaldehyde: dehydrated alcohol=1:2, continuous reaction obtains liquid phase product, and liquid phase product passes through molecular distillation device, and at temperature is 10 ℃, Pressure is that distillation under 50Pa obtains the benzaldehyde 3g h that purity is more than 99wt% -1 .

Embodiment 2

[0032] A kind of continuous catalytic ozone oxidation cinnamaldehyde is the preparation method of benzaldehyde

[0033]Taking cinnamaldehyde as raw material, the mixed solution of loading 50g cinnamaldehyde and dehydrated alcohol is in the continuous ozonation reactor (attached figure 1 ), add 5.0% ZnO catalyst, at 20°C, pass 0.85g of ozone per hour per gram of cinnamaldehyde to carry out ozonation reaction, and react with 100g h -1 g cat -1 Continuously feed the mixed solution of cinnamaldehyde and dehydrated ethanol, their mass ratio is cinnamaldehyde: dehydrated alcohol=1:3), continuous reaction obtains the liquid phase product, and the liquid phase product passes through the molecular distillation device, at a temperature of 30 ℃ , the pressure is that distillation under 80Pa obtains the benzaldehyde 45g h that purity is more than 99wt% -1 .

Embodiment 3

[0035] A kind of continuous catalytic ozone oxidation cinnamaldehyde is the preparation method of benzaldehyde

[0036] Taking cinnamaldehyde as raw material, the mixed solution of loading 50g cinnamaldehyde and dehydrated alcohol is in the continuous ozonation reactor (attached figure 1 ), adding 2.5% Fe 2 o 3 Catalyst, at 10°C, pass 0.45g of ozone per hour per gram of cinnamaldehyde to carry out ozonation reaction, after 10 minutes of reaction, use 70g·h -1 g cat -1 Continuously feed the mixed solution of cinnamaldehyde and dehydrated alcohol, their mass ratio is cinnamaldehyde: dehydrated alcohol=1:6, continuous reaction obtains liquid phase product, and liquid phase product passes through molecular distillation device, and at temperature is 80 ℃, Distillation at a pressure of 150 Pa to obtain a purity of more than 99wt% benzaldehyde 6g h -1 .

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Abstract

The invention discloses a preparation method of benzaldehyde from cinnamaldehyde by continuous catalytic ozone oxidation, which comprises the following steps: by using cinnamaldehyde or cassia oil as the raw material, adding a mixed solution of 50g cinnamaldehyde and anhydrous ethanol into a continuous ozonization reactor, adding 0.5-5.0% of one or more of MnO2, ZnO, Fe2O3 and CaO as a catalyst, introducing 0.05-0.85g of ozone to every gram of cinnamaldehyde per hour at -5-20 DEG C to carry out ozonization reaction for 10 minutes, continuously introducing the cinnamaldehyde-anhydrous ethanol mixed solution at the rate of 50-100g.h<-1>.gcat<-1> to continuously react to obtain a liquid-phase product, and distilling the liquid-phase product in a molecular distillation device at certain temperature under certain pressure to obtain the higher-purity benzaldehyde. The method has the advantages of simple technique, green reaction process, favorable selectivity and high benzaldehyde yield, can maintain the nature of the benzaldehyde, and can implement continuous production of natural benzaldehyde.

Description

technical field [0001] The invention belongs to the field of intensive processing of agricultural and forestry chemical products, in particular to a preparation method for continuously catalytic ozone oxidation of cinnamaldehyde to benzaldehyde. Background technique [0002] With the improvement of living standards, people have higher and higher requirements for food safety, and they are more inclined to use safer and healthier natural food additives. As an important natural food flavor, natural benzaldehyde is widely used in food, beverage, tobacco and cosmetic industries. Natural benzaldehyde has a special smell of almonds, and exists in large quantities in essential oils such as cinnamon oil, bitter almond oil, and walnut oil. It is the second largest spice in the world in terms of quantity, with an annual demand of about 8,000 tons. At present, the demand for natural benzaldehyde is increasing day by day, and it belongs to one of the goods in short supply of internation...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/54C07C45/40
CPCC07C45/40C07C47/54
Inventor 秦祖赠韩琦苏通明纪红兵
Owner GUANGXI UNIV
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