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Benzaldehyde preparation method

A technology of benzaldehyde and cinnamaldehyde, which is applied in the field of preparation of natural benzaldehyde, can solve the problems such as difficult contact of reactants, unfavorable maintenance of p-benzaldehyde, increase in processing cost, etc., and achieves no effect on naturalness, easy operation, and processing capacity. big effect

Active Publication Date: 2018-07-27
GUANGXI UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage of this method is that cinnamaldehyde and water are two immiscible liquids, and it is difficult to fully contact the reactants in the two-phase reaction. At the same time, using a large amount of lye will increase the processing cost and easily pollute the environment.
Chinese patents (CN1446789A, CN1749231A, CN1911891A, CN101985414A) have improved the production equipment of this method, the cost has been reduced, and the quality has also been improved, but the impurity content is still relatively high, and there is still the problem of using a large amount of lye
Chinese patents (CN1179934C, CN1634837A), U.S. patents (US4683342, US4617419) introduce phase transfer catalysts or surfactants to improve the solubility of cinnamaldehyde in water, but the above two additives are not conducive to the maintenance of the natural degree of benzaldehyde
Qinzu et al. (CN201710532001.4) catalyzed the oxidation of cinnamaldehyde to synthesize benzaldehyde by gas-solid reaction. 2 Or air is the oxygen source, the reaction does not need to use a solvent, the product is easy to separate, and the natural degree of benzaldehyde is high, but the temperature of the reaction process is high, so that cinnamaldehyde is over-oxidized to CO 2 and water

Method used

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  • Benzaldehyde preparation method

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Experimental program
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Effect test

Embodiment 1

[0029] Weigh 1.0g V oxide catalyst and put it into a fixed-bed reactor, heat the fixed-bed temperature to 120°C, and pass the cinnamaldehyde with a content of more than 95wt% through a heating device at 120°C at a flow rate of 0.05mL / min, in the mist Mix it with 5 atmospheres of air or oxidation at a flow rate of 50mL / min heated at 120°C in the atomization nozzle, spray it into a fixed-bed reactor after atomization, and carry out the catalytic oxidation reaction of cinnamaldehyde to obtain crude benzaldehyde.

[0030] Under the conditions of 60° C. and 100 Pa, the above crude benzaldehyde was subjected to molecular distillation, and the yield of natural benzaldehyde with a content greater than 98% was obtained after the reaction was stable was 22%.

Embodiment 2

[0032] Weigh 1.0g of Ba oxide catalyst and put it into a fixed-bed reactor, heat the fixed-bed temperature to 150°C, and put cinnamaldehyde with a content of more than 95wt% through a heating device at 150°C at a flow rate of 1.0mL / min. Mix it with 5 atmospheric pressure air or oxidation at a flow rate of 150mL / min heated at 150°C in the atomization nozzle, spray it into a fixed-bed reactor after atomization, and carry out the catalytic oxidation reaction of cinnamaldehyde to obtain crude benzaldehyde.

[0033] Under the conditions of 60° C. and 100 Pa, the above-mentioned crude benzaldehyde was subjected to molecular distillation, and the yield of natural benzaldehyde with a content greater than 98% was obtained after the reaction was stable was 36%.

Embodiment 3

[0035] Weigh 1.0g Mg-V oxide catalyst and put it into a fixed bed reactor, heat the fixed bed temperature to 150°C, and pass the cinnamaldehyde with a content of more than 95wt% through a heating device at 150°C at a flow rate of 1.0mL / min, In the atomizing nozzle, it is mixed with 5 atmospheres of air or oxidation at a flow rate of 150mL / min heated at 150°C, sprayed into a fixed-bed reactor after atomization, and cinnamaldehyde is catalytically oxidized to obtain crude benzaldehyde.

[0036] Under the conditions of 60° C. and 100 Pa, the above-mentioned crude benzaldehyde was subjected to molecular distillation, and the yield of natural benzaldehyde with a content greater than 98% was obtained after the reaction was stable was 36%.

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Abstract

The invention discloses a natural benzaldehyde preparation method. According to the invention, one oxide or two or three composite oxides from V, Ti, Ag, Ba, and Mg can be taken as a catalyst, O2 or air is introduced as an oxygen source, cinnamaldehyde is atomized through compressed air or oxidation, and then is introduced into a fixed bed reactor, a gas-solid phase catalysis continuous reaction is carried out under normal pressure at the temperature of 120-200 DEG C, a product continuously passes through a molecular distillation apparatus, molecular distillation is carried out at the temperature of 60 DEG C under 100 Pa, and the natural benzaldehyde product is obtained. The natural benzaldehyde preparation method has the advantages of simple and novel process, simple operation, no requirement of solvent, simple separation, and fast reaction rate, excessive oxidation of cinnamaldehyde is prevented, a reaction process is environmentally friendly, the natural degree of benzaldehyde is good, and the product purity is high.

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] Benzaldehyde is the second largest spice in the world, second only to vanillin, with an annual demand of about 7,000 tons. It is used as an additive in food, beverage, tobacco and cosmetic industries. Since the beginning of the 21st century, consumers have gradually returned to the ranks of the tendency to use natural food additives, and have incorporated the concept of "natural compounds are healthier than chemically synthesized ones" into the newly formulated food regulations. International organizations such as the Food Flavor Industry International Organization restrict or prohibit the use of chemically synthesized food additives that can cause toxicity, teratogenicity, and carcinogenicity. Under the double impact of the change of consumer consumption ...

Claims

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Application Information

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IPC IPC(8): C07C45/36C07C47/54
CPCC07C45/36C07C47/54
Inventor 罗轩杜鹏举蒋月秀秦祖赠苏通明纪红兵
Owner GUANGXI UNIV
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