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Guaiazulene and extraction process thereof

A technology of guaiazulene and extraction process, which is applied in the field of extracting guaiazulene, can solve problems such as unsuitability for industrialized batch production, limited guaiazulene amount, difficult separation of guaiazulene, etc., and achieve High marketing value, promote wound healing, improve the effect of purity

Pending Publication Date: 2018-11-23
昆山铭达百晟贸易有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Most of the existing guaiazulene is artificially synthesized, and the guaiazulene obtained by extracting volatile oil from natural spices generally contains a mixture of various compounds, and the properties of each component are similar to guaiazulene. Difficult to isolate high-purity guaiazulene from
In addition, the content of guaiazulene in plants is low, so the amount of guaiazulene extracted from a single plant in the prior art is limited, and it is not suitable for industrial batch production

Method used

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  • Guaiazulene and extraction process thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Put 2000kg of natural essence and fragrance oil containing azulene compounds into a fractionation still, distill by steam distillation, and then fractionate under reduced pressure, collect the cuts at 125°C in a vacuum environment to obtain guaiazulene-containing oil fraction A of hydrocarbons;

[0033] (2) Inhale 800 kg of the obtained fraction A into a vacuum dehydration reactor, and simultaneously add 24 kg of boric acid, slowly heat to 200° C., carry out dehydration treatment, and then undergo vacuum distillation to obtain fraction B after the reaction is completed;

[0034] (3) Inhale 720 kg of the obtained fraction B in the dehydrogenation reactor, and add 144 kg of sulfur as a catalyst at the same time, heat to 210 ° C, carry out dehydrogenation treatment, after the reaction is completed, cool, and then inhale in the vacuum still, heat Distill at 210°C to obtain a blue oil-containing hydrocarbon mixture;

[0035] (4) After cooling the gained blue oleo hydroc...

Embodiment 2

[0041] (1) Put 2000kg of natural essence and fragrance oil containing azulene compounds into a fractionation still, distill by steam distillation, and then fractionate under reduced pressure, collect the cuts at 124°C in a vacuum environment to obtain guaiazulene-containing oil fraction A of hydrocarbons;

[0042] (2) Inhale 800 kg of the obtained fraction A in the vacuum dehydration reactor, and add 8 kg of sulfuric acid at the same time, slowly heat to 210° C., carry out dehydration treatment, and after the reaction is completed, then undergo vacuum distillation to obtain the fraction B;

[0043] (3) Inhale 720 kg of the obtained fraction B into the dehydrogenation reactor, and simultaneously add 36 kg of sulfur as a catalyst, heat to 220 ° C, and perform dehydrogenation treatment. Distill at 220°C to obtain a mixed liquid containing blue oil and hydrocarbons;

[0044] (4) After cooling the obtained blue oleohydrocarbon mixed solution 570kg to room temperature, add 160kg an...

Embodiment 3

[0050] (1) Put 1000kg of natural essence and fragrance oil containing azulene compounds into a fractionation still, distill by steam distillation, and then fractionate under reduced pressure, collect the fractions at 120°C in a vacuum environment to obtain guaiazulene-containing oil fraction A of hydrocarbons;

[0051] (2) Inhale 400 kg of the obtained fraction A into a vacuum dehydration reactor, and simultaneously add 8 kg of boric acid, slowly heat to 200° C., carry out dehydration treatment, and then undergo vacuum distillation to obtain fraction B after the reaction is completed;

[0052] (3) Inhale 360 ​​kg of the obtained fraction B in the dehydrogenation reactor, and add 54 kg of sulfur as a catalyst at the same time, heat to 220 ° C, carry out dehydrogenation treatment, after the reaction is completed, cool, and then inhale in the vacuum still, heat Distill at 220°C to obtain a mixed liquid containing blue oil and hydrocarbons;

[0053] (4) After cooling the obtained...

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Abstract

The invention discloses guaiazulene and an extraction process thereof. The extraction process comprises the following steps: distilling and vacuum collecting natural essence and fragrance oil comprising an azulene compound, and obtaining a fraction A; dehydrating the fraction A, decompression distilling, and obtaining a fraction B; dehydrogenating the fraction B, vacuum distilling, and obtaining an azulene-containing mixed solution; adding an acid solution B and organic solvent into the azulene-containing mixed solution, uniformly mixing, standing, layering, uniformly mixing and stirring the acid layer solution, cold water A and petroleum ether, settling, discharging the acid water, filtering the residues, placing the residual solution into a recycling kettle, adding cold water B into therecycling kettle, slowly heating until all petroleum ether is completely distilled, cooling, standing, layering, removing the moisture, and obtaining a guaiazulene crude product; and crystallizing andfiltering the guaiazulene crude product, and obtaining a guaiazulene pure product with the purity being 99 percent or above and the yield of 2.9 to 3.6 percent. The extraction process is safe, and environmentally friendly, and prepared guaiazulene is high in purity and high in yield.

Description

technical field [0001] The invention relates to the technical field of compound extraction, and specifically provides a process for extracting guaiazulene from natural essential oils containing azulene compounds. Background technique [0002] Guaiazulene is a blue oily liquid or light blue-purple flaky crystal, which is sensitive to light, and will change from blue to green and finally yellow after continuous exposure to light; it is also resistant to heat, weak acids, and weak bases. Stable, easily soluble in liquid paraffin, soluble in hot ethanol and ether, extremely difficult to dissolve in water. In terms of efficacy, guaiazulene has anti-inflammatory effect, has significant inhibitory effect on dextran-induced edema in rats, only moderately inhibits hyaluronidase, formaldehyde, and histamine-induced edema, and can inhibit histamine, 5 - Release of serotonin, and has anti-histamine and anti-hyaluronic acid effects, thus reducing the permeability of capillaries. In add...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C13/52C07C7/00C07C7/04C07C7/11C07C7/12C07C7/14C07C7/148
CPCC07C7/005C07C7/04C07C7/14C07C7/14808C07C2602/30C07C7/10C07C13/52
Inventor 许峰
Owner 昆山铭达百晟贸易有限公司
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