WO2021093459A1 - 一种利用超临界co2萃取和二级分子蒸馏工艺制备艾叶精油及其副产物的方法 - Google Patents

一种利用超临界co2萃取和二级分子蒸馏工艺制备艾叶精油及其副产物的方法 Download PDF

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WO2021093459A1
WO2021093459A1 PCT/CN2020/116716 CN2020116716W WO2021093459A1 WO 2021093459 A1 WO2021093459 A1 WO 2021093459A1 CN 2020116716 W CN2020116716 W CN 2020116716W WO 2021093459 A1 WO2021093459 A1 WO 2021093459A1
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mugwort
extraction
essential oil
molecular distillation
supercritical
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English (en)
French (fr)
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林泽斌
黄建香
李�杰
黄丽华
邢澍祺
韩惠娟
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广东暨晴生物医药科技有限公司
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    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00—Essential oils; Perfumes
    • C11B9/02—Recovery or refining of essential oils from raw materials
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00—Essential oils; Perfumes
    • C11B9/02—Recovery or refining of essential oils from raw materials
    • C11B9/022—Refining
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00—Essential oils; Perfumes
    • C11B9/02—Recovery or refining of essential oils from raw materials
    • C11B9/025—Recovery by solvent extraction
    • C—CHEMISTRY; METALLURGY
    • C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
    • C11B9/00—Essential oils; Perfumes
    • C11B9/02—Recovery or refining of essential oils from raw materials
    • C11B9/027—Recovery of volatiles by distillation or stripping

Definitions

  • the invention relates to the technical field of wormwood processing biology, in particular to a method for preparing wormwood essential oil and its by-products by using supercritical CO 2 extraction and two-stage molecular distillation processes.
  • Mugwort leaves are dried leaves of wormwood, a herbaceous plant belonging to the genus Artemisia of the family Compositae.
  • Artemisia argyi is warm and pungent in nature and bitter in taste. It returns to the liver, spleen and kidney meridians.
  • Ai is mainly grown in the temperate zone of the northern hemisphere, Asia, Europe, North America and other regions around the world, and is mainly produced in Hubei, Anhui, Shandong, Hebei, Henan and other places in China.
  • the effective chemical components of mugwort mainly include volatile oil, flavonoids, tannins, polysaccharides, eucalyptanes, trace elements, etc.
  • composition and main component content also vary with the place of production, cultivation methods, selection of varieties, and harvest time. There are differences in the differences. Volatile oil is one of the main effective components of mugwort leaf.
  • the chemical composition of mugwort leaf volatile oil is not only very complex but also has a wide variety. Its main ingredients are eucalyptol, caryophyllene, caryophyllene oxide, borneol, camphor, enterpene alcohol and so on.
  • Supercritical CO 2 extraction is a chemical separation technology that has developed rapidly in the past two to three decades. In recent years, it has been applied to the extraction of natural products by many scholars at home and abroad with remarkable results.
  • Supercritical fluid refers to a fluid whose temperature and pressure are above the critical temperature and critical pressure, and has the advantages of both liquid and gas. By adjusting the temperature and adding suitable entrainers, it is possible to extract volatile oils, alkaloids, phenylpropanoids, flavonoids, organic phenolic acids and natural pigments from plants.
  • Supercritical CO 2 extraction technology often uses low-temperature extraction, which is not easy to destroy the heat sensitivity and aroma components of the raw materials, so it is especially suitable for extracting volatile components.
  • Molecular distillation technology is a distillation method that operates under high vacuum. It uses the difference in mean free path between different vapor molecules to separate liquid mixtures. Molecular distillation is operated at a temperature far below the boiling point, which is very suitable for the separation of heat sensitive and high boiling point compounds. At the same time, molecular distillation is operated at a very low pressure, and the materials are not easily damaged by oxidation. The residence time of the materials at the distillation temperature is generally between a few seconds to tens of seconds, which reduces the chance of thermal decomposition of the materials. The fractionation process of molecular distillation is a physical process, so it can well protect the separated substances from pollution.
  • the main industrial production technology of argyi leaf essential oil is steam distillation and organic solvent extraction.
  • the steam distillation method has high energy consumption, long heating time, easy destruction of heat-sensitive components, and mixed taste.
  • the solvent extraction method often contains solvent residues and insufficient extraction target selectivity, which has a certain impact on the composition and odor of mugwort essential oil.
  • the main methods for extracting essential oil from mugwort leaf are currently steam distillation method (CN201710698336.3) and solvent extraction method (CN201910348856.0), or a combination of the two with other methods, such as column chromatography (CN201510792656) .6).
  • the present invention prepares a product different from the steam distillation method of mugwort essential oil, and ensures the maximum retention of natural components of mugwort essential oil, and provides a process using supercritical CO 2 extraction and two-stage molecular distillation. Method for preparing mugwort essential oil and its by-products.
  • a method for preparing mugwort essential oil and its by-products by using supercritical CO 2 extraction and two-stage molecular distillation processes including the following steps:
  • Raw material pretreatment exposing fresh mugwort leaf material to rapid dehydration, drying in the shade, defoliating, selecting, removing impurities and smashing to obtain mugwort leaf powder;
  • Fine filtration filtering the semi-finished mugwort essential oil to obtain a finished mugwort essential oil
  • Two-stage molecular distillation the heavy phase of the crude oil extract of mugwort leaf I and the crude oil extract are mixed, heated in a water bath to dissolve, and second-stage molecular distillation is performed to obtain heavy mugwort leaf oil and mugwort wax.
  • the wormwood raw material is the wormwood leaf that can be used as a plant of the genus Artemisia of the wormwood family, including more than one wormwood leaf from the group consisting of wormwood, Nanyang wormwood, Tangyin wormwood and southern wormwood.
  • the water content of the mugwort leaf powder is 8-15 wt%, and the particle size is 10-40 mesh.
  • the extraction temperature of the extraction is 45-65° C.
