CN108504460B - Method for extracting essential oil of Filipendula ulmaria - Google Patents
Method for extracting essential oil of Filipendula ulmaria Download PDFInfo
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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
- C11B9/027—Recovery of volatiles by distillation or stripping
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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
- C11B9/022—Refining
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Abstract
A method for extracting essential oil from Filipendula ulmaria relates to the field of Filipendula ulmaria processing, and solves the problem of low oil yield of the existing method for extracting essential oil from Filipendula ulmaria. The invention comprises the following steps: pretreating raw materials; canning; distilling; separating and refining; and (3) connecting two oil-water separators in series by adopting a two-stage separation mode, prolonging the retention time of the essential oil to completely separate the oil from the water, taking out the essential oil floating on the upper layer, drying and filtering to obtain the essential oil of the dropwort. The mosquito-repellent incense essential oil obtained by the invention is evaluated by experts in the perfume industry and perfumers, and the experts consider that: the essential oil of the mosquito-repellent incense extracted by the invention is warm and sweet, caramel, light green and micro herb, has the fragrance type, faint scent type, rose scent type and herb type, has fresh, natural and powerful whole fragrance, and is a novel fragrant raw material in daily chemical blending. The invention has simple process and equipment, less investment, no waste of raw materials, low cost, good quality and high yield of the essential oil, and the yield of the essential oil can reach 0.40 percent.
Description
Technical Field
The invention relates to the technical field of processing of Filipendula esculenta, and particularly relates to a method for extracting Filipendula esculenta essential oil.
Background
Filipendula officinalis is a perennial herb of the genus Filipendula of the family Rosaceae (Rosaceae), and is commonly grown in hillsides, riverside wetlands, meadows and forest edges. The height is 1-1.4 m. The rootstock is thick and strong, and the rootstock is horizontal and has more fibrous roots. Upright diameter, thick, thin edge, smooth, tan. Leaf intergrowth, pinnate compound leaf or discontinuous pinnate compound leaf; the basal leaves and the lower cauline leaves have long stems; the leaf quality is thick; the small leaves at the top end are extra large, the palm shape is 7-9 deep cracks, and the length is 8-13 cm. The width of the leaf is 12-15 cm, the split piece is in a shape of a wide needle or a long round needle, the tip of the leaf is gradually sharp or long and gradually sharp, and irregular and thick sawteeth are arranged at the edge of the leaf. The upper side is green, the lower side is dense white villi, and veins are convex; a pair of lobules are lateral, often with 3 cleft; big leaf, half heart, chamber-shaped, coniform, big; small and most flowers; calyx 4 is fissured; petals 5, white, round or nearly round, 3 mm long; stamens are numerous and longer than petals; 6-8 of carpel. The lean fruit has a handle, a half moon shape, and eyelashes, flower pillars and calyx at the edge for storing. The calyx is reversely broken, the flowering phase is 6-7 months, and the fruit phase is 7-9 months. Growing in hilly grassland, riverside wetlands, meadows and forest edges. Distributed in northeast, northeast China, Korea, northern Japan, Mongolia, Siberian Su-Union and the far east.
Since the mosquitos are fragrant and pleasant in flowering phase and form a strong and elegant fragrance which integrates the effects of freshness, freshness and sweetness, the mosquitos are widely used in spice processing.
At present, the oil yield of the essential oil of the dropwort extracted by adopting the traditional essential oil extraction method is about 0.3 percent, the oil yield is lower, the raw materials are seriously wasted, and the cost is increased.
Disclosure of Invention
The invention provides a method for extracting essential oil of Filipendula ulmaria, aiming at solving the problem of low oil yield of the existing method for extracting essential oil of Filipendula ulmaria.
