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Method and device for extracting cinnamaldehyde-rich composition from cinnamon bark

A technology of cinnamon bark and cinnamaldehyde, applied in separation methods, chemical instruments and methods, solvent extraction, etc., can solve the problems of difficult separation of essential oils, insufficient efficiency, and low content of cinnamaldehyde

Active Publication Date: 2020-06-05
三益创价生物科技(深圳)有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

In addition, CN201210518917.1, CN102964228B, CN102964229B, CN201210518899.7, CN201210518963.1, CN201220666255.8, CN201220666403.6 respectively utilize complex steam distillation equipment to extract cinnamaldehyde, to still not improve the yield, but the efficiency
[0004] Take the solvent extraction method as an example, for example: China Taiwan No. 401394 patent, with methanol, CH containing ether 2 N 2 Organic solvent extraction such as solution, and then chloroform distribution extraction; Chinese Taiwan No. I495487 patent, by being selected from ethanol, propylene glycol, 1,3-butanediol, chloroform, dichloroethane, carbon tetrachloride, acetone, One or two or more extraction solvents of ethyl acetate and hexane are used for extraction; China Taiwan Patent No. I549686 continuously extracts cinnamon with methanol, and after three consecutive extractions, methanol extract is obtained. The methanol extract uses Methanol, water and n-hexane are used for partition extraction; CN201710245493.9 uses n-hexane as a solvent to extract cinnamon; but the disadvantage of these organic solvent extraction methods is that it is difficult to completely remove harmful organic solvents after extraction
[0005] Taking the supercritical carbon dioxide extraction method as an example, for example: China Taiwan No. I352611 patent, extracts the fat-soluble essential oil components in the cinnamon leaf fragments with supercritical carbon dioxide; but the extract obtained by the supercritical carbon dioxide extraction method has a main component of Essential oil, cinnamaldehyde content is low, and it is not easy to separate from essential oil

Method used

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  • Method and device for extracting cinnamaldehyde-rich composition from cinnamon bark
  • Method and device for extracting cinnamaldehyde-rich composition from cinnamon bark
  • Method and device for extracting cinnamaldehyde-rich composition from cinnamon bark

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0081] Leaves of Cinnamomum cassia were washed, dried, and then crushed into 1-10 mm pieces.

[0082] Weigh 350 grams of cinnamon leaf fragments, pour them into the extraction tank of the subcritical propane fluid extraction device, and then in order: determine the path of the pump, extraction tank, separation tank, etc. to empty the original air; inject propane with the same pressure as the propane storage tank (8 bar); set the extraction conditions as follows: propane flow rate 12 liters / hour, extraction tank pressure 45 bar / temperature 60°C, separation tank pressure 8-10 bar / temperature 50°C. Carry out propane subcritical extraction 2 hours with above-mentioned condition, obtain product 3.7 grams, its GC-MS collection of illustrative plates sees figure 1 , where the main components: cinnamaldehyde content of about 42%, the extraction rate of 86.3% (3.7x0.42 / 1.8); secondary components: o-methoxycinnamic aldehyde (o-methoxycinnamic aldehyde) about 11.2%, stearic acid formald...

Embodiment 2～13

[0087] Similar to Preliminary Example 1, but the subcritical extraction conditions are slightly different, see Table 2, and the amount of the obtained product is also shown in Table 2 below. Wherein the GC-MS collection of illustrative plates of preliminary embodiment 8,9,12,13 see respectively figure 2 , 3, 4, 5, wherein the cinnamaldehyde content is about 36-42%, and the yield is about 2.5-3.5g.

[0088] Table 2: Propane flow rate (L / hr), extraction tank pressure (bar), extraction tank temperature (° C.), product weight (g) in preliminary examples 1 to 13.