  • the extraction pressure is 18-30 MPa
  • the extraction time is 2 to 4 hours.
  • the separation pressure of the high-pressure separation is 10-15 MPa, and the separation temperature is 35-60°C, more preferably 35-50°C.
  • the separation pressure of the low-pressure separation is 4-7 MPa, and the separation temperature is 30-50°C.
  • the temperature at which the water bath is heated and dissolved is 80°C.
  • the distillation temperature of the first-stage molecular distillation is 90-120°C
  • the vacuum degree is 15-200 Pa
  • the internal condensation temperature is 40-70°C
  • the cold trap temperature is -18-5°C. .
  • step (3) the semi-finished mugwort essential oil is collected in a cold trap.
  • the filter medium is a 0.45 ⁇ m pore size filter membrane.
  • the heating and dissolving temperature of the water bath after the heavy phase mixing of the crude oil extract I of mugwort leaf and the crude oil extract is 85°C.
  • the distillation temperature of the second-stage molecular distillation is 120-160°C
  • the vacuum degree is 5-50 Pa
  • the internal condensation temperature is 24-70°C, more preferably 20-40°C
  • the cold trap temperature It is -18 ⁇ 5°C.
  • the present invention has the following advantages and beneficial effects:
  • the method of the present invention pulverizes mugwort leaves, it is separated by supercritical CO 2 extraction and secondary molecular distillation to obtain mugwort leaf essential oil and its by-products mugwort leaf heavy oil and mugwort wax; wherein, the supercritical CO 2 extraction is carried out at low temperature
  • Molecular distillation is a short-time high-vacuum and low-pressure distillation, which can effectively protect the natural components of mugwort essential oil from being destroyed, and does not add any chemical solvents.
  • the obtained mugwort essential oil is natural, pollution-free, and has a pure and strong odor, which is the essential oil of mugwort.
  • the production and related product development provide technology and product quality assurance.
  • the method of the present invention undergoes secondary condensation on the internal condensation surface and cold trap, and finally collects mugwort essential oil at the cold trap, which can greatly improve the aroma and quality of mugwort essential oil;
  • the obtained mugwort essential oil is A light yellow or yellow-green clear liquid, the characteristic aroma of wormwood is strong and pure, and it is significantly different from the wormwood essential oil obtained by steam distillation and organic solvent extraction in terms of composition, color and smell.
  • the method of the present invention can extract the oil components of mugwort leaves to the greatest extent, and simultaneously obtain mugwort leaf essential oil, mugwort leaf heavy oil and mugwort wax, with high utilization rate of mugwort leaf resources; among them, mugwort leaf essential oil can be used in medicine, health care and cosmetics industries; mugwort leaf Heavy oil and wax can be used as raw materials for cleaning and skin care products.
  • Figure 1 is a process flow diagram of the present invention using supercritical CO 2 extraction and two-stage molecular distillation processes to prepare mugwort essential oil and its by-products.
  • the method for preparing mugwort essential oil and its by-products by using supercritical CO 2 extraction and two-stage molecular distillation process in the present invention includes the following steps:
  • Raw material pretreatment the fresh wormwood raw material is exposed to rapid dehydration, dried in the shade, defoliated, selected and removed, and crushed to obtain wormwood powder;
  • Fine filtration filtering the semi-finished mugwort essential oil to obtain a finished mugwort essential oil
  • Secondary molecular distillation mixing the crude oil extract I of mugwort leaf and the crude oil extract in heavy phase, heating and dissolving in a water bath, and performing a second-stage molecular distillation separation to obtain heavy oil of mugwort leaf and mugwort wax.
  • a method for preparing mugwort essential oil and its by-products by using supercritical CO 2 extraction and two-stage molecular distillation processes including the following steps:
  • step (2) Weigh 5 kg of Tangyin Bei Ai leaf powder from step (1) and place it in a 24L supercritical CO 2 extraction device, adjust the supercritical extraction temperature to 65°C, extraction pressure to 25MPa, and extraction time to 4h;
  • separation vessel I and separation vessel II After the extraction is completed, it is separated by separation vessel I and separation vessel II in turn; among them, the separation temperature of separation vessel I is 50°C, and the separation pressure is 15MPa; the separation temperature of separation vessel II is 50°C, and the separation pressure is 5.5MPa; I and separation kettle II are separated to obtain 38.5g of crude oil extract of mugwort leaf I and 130.5g of crude oil extract of mugwort leaf II respectively;
  • step (4) The semi-finished mugwort essential oil obtained in step (4) is allowed to stand for 2 hours, and filtered with a 0.45 ⁇ m pore size filter membrane to obtain 11.6 g of mugwort essential oil product.
  • step (3) After mixing the heavy phase of the crude oil extract I of mugwort leaf obtained in step (2) and the crude oil extract obtained in step (4), heat it in a water bath at 85°C to dissolve, and perform the second-stage molecular distillation.
  • the vacuum degree of molecular distillation is 5Pa, a distillation temperature of 160°C, an internal condensation temperature of 20°C, and a cold trap temperature of -5°C, molecular distillation yielded 42.1g of mugwort heavy oil and 88.2g of mugwort wax.
  • the southern mugwort essential oil prepared in this example is a yellow-green clear liquid, the main components are monoterpenes and sesquiterpenoids, and the yield of mugwort essential oil is 0.23%.
  • Mugwort heavy oil is a reddish-brown extract with a yield of 0.84%.
  • Mugwort wax is a dark brown solid with a yield of 1.76%. The total yield of the three products is 2.83%.
  • a method for preparing mugwort essential oil and its by-products by using supercritical CO 2 extraction and two-stage molecular distillation processes including the following steps:
  • the fresh wormwood wormwood raw material is exposed to rapid dehydration, dried in the shade, defoliated, selected and removed, and then pulverized through a 20-mesh sieve to obtain a wormwood wormwood powder with a moisture content of 12 wt%.