The technical scheme adopted by the invention for solving the technical problem is as follows:
the invention relates to a method for extracting essential oil of Filipendula ulmaria, which comprises the following steps:
step one, raw material pretreatment
When 70% of flowers of the Filipendula esculenta are open in 6-7 months, harvesting the Filipendula esculenta raw material, and removing withered leaves and thick stalks on the lower part;
step two, canning
Weighing raw materials, putting into a distillation kettle, uniformly and uniformly charging, compacting the periphery, and matching leaves and stems in a staggered manner; tightly sealing the tank opening, checking whether a gas leakage place exists or not, and closing a sewage discharge valve;
step three, distillation
(1) Setting the pressure of a steam boiler to be 0.2-0.35 MPa, introducing steam into the distillation kettle, and opening an air release valve to carry out distillation;
(2) opening a cooling water valve of the condenser, introducing cooling water into the condenser, controlling the temperature of the cooling water to be 10-30 ℃, controlling the consumption of the cooling water to be 1.0T/h, adjusting an air release valve of the distillation kettle, keeping the temperature of a cooling water outlet at 30-40 ℃, and keeping the temperature of distilled water at 30-40 ℃;
(3) controlling the steam speed to enable the oil-water mixture to flow out, and distilling for 2-2.5 hours;
step three, separation and refining
And (3) connecting two oil-water separators in series by adopting a two-stage separation mode, prolonging the retention time of the essential oil to completely separate the oil from the water, taking out the essential oil floating on the upper layer, drying and filtering to obtain the essential oil of the dropwort.
In the preferred embodiment, in the third step, the pressure of the steam boiler is set to 0.25 MPa.
In a preferred embodiment, the temperature of the cooling water is controlled to be 20 ℃ in the third step.
In a preferred embodiment, in step three, the condenser leaving water temperature is maintained at 35 ℃.
In a preferred embodiment, the temperature of the distilled water in step three is maintained at 40 ℃.
The invention has the beneficial effects that: the invention adopts the pressurized steam distillation technology to extract the essential oil of the dropwort, researches the extraction technology of the essential oil of the dropwort, researches the influence of the steam pressure, the distillation time, the separation mode (dissolved part in water), the refining of the essential oil, the content measurement of the essential oil at different parts, the recovery time of the dropwort and other aspects on the oil yield, carries out the evaluation and the application test of the fragrance of the obtained product, and provides a scientific basis for guiding the production.
The mosquito-repellent incense essential oil obtained by the invention is evaluated by experts in the perfume industry and perfumers, and the experts consider that: the essential oil of the mosquito-repellent incense extracted by the invention is warm and sweet, caramel, light green and micro herb, has the fragrance type, faint scent type, rose scent type and herb type, has fresh, natural and powerful whole fragrance, and is a novel fragrant raw material in daily chemical blending.
The invention adopts the pressurized steam distillation technology to extract the essential oil of the dropwort, has simple process and equipment, less investment, no waste of raw materials, low cost, good quality of the essential oil and high yield, and the yield of the essential oil can reach 0.40 percent.
Drawings
FIG. 1 is a flow chart of the method for extracting essential oil from Filipendula ulmaria according to the present invention.
Detailed Description
As shown in fig. 1, the method for extracting essential oil from Filipendula ulmaria of the present invention is specifically realized by the following steps:
step one, raw material pretreatment
And (4) harvesting the mosquito raw material when 70% of flowers of the mosquito are open in 6-7 months, and removing withered leaves and thick stalks at the lower part.
Step two, canning
(1) The raw materials are filled into a distillation kettle (hereinafter referred to as a pot for short), the materials are required to be uniformly filled, the periphery of the materials is compacted, and leaves and stems are matched in a staggered manner, so that the ventilation is facilitated;
(2) tightly sealing the tank opening, checking whether a gas leakage place exists or not, and closing a sewage discharge valve;
step three, distillation
(1) Setting the pressure of a steam boiler to be 0.2-0.35 MPa, opening a steam valve of the steam boiler, introducing steam into a distillation kettle, and opening an air release valve to carry out distillation;
(2) opening a cooling water valve of the condenser, and introducing cooling water into the condenser, wherein the temperature of the cooling water is controlled to be about 10-30 ℃, and the using amount of the cooling water is 1.0T/h; adjusting a gas release valve of the distillation kettle to keep the temperature of the outlet water of the condenser at about 30-40 ℃, and keeping the temperature of the distilled water at 30-40 ℃;
(3) controlling the steam speed of the steam outlet to enable the oil-water mixture to flow out as soon as possible, and distilling for 2-2.5 hours;
step three, separation and refining
In order to ensure that the separation is more complete, a two-stage separation mode is adopted, two oil-water separators are connected in series, the retention time of essential oil is prolonged, the oil and the water are completely separated, and the essential oil floating on the upper layer is taken out for drying and filtering to obtain the essential oil of the dropwort.
