Method and apparatus for separating benzaldehyde, phenylpropyl aldehyde, cinnamaldehyde, cinnamyl acetate and o-methoxycinnamaldehyde from cinnamon oil

A technology of cinnamon oil and molecular distillation, which is applied in chemical instruments and methods, fat oil/fat refining, separation/purification of carbonyl compounds, etc., can solve the problems of high cost, waste of resources, high energy consumption, etc. The effect of improving yield and efficient separation

Active Publication Date: 2014-08-13
SUN YAT SEN UNIV
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  • Summary
  • Abstract
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Problems solved by technology

The disadvantage of the above-mentioned studies is that although the yield of cinnamon essential oil is high, the purity of cinnamaldehyde is low, and it is difficult to meet the requirements for high-purity natural cinnamaldehyde
This study shows that in the absence of a substrate circulation pump, it is difficult to ensure the recovery of the product while increasing the concentration of the p

Method used

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  • Method and apparatus for separating benzaldehyde, phenylpropyl aldehyde, cinnamaldehyde, cinnamyl acetate and o-methoxycinnamaldehyde from cinnamon oil

Examples

Experimental program
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Effect test

Embodiment 1

[0027] Add 500.0 g of cinnamon oil containing 1.2% benzaldehyde, 0.7% phenylpropanal, 85% cinnamaldehyde, 0.7% acetate cinnamaldehyde and 4.5% o-methoxycinnamaldehyde. Water sodium sulfate for dehydration, put the processed cinnamon oil into material tank 1, control the rectifying column temperature at 75℃, evaporation temperature at 45℃, total reflux for 30min, reflux ratio of 1.5 and vacuum degree of 200 Pa, and collect the components in this section Obtain 3.2g of benzaldehyde with a purity of 63.2%; increase the rectifying column temperature to 85°C, evaporation temperature 55°C, total reflux for 40min, reflux ratio of 2.5 and vacuum degree of 130Pa, collect the components in this section, and obtain 1.8g with a purity of 51.4 % Phenylpropanal; keep the distillation column temperature 85℃, increase and control the evaporation temperature 80℃, total reflux 40 min, reflux ratio 3 and vacuum degree 50 Pa, collect 370.0g cinnamon with 99.5% purity in this section Aldehydes; inc...

Embodiment 2

[0030] Add 500.0 g of cinnamon oil containing 1.2% benzaldehyde, 0.7% phenylpropanal, 85% cinnamaldehyde, 0.7% acetic acid cinnamaldehyde, and 4.5% o-methoxycinnamaldehyde, and add 45g Water sodium sulfate is dehydrated, the processed cinnamon oil is put into material tank 1, and the material tank 1 of the molecular distillation and rectification coupling device is added to control the temperature of the rectification column, the evaporation temperature, the reflux ratio, the degree of vacuum, and the rectification conditions. As follows: distillation column temperature 78℃, evaporation temperature 40℃, total reflux 35min, reflux ratio 2 and vacuum degree 220Pa. Collect the components in this section to obtain 3.1g of benzaldehyde with a purity of 61.7%; increase the distillation column temperature by 82 ℃, evaporation temperature 60℃, total reflux 48min, reflux ratio 3 and vacuum degree 120Pa, collect the components in this section, obtain 1.92g phenylpropanal with a purity of ...

Embodiment 3

[0033] Add 500.0g of cinnamon oil with 1.2% benzaldehyde content, 0.7% phenylpropanal content, 85% cinnamaldehyde content, 0.7% acetate cinnamaldehyde content, and 4.5% o-methoxycinnamaldehyde content. Water sodium sulfate is dehydrated, the processed cinnamon oil is put into material tank 1, and the material tank 1 of the molecular distillation and rectification coupling device is added to control the temperature of the rectification column, the evaporation temperature, the reflux ratio, the degree of vacuum, and the rectification conditions. As follows: distillation column temperature 80℃, evaporation temperature 50℃, total reflux 40 min, reflux ratio 1.5 and vacuum degree 180 Pa. Collect the components in this section to obtain 3.6g of benzaldehyde with a purity of 66.0%; raise the distillation column Temperature 88℃, evaporating temperature 68℃, total reflux 40 min, reflux ratio 3 and vacuum degree 110Pa, collect the components in this section, obtain 2.06g phenylpropanal wi...

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Abstract

The present invention discloses a method and an apparatus for separating benzaldehyde, phenylpropyl aldehyde, cinnamaldehyde, cinnamyl acetate and o-methoxycinnamaldehyde from cinnamon oil. The method comprises: (1) dewatering cinnamon oil, wherein vapor distillation is performed to obtain cinnamon oil, and anhydrous sodium sulfate is added, wherein a weight ratio of anhydrous sodium sulfate to cinnamon oil is 1:10-1:12; and (2) adding the treated cinnamon oil to a material tank, and controlling the rectification column temperature, the evaporation temperature, the reflux ratio and the vacuum degree so as to respectively obtain benzaldehyde having the purity of more than or equal to 60% and the yield of more than or equal to 50%, phenylpropyl aldehyde having the purity of more than or equal to 50% and the yield of more than or equal to 40%, cinnamaldehyde having the purity of more than or equal to 99% and the yield of more than or equal to 85%, cinnamyl acetate having the purity of more than or equal to 30% and the yield of more than or equal to 80%, and o-methoxycinnamaldehyde having the purity of more than or equal to 30% and the yield of more than or equal to 85%. The apparatus combines advantages of molecular distillation and rectification, such that the concentrations of benzaldehyde and other components are significantly increased, the product yield is significantly increased, the production cost is substantially reduced, and the low energy consumption and efficient separation of a plurality of heat-sensitive materials can be achieved at a low temperature.

Description

Technical field [0001] The invention relates to the field of separation of spices, in particular to a method and device for separating benzaldehyde, phenylpropanal, cinnamaldehyde, cinnamyl acetate and o-methoxycinnamaldehyde from cinnamon oil. Background technique [0002] Cinnamon is mainly distributed in Guangxi and Guangdong in China. Cinnamon oil can be obtained from the bark, branches and leaves of cinnamon after steam extraction. my country is a large exporter of cinnamon oil, which accounts for about 80% of the world’s exports, but mainly crude cinnamon oil is exported with low added value. The method of increasing the content of components in cinnamon oil or separating them from cinnamon oil is called single ionization. For cinnamon oil separated products with higher purity, the added value of the products will be significantly improved. In this regard, further research and development are urgently needed. The main component of cinnamon oil is cinnamaldehyde, which acc...

Claims

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Application Information

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IPC IPC(8): C11B3/12C07C45/82C07C47/54C07C47/228C07C47/232C07C47/277C07C67/54C07C69/157
CPCY02P20/582
Inventor 纪红兵杨祖金
Owner SUN YAT SEN UNIV
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