  • separation vessel I After the extraction is completed, it is separated by separation vessel I and separation vessel II in turn; among them, the separation temperature of separation vessel I is 35°C, and the separation pressure is 10MPa; the separation temperature of separation vessel II is 35°C, and the separation pressure is 4MPa; after separation vessel I Separate from Separation Kettle II to obtain 21.6 g of crude oil extract of mugwort leaf and 138.9 g of crude oil extract of mugwort leaf II, respectively.
  • step (4) The semi-finished mugwort essential oil obtained in step (4) is allowed to stand for 2 hours, and filtered with a 0.45 ⁇ m pore size filter membrane to obtain 15.2 g of mugwort essential oil product.
  • the southern mugwort essential oil prepared in this example is yellow-green, and its main components are monoterpenes and sesquiterpenoids.
  • the yield of mugwort essential oil is 0.25%.
  • Mugwort heavy oil is a reddish brown solid with a yield of 0.92%.
  • Mugwort wax is a dark brown solid with a yield of 1.22%.
  • the total yield of the three products is 2.40%.
  • a method for preparing mugwort essential oil and its by-products by using supercritical CO 2 extraction and two-stage molecular distillation processes including the following steps:
  • step (2) Weigh 70kg of Tangyin Bei Ai leaf powder from step (1) and place it in a 220L supercritical CO 2 extraction device for extraction.
  • the supercritical extraction temperature is 45°C
  • the extraction pressure is 21MPa
  • the extraction time is 3h;
  • separation vessel I After the extraction is completed, it is separated by separation vessel I and separation vessel II in turn; among them, the separation temperature of separation vessel I is 60°C, and the separation pressure is 12MPa; the separation temperature of separation vessel II is 30°C, and the separation pressure is 6MPa; after separation vessel I Separate from Separation Kettle II to obtain 359g of crude oil extract of mugwort leaf and 1935g of crude oil extract of mugwort leaf II, respectively.
  • step (4) The argyle leaf light oil obtained in step (4) is allowed to stand for 3 hours, and filtered with a 0.45 ⁇ m pore size filter membrane to obtain 265 g of argyle leaf essential oil product.
  • the wormwood essential oil prepared in this example is light yellow, and the main components are monoterpenes and sesquiterpenoids.
  • the yield of the wormwood essential oil is 0.38%.
  • Mugwort heavy oil is a red-brown solid with a yield of 0.87%, and the waxy moxa is a dark-brown solid with a yield of 1.67%.
  • the total yield of the three products is 2.91%.
  • a method for preparing mugwort essential oil and its by-products by using supercritical CO 2 extraction and two-stage molecular distillation processes including the following steps:
  • separation vessel I After the extraction is completed, it is separated by separation vessel I and separation vessel II in turn; among them, the separation temperature of separation vessel I is 45°C, and the separation pressure is 14Mpa; the separation temperature of separation vessel II is 45°C, and the separation pressure is 4MPa; after separation vessel I Separate from Separator II to obtain 361g of crude oil extract of mugwort leaf and 1389g of crude oil extract of mugwort leaf respectively;
  • step (4) The semi-finished mugwort essential oil obtained in step (4) is allowed to stand for 2 hours and filtered with a 0.45 ⁇ m pore size filter membrane to obtain 172 g of mugwort essential oil product.
  • the essential oil of mugwort leaf prepared in this example is light yellow, and its main components are monoterpenes and sesquiterpenoids.
  • the yield of mugwort essential oil is 0.34%.
  • Mugwort heavy oil is a reddish-brown solid with a yield of 0.88%.
  • Mugwort wax is a dark brown solid with a yield of 2.01%.
  • the total yield of the three products is 3.23%.
  • a method for preparing mugwort essential oil and its by-products by using supercritical CO 2 extraction and two-stage molecular distillation processes including the following steps:
  • step (2) Weigh 60kg of Mugwort Artemisia leaf powder from step (1) and place it in a 220L supercritical CO 2 extraction device.
  • the supercritical extraction temperature is 65°C
  • the extraction pressure is 27MPa
  • the extraction time is 3h;
  • separation vessel I After the extraction is completed, it is separated by separation vessel I and separation vessel II in turn; among them, the separation temperature of separation vessel I is 40°C, and the separation pressure is 12MPa; the separation temperature of separation vessel II is 35°C, and the separation pressure is 7MPa; after separation vessel I Separate from Separation Kettle II to obtain 350g of crude oil extract of mugwort leaf and 1940g of crude oil extract of mugwort leaf II, respectively.
  • step (4) The argyle leaf light oil obtained in step (4) is allowed to stand for 2 hours and filtered with a 0.45 ⁇ m pore size filter membrane to obtain 193 g of argyle leaf essential oil product.
  • step (2) Dissolve the crude oil extract I of mugwort leaf obtained in step (2) and the heavy phase mixed water bath of crude oil extract obtained in step (4) at 85°C, and perform the second-stage molecular distillation.
  • the vacuum degree of molecular distillation is 50 Pa.
  • the temperature is 120°C
  • the internal condensation temperature is 70°C
  • the cold trap temperature is -10°C
  • 557g of mugwort leaf oil and 1336g of mugwort wax are obtained by distillation.
  • the wormwood essential oil prepared in this example is a light yellow liquid, and the main components are monoterpenes and sesquiterpenoids.
  • the yield of the wormwood essential oil is 0.32%.
  • Mugwort heavy oil is a reddish brown solid with a yield of 0.93%.
  • Mugwort wax is a dark brown solid with a yield of 2.23%.
  • the total yield of the three products is 3.48%.
  • a method for preparing mugwort essential oil and its by-products by using supercritical CO 2 extraction and two-stage molecular distillation processes including the following steps:
  • step (2) Weigh 180 kg of Tangyin Bei Ai Ye powder from step (1) and place it in a 700L supercritical CO 2 extraction device, the supercritical extraction temperature is 45°C, the extraction pressure is 18MPa, and the extraction time is 3h;
  • separation vessel I After the extraction is completed, it is separated by separation vessel I and separation vessel II in turn; among them, the separation temperature of separation vessel I is 60°C, and the separation pressure is 13MPa; the separation temperature of separation vessel II is 35°C, and the separation pressure is 5MPa; after separation vessel I Separate from Separation Pot II to obtain 0.98 kg of crude oil extract of mugwort leaf and 4.47 kg of crude oil extract of mugwort leaf II, respectively.
