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A kind of preparation method of benzaldehyde

A technology of benzaldehyde and cinnamaldehyde, which is applied in the field of preparation of natural benzaldehyde, and achieves the effects of easy product separation, large processing capacity and no influence on naturalness

Active Publication Date: 2020-11-13
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The present invention proposes to use gas-phase catalytic oxidation of cinnamaldehyde to synthesize benzaldehyde, with O 2 Or air is oxygen source, and reaction does not need to use solvent, and product separation is simple and easy, and benzaldehyde natural degree is high, and does not produce pollution, yet there is not yet the report of using tube furnace reactor to carry out gas-phase catalytic oxidation of cinnamaldehyde to synthesize benzaldehyde, Gas-phase catalytic oxidation of cinnamaldehyde to benzaldehyde using a tubular reactor has certain potential and industrial value

Method used

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  • A kind of preparation method of benzaldehyde

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Experimental program
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Effect test

Embodiment 1

[0026] Gas-phase catalytic oxidation reaction: Weigh 0.5g of Fe-Mo composite oxide catalyst mixed with a molar ratio of 1:1 and put it into a fixed-bed reactor, and beat cinnamaldehyde with a content of more than 95wt% at a flow rate of 0.03mL / min. Put it into a gasifier at 260°C, make the cinnamaldehyde gasify into a gas, and then pass it into a fixed-bed reactor. When the temperature of the fixed bed reached 260°C, oxygen was introduced at a flow rate of 10 mL / min as an oxygen source to carry out the catalytic oxidation reaction of cinnamaldehyde to obtain crude benzaldehyde.

[0027] Molecular distillation: under the conditions of 60° C. and 100 Pa, carry out molecular distillation on the above-mentioned crude benzaldehyde, after the reaction is stable, the yield of natural benzaldehyde with a content greater than 98% is 20%.

Embodiment 2

[0029]Gas-phase catalytic oxidation reaction: Weigh 0.5 g of Fe-Mo-Ca composite oxide catalyst mixed with a molar ratio of 1:1:1 and put it into a fixed-bed reactor, and the content is more than 95wt% at a flow rate of 0.3mL / min. The cinnamaldehyde is injected into a gasifier at 260°C, and the cinnamaldehyde is vaporized into a gas and then passed into a fixed-bed reactor. When the temperature of the fixed bed reached 305° C., oxygen was introduced at a flow rate of 20 mL / min as an oxygen source to carry out the catalytic oxidation reaction of cinnamaldehyde to obtain crude benzaldehyde.

[0030] Molecular distillation: under the conditions of 60° C. and 100 Pa, carry out molecular distillation on the above-mentioned crude benzaldehyde, and after the reaction is stable, the yield of natural benzaldehyde with a content greater than 98% is 29%.

Embodiment 3

[0032] Gas-phase catalytic oxidation reaction: Weigh 0.5g of Ga-Mo-W composite oxide catalyst mixed with a molar ratio of 1:1:1 and put it into a fixed-bed reactor. The cinnamaldehyde is injected into a gasifier at 260°C, and the cinnamaldehyde is vaporized into a gas and then passed into a fixed-bed reactor. When the temperature of the fixed bed reached 365° C., oxygen was introduced at a flow rate of 45 mL / min as an oxygen source to carry out the catalytic oxidation reaction of cinnamaldehyde to obtain crude benzaldehyde.

[0033] Molecular distillation: under the conditions of 60° C. and 100 Pa, carry out molecular distillation on the above-mentioned crude benzaldehyde, and after the reaction is stable, the yield of natural benzaldehyde with a content greater than 98% is 33%.

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Abstract

The invention discloses a method for preparing natural benzaldehyde. The method comprises the steps of gasifying cinnamyl aldehyde at the temperature of 260 DEG C in a manner of taking a composite oxide of two or three of Fe, Mo, W, Mn, Ca, Al, Cu and Zn as a catalyst and introducing O2 or air as an oxygen supply, then, enabling cinnamyl aldehyde gas to enter a fixed-bed reactor, carrying out a gas-solid catalytic continuous reaction, and subjecting a product to molecular distillation continuously through a molecular distillation device at the temperature of 60 DEG C under the pressure of 100Pa, thereby obtaining the natural benzaldehyde product. The method has the advantages that the process is simple and novel, the operation is simple, a solvent is not required to be used, the separation is simple and convenient, the reaction rate is high, the reaction process is environmentally friendly, the natural degree of the benzaldehyde is good, and the obtained product is high in purity.

Description

technical field [0001] The invention belongs to the field of deep processing of agricultural and forestry chemical products. Specifically, it is a preparation method of natural 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 international and domestic spices; at the same time, natural spic...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C47/54C07C45/36
CPCC07C45/36C07C47/54
Inventor 秦祖赠胡刚罗轩苏通明纪红兵
Owner GUANGXI UNIV
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