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Preparation method of natural benzaldehyde

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

Inactive Publication Date: 2012-12-19
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°C, 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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  • Preparation method of natural benzaldehyde

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Experimental program
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Effect test

Embodiment 1

[0025] In the bubbling reactor, add 5.26g cinnamaldehyde (more than 95% of cinnamaldehyde content), 10.00g dehydrated alcohol, 0.25g TiO 2 Catalyst, pass ozone into the bubbling reactor at a flow rate of 0.1g (ozone) / g (cinnamaldehyde) / h, and perform an ozonation reaction at 0° C. for 2 hours to obtain an ozonide intermediate. Then dissolve 3.00g of thiourea and 0.21g of oxalic acid in 30mL of deionized water, slowly drop the ozonated intermediate into the aqueous solution of thiourea, perform a reduction reaction at 0°C for 2 hours, separate oil from water, Molecular distillation was carried out under the following conditions, and the available benzaldehyde product was 1.85g, and the yield of benzaldehyde was 46.1%.

Embodiment 2

[0027] In the bubbling reactor, add 5.31g cinnamaldehyde (more than 95% of cinnamaldehyde content), 10.1g dehydrated alcohol, 0.50g gac respectively, by 0.1g (ozone) / g (cinnamaldehyde) / h flow rate, ozone is passed into In the bubbling reactor, the ozonation reaction was carried out at 5° C. for 2 h to obtain the ozonide intermediate. Then dissolve 3.10g of thiourea and 0.19g of oxalic acid in 30mL of deionized water, slowly drop the ozonated intermediate into the aqueous solution of thiourea, perform a reduction reaction at 0°C for 2 hours, separate oil from water, Molecular distillation was carried out under the following conditions, and the benzaldehyde product was 1.59g, and the yield of benzaldehyde was 39.3%.

Embodiment 3

[0029] In the bubbling reactor, add respectively 5.28g cinnamaldehyde (more than 95% of cinnamaldehyde content), 10.03g dehydrated alcohol, 0.25g MnO 2 Catalyst, pass ozone into the bubbling reactor at a flow rate of 0.1g (ozone) / g (cinnamaldehyde) / h, and perform an ozonation reaction at 0° C. for 2 hours to obtain an ozonide intermediate. Then dissolve 2.99g of thiourea and 0.22g of oxalic acid in 30mL of deionized water, slowly drop the ozonated intermediate into the aqueous solution of thiourea, perform a reduction reaction at 0°C for 2 hours, separate oil from water, Molecular distillation was carried out under the following conditions, and the benzaldehyde product was 2.04g, and the yield of benzaldehyde was 50.6%.

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Abstract

The invention discloses a preparation method of natural benzaldehyde. The method comprises the following steps of: getting cinnamyl aldehyde or cinnamon oil as a raw material; adding one or more of multi-phase catalysts of 0.5% to 10% of MnO2, TiO2, Al2O3, SnO2, Fe2O3, MgO, CuO, CeO2, ZrO2, Bi2O3, Y2O3 or active carbon; pouring 0.05 to 0.5g of ozone in a bubbling reactor at -5 to 20 DEG C based on 1g of cinnamyl aldehyde per hour; carrying out an ozonization reaction for 0.5 to 10 hours to obtain an ozonide intermediate; dropping the ozonide intermediate into the thiourea aqueous solution to be reduced while agitating at a constant low temperature, so as to obtain an oil-water mixture; separating the oil from the water to obtain a rough benzaldehyde product; and finally operating a molecular distillation device to obtain the benzaldehyde with relatively high purity. The preparation method has the advantages of simple technology, green reaction, being capable of remaining the natural property of the benzaldehyde, high selectivity, and high yield of the benzaldehyde.

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 Applications(China)
IPC IPC(8): C07C47/54C07C45/40B01J23/889
Inventor 秦祖赠刘杰王锦文曾玉凤刘自力
Owner GUANGXI UNIV
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