  • step (4) The argyle leaf light oil obtained in step (4) was allowed to stand for 2 hours and filtered with a 0.45 ⁇ m pore size filter membrane to obtain 0.55 kg of argyle leaf essential oil product.
  • the wormwood essential oil prepared in this example is light yellow, the wormwood aroma is pure and strong, the main components are monoterpenes and sesquiterpenoids, and the yield of the wormwood essential oil is 0.31%.
  • Mugwort heavy oil is a reddish-brown solid with a yield of 0.86%.
  • Mugwort wax is a dark brown solid with a yield of 1.64%. The total yield of the three products is 2.81%.

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Abstract

本发明公开了一种利用超临界CO2萃取和二级分子蒸馏工艺制备艾叶精油及其副产物的方法。该方法包括如下步骤：(1)原料预处理，得到艾叶粉；(2)将艾叶粉进行超临界萃取分离，得到艾叶粗油提取物Ⅰ和艾叶粗油提取物Ⅱ；(3)艾叶粗油提取物Ⅱ经第一级分子蒸馏，得到艾叶精油半成品和粗油提取物重相；(4)艾叶精油半成品精滤，得到艾叶精油成品；(5)艾叶粗油提取物Ⅰ和粗油提取物重相混合，经第二级分子蒸馏分离，得到艾叶重油和艾叶蜡质。本发明方法能有效保护艾叶精油中的功能组分，所得艾叶精油纯天然、无污染、气味纯正浓郁。且得到艾叶重油和艾叶蜡质副产品，可作为清洁类、护肤类日化用品的制作原料，提高了艾叶资源的利用率。

Description

一种利用超临界CO 2萃取和二级分子蒸馏工艺制备艾叶精油及其副产物的方法 技术领域
本发明涉及艾草加工生物技术领域，特别涉及一种利用超临界CO 2萃取和二级分子蒸馏工艺制备艾叶精油及其副产物的方法。
背景技术
艾叶是菊科蒿属草本植物艾的干燥叶。艾叶性温、辛，味苦，归肝、脾、肾经，具有散寒止痛、温经止血的作用。艾在全球范围内主要种植于北半球的温带，亚欧、北美等地区，在国内主产于湖北、安徽、山东、河北、河南等地。艾叶的有效化学成分主要有挥发油、黄酮类、鞣质类、多糖类、桉叶烷类、微量元素等，其成分组成以及主要成分含量也是随着产地、栽培方式、品种选用、采收时间等的不同有所差异。挥发油为艾叶主要有效成分之一,艾叶挥发油的化学成分不仅十分复杂而且种类繁多，其主要成分有桉油精、石竹烯、氧化石竹烯、龙脑、樟脑、烯萜醇等。
超临界CO 2萃取是近二三十年迅速发展起来的一项化工分离技术，近年来被国内外很多学者应用于天然产物的提取，成果显著。超临界流体是指其温度及压力处于临界温度及临界压力以上的流体，兼具液体和气体的优点。通过调节温度、加入适宜的夹带剂等方法，便能够从植物中提取挥发油、生物碱、苯丙素、黄酮类、有机酚酸以及天然色素等成分。超临界CO 2萃取技术往往采用低温萃取，不容易破坏原料热敏性和香气成分，故尤其适宜于提取挥发性成分。
分子蒸馏技术是一种在高真空下操作的蒸馏方法，它利用不同蒸气分子间平均自由程的差异，对液体混合物进行分离。分子蒸馏是在远低于沸点的 温度下进行操作的，非常适合热敏性、高沸点化合物的分离。同时分子蒸馏在很低的压强下进行操作，物料不易氧化受损。物料在蒸馏温度下停留时间一般几秒至几十秒之间，减少了物料热分解的机会。分子蒸馏的分馏过程是物理过程，因而可很好地保护被分离物质不受污染。
目前工业上艾叶精油生产工艺主要为水蒸气蒸馏法和有机溶剂提取法。水蒸气蒸馏方法能耗大，加热时间长，热敏性成分易破坏，味道较杂。而溶剂提取法往往含有溶剂残留，提取目标选择性不足，对艾叶精油成分和气味具有一定影响。从艾叶精油提取现有专利技术上分析，目前艾叶精油提取方法主要为水蒸气蒸馏方法(CN201710698336.3)和溶剂提取方法(CN201910348856.0)，或者两者结合其他方法，如柱层析(CN201510792656.6)。最近采用的较为先进的提取方法如亚临界提取( CN201510752008.8)和超临界CO 2结合乙醇脱蜡法( CN201711378632.1)，也不可避免使用到有机溶剂。因此，研发一种天然、安全、无污染的艾叶精油提取制备方法对于艾叶精油在医药、保健和化妆品行业应用具有重要现实和经济意义。