Example 1 determination of optimum test conditions
Production equipment
(1) A distillation kettle (made of stainless steel and having an effective volume of 2.5 cubic meters);
(2) a condenser (aluminum coil, cooling area 2.5 cubic meters);
(3) a steam boiler (0.5T/h);
(4) an oil-water separator (made of galvanized iron plate);
(5) a dryer (made of a 50 liter enamel barrel);
(6) various connecting pipe fittings.
Second, the experimental contents
Opening a charging hole at the upper part of the distillation kettle, charging the raw materials into the distillation kettle, sealing after uniformly treading, opening a steam valve, opening a water valve of a condenser when a pressure gauge on the kettle reaches a specified pressure, and slowly opening a steam outlet valve at the upper part. At the moment, oil is taken from a measuring cylinder on the oil-water separator at intervals, and the oil rate is calculated according to the weight. And discharging residual water at the bottom of the kettle after the distillation is finished, opening a discharge port, taking out residues and pushing the residues to a waste storage yard.
(1) Influence of distillation pressure and time on oil yield
According to years of experience, the extraction pressure of herbal essential oil is an important link influencing the aroma quality of the essential oil, the essential oil with overhigh pressure has burnt smell, and the key for extracting the essential oil is to control the steam pressure. The whole grass of the overground part of the mosquito grass harvested in the late bud stage is selected according to the operation conditions for canning and extracting. Distillation tests were performed under different pressure conditions and essential oil extraction was performed for set time periods (see table 1).
TABLE 1
As can be seen from the data in Table 1, when the distillation time is the same, the yield of the essential oil increases by increasing the distillation pressure, and when the distillation pressure is 0.1 to 0.2MPa, the yield is 0.43% at the highest, but when the aroma comparison shows that the aroma of the essential oil has a scorched smell, the distillation pressure is considered to be 0.1 to 0.2MPa, which is not preferable. By comparing the essential oil obtained at normal pressure with the essential oil obtained at a pressure of 0.05MPa, there was no difference in the aroma, and the yield at 0.40% was also satisfactory. When the essential oil is distilled for 2 hours, it is preferable that the distillation time is 2 to 2.5 hours when 90% or more of the essential oil is distilled out.
(2) Determination of essential oil content at different parts
1) Purpose of the experiment: the content of essential oil at different parts is determined by tests.
2) The experimental method comprises the following steps: four growth stages are designed, and volatile oil extraction is respectively carried out.
3) The experimental contents are as follows: selecting mosquito leaves, flowers, stems and whole plants to respectively extract volatile oil.
4) The results are shown in Table 2.
TABLE 2 yield table of essential oil content in different parts
As can be seen from the comparison of the data in Table 2, the essential oil content is highest in flower, second in leaf and lowest in stem. Therefore, during extraction, part of thick stems can be removed, so that the content of essential oil is increased, and the economic benefit is improved.
(3) Determination of harvesting time
1) Purpose of the experiment: the best recovery time is determined through experiments, and the highest extraction yield is obtained.
2) The experimental method comprises the following steps: three growth stages are designed, and volatile oil extraction is respectively carried out.
3) The experimental contents are as follows: the growth stages are divided as follows: early flowering, flowering and fruit stage.
4) The results are shown in Table 3.
TABLE 3 test of essential oil content at different harvesting periods
As can be seen from the data in table 3, the yield of essential oil extracted at the flowering phase was the highest at the time of harvest, and therefore, mosquito grass feedstock was best harvested at the flowering phase.
