Natural benzaldehyde preparation method

A benzaldehyde and natural technology, applied in the field of preparation of natural benzaldehyde, can solve the problems of low ozone utilization rate and the like, and achieve the effects of high ozone utilization rate, good naturalness and good reaction rate

Active Publication Date: 2012-10-10
GUANGXI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the reaction system must be anhydrous, the reaction temperature must be strictly controlled at 0 ℃, and the utilization rate of ozone is low
In recent years, the research on the combination of ozone and catalysis or combination with other processes to strengthen ozone oxidation is increasing, the purpose is to increase the reaction rate and improve the utilization rate of ozone. method, therefore, the method for preparing natural benzaldehyde by catalytic ozone selective oxidation of cinnamaldehyde or cinnamon oil has broad application prospects

Method used

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  • Natural benzaldehyde preparation method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1. Prepare 0.1 mol / L hydrochloric acid solution, weigh 5 g of columnar activated carbon, grind it into powder, soak activated carbon in the above hydrochloric acid solution for 24 h, wash, 110 o C dry at 250 o C activation yields acid-activated activated carbon.

[0028] 2. In the bubbling reactor, respectively add 4 g cinnamaldehyde (cinnamaldehyde content above 95%), 12.00 g absolute ethanol, 0.02 g activated carbon catalyst activated by 0.1 mol / L hydrochloric acid, press 0.1 g (ozone) / g (cinnamaldehyde) / h flow rate, the ozone is passed into the bubble reactor, and the ozonation reaction is carried out at 0 °C for 2 h to obtain the ozonide intermediate.

[0029] 3. Dissolve 3.00 g of thiourea and 0.4 g of oxalic acid in 50 mL of deionized water, slowly drop the ozonated intermediate into the thiourea aqueous solution, perform a reduction reaction at below 10 °C for 3 h, centrifuge, and take out the organic phase.

[0030] 4. Molecularly distill the organic phase at...

Embodiment 2

[0032] 1. Prepare 0.2 mol / L hydrochloric acid solution, weigh 5 g of columnar activated carbon, grind it into powder, soak the activated carbon in the above hydrochloric acid solution for 24 h, wash, 110 o C dry at 250 o C activation yields acid-activated activated carbon.

[0033] 2. In the bubbling reactor, add 4 g cinnamaldehyde (the content of cinnamaldehyde is more than 95%), 12.00 g absolute ethanol, 0.04 g activated carbon catalyst activated by 0.2 mol / L hydrochloric acid, press 0.1 g (ozone) / The flow rate of g (cinnamaldehyde) / h is to pass ozone into the bubbling reactor, and perform an ozonation reaction at 0 °C for 0.5 h to obtain an ozonide intermediate.

[0034] 3. Dissolve 3.00 g of thiourea and 0.4 g of oxalic acid in 50 mL of deionized water, slowly drop the ozonated intermediate into the thiourea aqueous solution, perform a reduction reaction at below 10 °C for 3 h, centrifuge, and take out the organic phase.

[0035] 4. Molecularly distill the organic phase...

Embodiment 3

[0037] 1. Prepare 0.3 mol / L hydrochloric acid solution, weigh 5 g of columnar activated carbon, grind it into powder, soak the activated carbon in the above hydrochloric acid solution for 24 h, wash, 110 o C dry at 250 o C activation yields acid-activated activated carbon.

[0038]2. In the bubbling reactor, add 4 g of cinnamaldehyde (the content of cinnamaldehyde is more than 95%), 12.00 g of absolute ethanol, and 0.16 g of activated carbon catalyst activated by 0.3 mol / L hydrochloric acid, and press 0.2 g (ozone) / The flow rate of g (cinnamaldehyde) / h is to pass ozone into the bubbling reactor, and perform an ozonation reaction at 30 °C for 1 h to obtain an ozonide intermediate.

[0039] 3. Dissolve 3.00 g of thiourea and 0.4 g of oxalic acid in 50 mL of deionized water, slowly drop the ozonated intermediate into the thiourea aqueous solution, perform a reduction reaction at below 10 °C for 3 h, centrifuge, and take out the organic phase.

[0040] 4. Molecularly distill th...

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Abstract

The invention discloses a natural benzaldehyde preparation method, which comprises the following steps of: taking cinnamaldehyde as raw material; adding 0.5-10% of activated carbon catalyst modified by 0.1-1.0mol / L of hydrochloric acid; at the temperature of below-10-30DEG C, introducing in 0.05-1.0g of ozone at the rate of 1g of cinnamaldehyde per hour; carrying out ozonization reaction for 0.5-10 hours; under the condition of keeping the low temperature, dipping an ozonide intermediate into thiourea aqueous solution for reduction reaction; carrying out centrifugal separation; and finally carrying out molecular distillation at the temperature of 60DEG C and the pressure of 100Pa by a molecular distillation device to obtain the natural benzaldehyde with higher purity. The natural benzaldehyde preparation method disclosed by the invention has the advantages of simple technology, simplicity in operation, high reaction rate, high ozone use ratio, green and environmental-friendly reaction process, efficient catalyst, and is cheap and non-toxic and easy to separate from a product, the natural degree of the benzaldehyde can be kept, the selectivity of the benzaldehyde is good, and the purity and yield of the benzaldehyde are 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] 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 it 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 is one of the goods in short supply in international and domestic spices; at the same time, natural flavors u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C47/54C07C45/40
Inventor 秦祖赠苏通明刘杰范有圆曾玉凤刘自力
Owner GUANGXI UNIV
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