发明内容
本发明为了提高艾叶资源的利用率，制备有别于水蒸气蒸馏法艾叶精油的产品，确保艾叶精油天然组分最大程度的保留，提供了一种利用超临界CO 2萃取和二级分子蒸馏工艺制备艾叶精油及其副产物的方法。
本发明的目的通过如下技术方案实现。
一种利用超临界CO 2萃取和二级分子蒸馏工艺制备艾叶精油及其副产物的方法，包括如下步骤：
(1)原料预处理：将新鲜的艾叶原料曝晒快速脱水、阴干、脱叶、挑选 除杂后粉碎，得到艾叶粉；
(2)超临界萃取分离：将所述艾叶粉置于超临界CO 2萃取装置内进行萃取，依次经分离釜Ⅰ和分离釜Ⅱ分别进行高压分离和低压分离，分别得到艾叶粗油提取物Ⅰ和艾叶粗油提取物Ⅱ；
(3)一级分子蒸馏：将所述艾叶粗油提取物Ⅱ水浴加热溶解，常温静置进行油水分离，待上层粗油提取物凝固后取出；再水浴加热溶解，经第一级分子蒸馏分离，得到艾叶精油半成品和粗油提取物重相；
(4)精滤：将所述艾叶精油半成品过滤，得到艾叶精油成品；
(5)二级分子蒸馏：将所述艾叶粗油提取物Ⅰ和粗油提取物重相混合，水浴加热溶解，进行第二级分子蒸馏分离，得到艾叶重油和艾叶蜡质。
优选的，所述艾叶原料为可作为艾用菊科蒿属植物的艾叶，包括蕲艾、南阳艾、汤阴北艾和南艾蒿中的一种以上的艾叶。
优选的，步骤(1)中，所述艾叶粉的含水量为8～15wt％，颗粒大小为10～40目。
优选的，步骤(2)中，所述萃取的萃取温度为45～65℃，萃取压力为18～30MPa，萃取时间为2～4h。
优选的，步骤(2)中，所述高压分离的分离压力为10～15MPa，分离温度为35～60℃，更优选为35～50℃。
优选的，步骤(2)中，所述低压分离的分离压力为4～7MPa，分离温度为30～50℃。
优选的，步骤(3)中，所述水浴加热溶解的温度均为80℃。
优选的，步骤(3)中，所述第一级分子蒸馏的蒸馏温度为90～120℃，真空度为15～200Pa，内冷凝温度为40～70℃，冷阱温度为-18～5℃。
优选的，步骤(3)中，所述艾叶精油半成品在冷阱处收集。
优选的，步骤(4)中，所述过滤介质为0.45μm孔径滤膜。
优选的，步骤(5)中，所述艾叶粗油提取物Ⅰ和所述粗油提取物重相混合后的水浴加热溶解温度为85℃。
优选的，步骤(5)中，所述第二级分子蒸馏的蒸馏温度120～160℃，真空度5～50Pa，内冷凝温度为24～70℃，更优选为20～40℃，冷阱温度为-18～5℃。
与现有技术相比，本发明具有如下优点和有益效果：
(1)本发明方法将艾叶进行粉碎后，经超临界CO 2萃取和二级分子蒸馏分离，得到艾叶精油及其副产品艾叶重油和艾叶蜡质；其中，超临界CO 2萃取为在低温下进行的萃取，而分子蒸馏为短时的高真空低压蒸馏，能有效保护艾叶精油天然组分不被破坏，且不添加任何化学溶剂，所得艾叶精油天然、无污染、气味纯正浓郁，从而为艾叶精油的生产及相关产品开发提供技术和产品质量保证。
(2)本发明方法将艾叶进行粉碎后，经超临界CO 2萃取和二级分子蒸馏，得到艾叶精油及其副产品艾叶重油和艾叶蜡质，步骤操作简便，无污染物产生，采用的设备均为常规设备，易实现工业化生产。
(3)本发明方法在第一级分子蒸馏过程中，经过内冷凝面和冷阱的二次冷凝，最后在冷阱处收集艾叶精油，能大大提高艾叶精油的香气和品质；所得艾叶精油为淡黄色或黄绿色清亮的液体，艾草特征香气浓郁纯正，与水蒸气蒸馏和有机溶剂萃取制取得到的艾叶精油在成分、颜色和气味上有显著差异。
(4)本发明方法能最大程度地提取艾叶中的油类成分，同时得到艾叶精油、艾叶重油和艾叶蜡质，艾叶资源利用率高；其中，艾叶精油可用于医药、 保健及化妆品行业；艾叶重油和蜡质可作为清洁类、护肤类日化用品的制作原料。
附图说明
图1为本发明利用超临界CO 2萃取和二级分子蒸馏工艺制备艾叶精油及其副产物的工艺流程图。
具体实施方式
以下结合具体实施例及附图对本发明的技术方案作进一步详细的描述，在此需要说明的是，对于这些实施方式的说明仅用于帮助理解本发明，本发明的保护范围及实施方式不限于此。此外，下面所描述的本发明各个实施方式中所涉及的技术特征只要彼此之间未构成冲突就可以相互组合。
参见图1所示，本发明利用超临界CO 2萃取和二级分子蒸馏工艺制备艾叶精油及其副产物的方法，包括如下步骤：
(1)原料预处理：将新鲜的艾草原料曝晒快速脱水、阴干、脱叶、挑选除杂后粉碎，得到艾叶粉；
(2)超临界萃取分离：将所述艾叶粉置于超临界CO 2萃取装置内进行萃取，依次经分离釜Ⅰ和分离釜Ⅱ进行高压分离和低压分离，分别得到艾叶粗油提取物Ⅰ和艾叶粗油提取物Ⅱ；
(3)一级分子蒸馏：将所述艾叶粗油提取物Ⅱ水浴加热溶解，常温静置进行油水分离，待上层粗油提取物凝固后取出；再水浴加热溶解，经第一级分子蒸馏分离，得到艾叶精油半成品和粗油提取物重相；
(4)精滤：将所述艾叶精油半成品过滤，得到艾叶精油成品；