[0089]

[0090] There are 16 main components, minor components, and other detected components of preliminary examples 2 to 13, all of which are similar to those of preliminary example 1, and the ratio is also similar, with figure 2 , 3, 4, 5 and figure 1 comparison can be confirmed. Also, the content of cinnamaldehyde in preliminary example 8 is 36%, and the yield is 2.5%; the content of cinnamaldehyde in prelim...

Embodiment 2

[0100] Extract cinnamon bark according to the SPE extraction conditions described in Preliminary Example 1. The raw material is cassia bark, obtain 386 grams of cinnamaldehyde composition, add alcohol twice the weight of cinnamaldehyde composition, stir well, and import it Figure 9 In the SFF extraction tank of the shown SFF device, the flow of carbon dioxide in the SFF extraction tank is 15 to 16 kg / hour, the pressure is 100 bar, and the temperature is 60°C; the flow of carbon dioxide in the first SFF fractionation tank is 15 to 16 kg / hour, The pressure is 75 bar and the temperature is 60°C; the carbon dioxide flow rate of the second SFF fractionation tank is 15-16 kg / hour, the pressure is 50 bar, and the temperature is 50°C; and the carbon dioxide flow rate of the third SFF fractionation tank is 15-16 kg per hour, the pressure is 45 bars, and the temperature is 20 ℃ under the conditions of supercritical fractionation, 261 grams of cinnamaldehyde-rich composition can be extrac...

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Abstract

The invention discloses a method and device for extracting a cinnamaldehyde-rich composition from cinnamon bark, and relates to the technical field of chemical extraction. The method comprises the following steps: washing cinnamon bark, drying and crushing into fragments; pouring the cinnamon bark fragments into an SPE extraction tank of a subcritical propane fluid extraction device for subcritical propane fluid extraction; introducing the extraction fluid into an SPE separation tank; removing propane in the SPE separation tank to obtain a cinnamaldehyde composition; performing supercritical fractionation on the cinnamaldehyde composition with supercritical fractionation equipment at least comprising an SFF extraction tank, a first SFF fractionation tank, a second SFF fractionation tank and a third SFF fractionation tank, wherein the subcritical propane fluid extraction conditions are as follows: the pressure of the SPE extraction tank is 30-55 bar, and the temperature is 40-75 DEG C;the supercritical fractionation conditions are as follows: the pressure of the SFF extraction tank is 75-350 bar, the temperature of the SFF extraction tank is 32-100 DEG C, the pressure of the firstSFF fractionation tank is 74-250 bar, the temperature of the first SFF fractionation tank is 32-100 DEG C, the pressure of the second SFF fractionation tank is 45-200 bar, the temperature of the second SFF fractionation tank is 32-100 DEG C, and the pressure of the third SFF fractionation tank is 40-150 bar, and the temperature is 5-100 DEG C.

Description

technical field [0001] The invention relates to the technical field of chemical extraction, in particular to a method and a device for extracting a composition rich in cinnamaldehyde from cinnamon bark. Background technique [0002] Cinnamon root / bark / branch / leaf contains cinnamaldehyde, and the known extraction methods include water extraction, organic solvent extraction, and supercritical fluid extraction. [0003] Take the water extraction method as an example, for example: China Taiwan Patent Application No. 099114436, which is extracted with distilled water in a boiling state; Boil soil cinnamon leaves to obtain extract; China Taiwan Patent No. I494117, continuous distillation with steam distillation method to obtain water extract containing cinnamaldehyde; CN201610660116.7 extract with water vapor; but because cinnamaldehyde is a hydrophobic substance , so the extraction efficiency of these methods is not high, and the content of cinnamaldehyde in the extracted compos...

Claims

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Application Information

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IPC IPC(8): B01D11/02B01D3/14
CPCB01D3/14B01D11/0203B01D11/0284B01D11/0288
Inventor 吴宇建蔡庆瑞林圣富林士闳卢士钧席美华吴靖苡吴鑫阳吴宣德
Owner 三益创价生物科技(深圳)有限公司
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