(5)二级分子蒸馏：将所述艾叶粗油提取物Ⅰ和所述粗油提取物重相混合，水浴加热溶解，进行第二级分子蒸馏分离，得到艾叶重油和艾叶蜡质。
实施例1
一种利用超临界CO 2萃取和二级分子蒸馏工艺制备艾叶精油及其副产物的方法，包括如下步骤：
(1)将新鲜汤阴北艾艾草原料曝晒快速脱水、阴干、脱叶、挑选除杂后粉碎过10目筛，得到含水率为10wt％的汤阴北艾艾叶粉。
(2)称取5kg步骤(1)的汤阴北艾艾叶粉，置于24L超临界CO 2萃取装置内，调节超临界萃取温度为65℃，萃取压力为25MPa，萃取时间为4h；
萃取完毕后，依次经分离釜Ⅰ和分离釜Ⅱ分离；其中，分离釜Ⅰ的分离温度为50℃，分离压力为15MPa；分离釜Ⅱ的分离温度为50℃，分离压力5.5MPa；经分离釜Ⅰ和分离釜Ⅱ分离，分别得到艾叶粗油提取物Ⅰ38.5g和艾叶粗油提取物Ⅱ130.5g；
(3)将得到的艾叶粗油提取物Ⅱ水浴加热至80℃溶解，常温放置2h，待上层粗油提取物完全凝固后倒出粗油提取物中沥出的水分；
(4)将步骤(3)除去水分的艾叶粗油提取物加热至80℃溶解，进行第一级分子蒸馏，分子蒸馏的蒸馏温度为110℃，真空度为15Pa，内冷凝温度为50℃，冷阱温度为-5℃，分离得到艾叶精油半成品12.4g及粗油提取物重相105.3g；
(5)将步骤(4)中得到的艾叶精油半成品静置2h，用0.45μm孔径滤膜过滤，得到艾叶精油产品11.6g。
(6)将步骤(2)得到的艾叶粗油提取物Ⅰ和步骤(4)中得到的粗油提取物重相混合后水浴加热85℃溶解，进行第二级分子蒸馏，分子蒸馏真空度为5Pa，蒸馏温度为160℃，内冷凝温度为20℃，冷阱温度为-5℃，分子蒸馏得到艾叶重油42.1g和艾叶蜡质88.2g。
本实例制得的南艾蒿精油为黄绿色清亮液体，主要成分为单萜及倍半萜类化合物，艾叶精油得率为0.23％。艾叶重油为红棕色浸膏，得率为0.84％。艾叶蜡质为黑褐色固体，得率为1.76％。3种产品总得率为2.83％。
实施例2
一种利用超临界CO 2萃取和二级分子蒸馏工艺制备艾叶精油及其副产物的方法，包括如下步骤：
(1)将新鲜南艾蒿艾草原料曝晒快速脱水、阴干、脱叶、挑选除杂后粉碎过20目筛，得到含水率为12wt％的南艾蒿艾叶粉。
(2)称取6kg步骤(1)的南艾蒿艾叶粉，置于24L超临界CO 2萃取装置内，超临界萃取温度为45℃，萃取压力为18MPa，萃取时间为2h；
萃取完毕后，依次经分离釜Ⅰ和分离釜Ⅱ分离；其中，分离釜Ⅰ的分离温度为35℃，分离压力为10MPa；分离釜Ⅱ的分离温度为35℃，分离压力4MPa；经分离釜Ⅰ和分离釜Ⅱ分离，分别得到艾叶粗油提取物Ⅰ21.6g和艾叶粗油提取物Ⅱ138.9g。
(3)将得到的艾叶粗油提取物Ⅱ水浴80℃溶解，常温放置2h，待上层粗油提取物完全凝固后倒出粗油提取物中沥出的水分；
(4)将步骤(3)除去水分的艾叶粗油提取物加热至80℃溶解，进行第一级分子蒸馏，分子蒸馏的蒸馏温度为120℃，真空度为100Pa，内冷凝温度为40℃，冷阱温度为-18℃，分离得到艾叶精油半成品15.8g及粗油提取物重相111.6g；
(5)将步骤(4)中得到的艾叶精油半成品静置2h，用0.45μm孔径滤膜过滤，得到艾叶精油产品15.2g。
(6)将步骤(2)得到的艾叶粗油提取物Ⅰ和步骤(4)中得到的粗油提 取物重相混合后水浴85℃溶解，进行第二级分子蒸馏，蒸馏温度为140℃，真空度为15Pa，内冷凝温度为30℃，冷阱温度为-18℃，分子蒸馏得到艾叶重油55.2g和艾叶蜡质73.4g。
本实例制得的南艾蒿精油呈黄绿色，主要成分为单萜及倍半萜类化合物，艾叶精油得率为0.25％。艾叶重油为红棕色固体，得率为0.92％。艾叶蜡质为黑褐色固体，得率为1.22％。3种产品总得率为2.40％。
实施例3
一种利用超临界CO 2萃取和二级分子蒸馏工艺制备艾叶精油及其副产物的方法，包括如下步骤：
(1)新鲜汤阴北艾收割后，经过曝晒快速脱水、阴干、脱叶、挑选除杂后粉碎过40目筛，得到含水率为12wt％的汤阴北艾艾叶粉。
(2)称取70kg步骤(1)的汤阴北艾艾叶粉，置于220L超临界CO 2萃取装置内萃取，超临界萃取温度为45℃，萃取压力为21MPa，萃取时间3h；
萃取完毕后，依次经分离釜Ⅰ和分离釜Ⅱ分离；其中，分离釜Ⅰ的分离温度为60℃，分离压力为12MPa；分离釜Ⅱ的分离温度为30℃，分离压力6MPa；经分离釜Ⅰ和分离釜Ⅱ分离，分别得到艾叶粗油提取物Ⅰ359g和艾叶粗油提取物Ⅱ1935g。
(3)将得到的艾叶粗油提取物Ⅱ水浴80℃溶解，常温放置8h，待上层粗油提取物凝固后取出上层粗油提取物；
(4)将步骤(3)除去水分的艾叶粗油提取物加热至80℃溶解，进行第一级分子蒸馏，分子蒸馏的蒸馏温度为120℃，真空度为150Pa，内冷凝温度为55℃，冷阱温度为5℃，分离得到艾叶精油半成品270g及其粗油提取物重相1504g；
(5)将步骤(4)中得到的艾叶轻油静置3h，用0.45μm孔径滤膜过滤，得到艾叶精油产品265g。
(6)将步骤(2)得到的艾叶粗油提取物Ⅰ和步骤(4)得到的粗油提取物重相混合后水浴85℃溶解，进行第二级分子蒸馏，分子蒸馏真空度为30Pa，蒸馏温度为150℃，内冷凝温度为30℃，冷阱温度为5℃，得到艾叶重油610g和艾叶蜡质1169g。
本实例制得的艾叶精油呈淡黄色，主要成分为单萜及倍半萜类化合物，艾叶精油得率为0.38％。艾叶重油为红棕色固体，得率为0.87％，艾叶蜡质为黑褐色固体，得率为1.67％。3种产品总得率为2.91％。
实施例4
一种利用超临界CO 2萃取和二级分子蒸馏工艺制备艾叶精油及其副产物的方法，包括如下步骤：
(1)将新鲜南艾蒿收割后，曝晒快速脱水、阴干、脱叶、挑选除杂后粉碎过10目筛，得到含水率为15wt％的南艾蒿艾叶粉。
(2)称取50kg步骤(1)的南艾蒿艾叶粉，置于220L超临界CO 2萃取装置内，超临界萃取温度为55℃，萃取压力为30MPa，萃取时间为3h；
萃取完毕后，依次经分离釜Ⅰ和分离釜Ⅱ分离；其中，分离釜Ⅰ的分离温度为45℃，分离压力为14Mpa；分离釜Ⅱ的分离温度为45℃，分离压力4MPa；经分离釜Ⅰ和分离釜Ⅱ分离，分别得到艾叶粗油提取物Ⅰ361g和艾叶粗油提取物Ⅱ1389g；
(3)将得到的艾叶粗油提取物Ⅱ在水浴80℃溶解，常温静置8h，待上层粗油提取物凝固后取出上层粗油提取物；
(4)将步骤(3)除去水分的艾叶粗油提取物加热至80℃溶解后，进行 第一级分子蒸馏，分子蒸馏的蒸馏温度为90℃，真空度为200Pa，内冷凝温度为70℃，冷阱温度为-10℃，分离得到艾叶精油半成品175g及其粗油提取物重相1104g；
(5)将步骤(4)中得到的艾叶精油半成品静置2h，0.45μm孔径滤膜过滤，得到艾叶精油产品172g。
(6)将步骤(2)得到的艾叶粗油提取物Ⅰ和步骤(4)中得到的粗油提取物重相混合水浴85℃溶解，进行第二级分子蒸馏。分子蒸馏真空度为50Pa，蒸馏温度为130℃，内冷凝温度为40℃，冷阱温度为-5℃，分子蒸馏得到艾叶重油439g和艾叶蜡质1007g。
本实例制得的艾叶精油呈淡黄色，主要成分为单萜及倍半萜类化合物，艾叶精油得率为0.34％。艾叶重油为红棕色固体，得率为0.88％。艾叶蜡质为黑褐色固体，得率为2.01％。3种产品总得率为3.23％。
实施例5
一种利用超临界CO 2萃取和二级分子蒸馏工艺制备艾叶精油及其副产物的方法，包括如下步骤：
(1)新鲜南艾蒿收割后，曝晒快速脱水、阴干、脱叶、挑选除杂后粉碎过10目筛，得到含水率为8wt％的南艾蒿艾叶粉。
(2)称取60kg步骤(1)的南艾蒿艾叶粉，置于220L超临界CO 2萃取装置内，超临界萃取温度为65℃，萃取压力27MPa，萃取时间3h；
萃取完毕后，依次经分离釜Ⅰ和分离釜Ⅱ分离；其中，分离釜Ⅰ的分离温度为40℃，分离压力为12MPa；分离釜Ⅱ的分离温度为35℃，分离压力7MPa；经分离釜Ⅰ和分离釜Ⅱ分离，分别得到艾叶粗油提取物Ⅰ350g和艾叶粗油提取物Ⅱ1940g。
(3)将得到的艾叶粗油提取物Ⅱ在80℃水浴溶解，常温放置8h，待上层粗油提取物凝固后取出上层粗油提取物；
(4)将步骤(3)除去水分的艾叶粗油提取物加热至80℃溶解后，进行第一级分子蒸馏，分子蒸馏的蒸馏温度为100℃，真空度为200Pa，内冷凝温度为60℃，冷阱温度为-5℃，分离得到艾叶精油半成品197g及粗油提取物重相1560g；
(5)将步骤(4)中得到的艾叶轻油静置2h，0.45μm孔径滤膜过滤，得到艾叶精油产品193g。
(5)将步骤(2)得到的艾叶粗油提取物Ⅰ和步骤(4)得到的粗油提取物重相混合水浴85℃溶解，进行第二级分子蒸馏，分子蒸馏真空度为50Pa，蒸馏温度为120℃，内冷凝温度为70℃，冷阱温度为-10℃，蒸馏得到艾叶重油557g和艾叶蜡质1336g。
本实例制得的艾叶精油为淡黄色液体，主要成分为单萜及倍半萜类化合物，艾叶精油得率为0.32％。艾叶重油为红棕色固体，得率为0.93％。艾叶蜡质为黑褐色固体，得率为2.23％。3种产品总得率为3.48％。
实施例6
一种利用超临界CO 2萃取和二级分子蒸馏工艺制备艾叶精油及其副产物的方法，包括如下步骤：
(1)新鲜汤阴北艾收割后，经曝晒快速脱水、阴干、脱叶、挑选除杂后粉碎过30目筛，得到含水率为15wt％的汤阴北艾艾叶粉。
(2)称取180kg步骤(1)的汤阴北艾艾叶粉，置于700L超临界CO 2萃取装置内，超临界萃取温度为45℃，萃取压力18MPa，萃取时间3h；
萃取完毕后，依次经分离釜Ⅰ和分离釜Ⅱ分离；其中，分离釜Ⅰ的分离 温度为60℃，分离压力为13MPa；分离釜Ⅱ的分离温度为35℃，分离压力5MPa；经分离釜Ⅰ和分离釜Ⅱ分离，分别得到艾叶粗油提取物Ⅰ0.98kg和艾叶粗油提取物Ⅱ4.47kg。
(3)将得到的艾叶粗油提取物Ⅱ在80℃水浴溶解，常温放置8h，待上层粗油提取物凝固后取出上层粗油提取物；
(4)将步骤(3)除去水分的艾叶粗油提取物加热至80℃溶解后，进行第一级分子蒸馏，蒸馏温度为100℃，真空度为150Pa，内冷凝温度为40℃，冷阱温度为-10℃，分离得到艾叶轻油0.56kg及其粗油提取物重相3.63kg；
(5)将步骤(4)中得到的艾叶轻油静置2h，0.45μm孔径滤膜过滤，得到艾叶精油产品0.55kg。
(5)将步骤(2)得到的艾叶粗油提取物Ⅰ和步骤(4)得到的粗油提取物重相混合水浴85℃溶解混匀，进行第二级分子蒸馏，分子蒸馏真空度为10Pa，蒸馏温度为150℃，内冷凝温度为40℃，冷却温度为-5℃，蒸馏得到艾叶重油1.54kg和艾叶蜡质2.94kg。
本实例制得的艾叶精油呈淡黄色，艾草香气纯正浓郁，主要成分为单萜及倍半萜类化合物，艾叶精油得率为0.31％。艾叶重油为红棕色固体，得率为0.86％。艾叶蜡质为黑褐色固体，得率为1.64％。3种产品总得率为2.81％。
以上实施例仅为本发明的较优实施例，仅在于对本发明技术方案作进一步详细描述，用于帮助理解本发明技术方案的原理。同时，对于本领域的一般技术人员，依据本发明技术方案，在具体实施方式以及应用范围上均会有改变之处，综上所述，任何未脱离本发明原理及其精神实质下所做的变更、组合、删除、替换或修改等均将包含在本发明的保护范围内。

Claims (10)

  1. 一种利用超临界CO 2萃取和二级分子蒸馏工艺制备艾叶精油及其副产物的方法，其特征在于，包括如下步骤：
    (1)原料预处理：将新鲜的艾叶原料曝晒快速脱水、阴干、脱叶、挑选除杂后粉碎，得到艾叶粉；
    (2)超临界萃取分离：将所述艾叶粉置于超临界CO 2萃取装置内进行萃取，依次经分离釜Ⅰ和分离釜Ⅱ分别进行高压分离和低压分离，分别得到艾叶粗油提取物Ⅰ和艾叶粗油提取物Ⅱ；
    (3)一级分子蒸馏：将所述艾叶粗油提取物Ⅱ水浴加热溶解，常温静置进行油水分离，待上层粗油提取物凝固后取出；再水浴加热溶解，经第一级分子蒸馏分离，得到艾叶精油半成品和粗油提取物重相；
    (4)精滤：将所述艾叶精油半成品过滤，得到艾叶精油成品；
    (5)二级分子蒸馏：将所述艾叶粗油提取物Ⅰ和所述粗油提取物重相混合，水浴加热溶解，进行第二级分子蒸馏分离，得到艾叶重油和艾叶蜡质。
  2. 根据权利要求1所述的一种利用超临界CO 2萃取和二级分子蒸馏工艺制备艾叶精油及其副产物的方法，其特征在于，步骤(1)中，所述艾叶原料包括蕲艾、南阳艾、汤阴北艾和南艾蒿中的一种以上的艾叶；所述艾叶粉的含水量为8～15wt％，颗粒大小为10～40目。
  3. 根据权利要求1所述的一种利用超临界CO 2萃取和二级分子蒸馏工艺制备艾叶精油及其副产物的方法，其特征在于，步骤(2)中，所述萃取的萃取温度为45～65℃，萃取压力为18～30MPa，萃取时间为2～4h。
  4. 根据权利要求1所述的一种利用超临界CO 2萃取和二级分子蒸馏工 艺制备艾叶精油及其副产物的方法，其特征在于，步骤(2)中，所述高压分离的分离压力为10～15MPa，分离温度为35～50℃。
  5. 根据权利要求1所述的一种利用超临界CO 2萃取和二级分子蒸馏工艺制备艾叶精油及其副产物的方法，其特征在于，步骤(2)中，所述低压分离的分离压力为4～7MPa，分离温度为30～50℃。
  6. 根据权利要求1所述的一种利用超临界CO 2萃取和二级分子蒸馏工艺制备艾叶精油及其副产物的方法，其特征在于，步骤(3)中，所述水浴加热溶解的温度均为80℃。
  7. 根据权利要求1所述的一种利用超临界CO 2萃取和二级分子蒸馏工艺制备艾叶精油及其副产物的方法，其特征在于，步骤(3)中，所述第一级分子蒸馏的蒸馏温度为90～120℃，真空度为15～200Pa，内冷凝温度为40～70℃，冷阱温度为-18～5℃；所述艾叶精油半成品在冷阱处收集。
  8. 根据权利要求1所述的一种利用超临界CO 2萃取和二级分子蒸馏工艺制备艾叶精油及其副产物的方法，其特征在于，步骤(4)中，所述过滤介质为0.45μm孔径滤膜。
  9. 根据权利要求1所述的一种利用超临界CO 2萃取和二级分子蒸馏工艺制备艾叶精油及其副产物的方法，其特征在于，步骤(5)中，所述水浴加热溶解的温度为85℃。
  10. 根据权利要求1所述的一种利用超临界CO 2萃取和二级分子蒸馏工艺制备艾叶精油及其副产物的方法，其特征在于，步骤(5)中，所述第二级分子蒸馏的蒸馏温度120～160℃，真空度5～50Pa，内冷凝温度为20～40℃，冷阱温度为-18～5℃。
PCT/CN2020/116716 2019-11-15 2020-09-22 一种利用超临界co2萃取和二级分子蒸馏工艺制备艾叶精油及其副产物的方法 WO2021093459A1 (zh)

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