Example 2 extraction of essential oil of Filipendula moschata
Step one, raw material pretreatment
When 70% of flowers of the Filipendula esculenta are open in 6-7 months, harvesting the Filipendula esculenta raw material, and removing withered leaves and thick stalks on the lower part;
step two, canning
(1) 380kg of the Filipendula ulmaria raw material is weighed and filled into a distillation kettle (hereinafter referred to as a pot for short), the filling is required to be uniform, the periphery is compacted, and leaves and stems are matched in a staggered manner, so that the ventilation is facilitated;
(2) tightly sealing the tank opening, checking whether a gas leakage place exists or not, and closing a sewage discharge valve;
step three, distillation
(1) Setting the pressure of a steam boiler to be 0.2MPa, opening a steam valve of the steam boiler, introducing steam into a distillation kettle, controlling the steam pressure to be about 0.05MPa, and opening a vent valve to perform distillation when the pressure reaches 0.03 MPa;
(2) opening a cooling water valve of the condenser, and introducing cooling water into the condenser, wherein the temperature of the cooling water is controlled to be about 20 ℃, and the consumption of the cooling water is 1.0T/h; adjusting a vent valve of the distillation kettle to keep the temperature of the outlet water of the condenser at about 35 ℃ and the temperature of the distilled water at 40 ℃;
(3) controlling the steam speed of the steam outlet to enable the oil-water mixture to flow out as soon as possible, and distilling for 2 hours;
step three, separation and refining
In order to ensure that the separation is more complete, a two-stage separation mode is adopted, two oil-water separators are connected in series, the retention time of essential oil is prolonged, the oil and the water are completely separated, and the essential oil floating on the upper layer is taken out for drying and filtering to obtain the essential oil of the dropwort.
Example 3 extraction of essential oil of Filipendula vulgaris
Step one, raw material pretreatment
When 70% of flowers of the Filipendula esculenta are open in 6-7 months, harvesting the Filipendula esculenta raw material, and removing withered leaves and thick stalks on the lower part;
step two, canning
(1) Weighing 380kg of raw materials, filling the raw materials into a distillation kettle (hereinafter referred to as a pot for short), wherein the raw materials are required to be uniformly filled, the periphery of the raw materials is compacted, and leaves and stems are matched in a staggered manner, so that the ventilation is facilitated;
(2) tightly sealing the tank opening, checking whether a gas leakage place exists or not, and closing a sewage discharge valve;
step three, distillation
(1) Setting the pressure of a steam boiler to be 0.25MPa, opening a steam valve of the steam boiler, introducing steam into a distillation kettle, controlling the steam pressure to be about 0.1MPa, and opening a vent valve to perform distillation when the pressure reaches 0.05 MPa;
(2) opening a cooling water valve of the condenser, and introducing cooling water into the condenser, wherein the temperature of the cooling water is controlled to be about 20 ℃, and the consumption of the cooling water is 1.0T/h; adjusting a vent valve of the distillation kettle to keep the temperature of the outlet water of the condenser at about 35 ℃ and the temperature of the distilled water at 40 ℃;
(3) controlling the steam speed of the steam outlet to enable the oil-water mixture to flow out as soon as possible, and distilling for 2.3 hours;
step three, separation and refining
In order to ensure that the separation is more complete, a two-stage separation mode is adopted, two oil-water separators are connected in series, the retention time of essential oil is prolonged, the oil and the water are completely separated, and the essential oil floating on the upper layer is taken out for drying and filtering to obtain the essential oil of the dropwort.
Example 4 extraction of essential oil of Filipendula vulgaris
Step one, raw material pretreatment
When 70% of flowers of the Filipendula esculenta are open in 6-7 months, harvesting the Filipendula esculenta raw material, and removing withered leaves and thick stalks on the lower part;
step two, canning
(1) Weighing 380kg of raw materials, filling the raw materials into a distillation kettle (hereinafter referred to as a pot for short), wherein the raw materials are required to be uniformly filled, the periphery of the raw materials is compacted, and leaves and stems are matched in a staggered manner, so that the ventilation is facilitated;
(2) tightly sealing the tank opening, checking whether a gas leakage place exists or not, and closing a sewage discharge valve;
step three, distillation
(1) Setting the pressure of a steam boiler to be 0.35MPa, opening a steam valve of the steam boiler, introducing steam into a distillation kettle, controlling the steam pressure to be about 0.2MPa, and opening a vent valve to perform distillation when the pressure reaches 0.15 MPa;
(2) opening a cooling water valve of the condenser, and introducing cooling water into the condenser, wherein the temperature of the cooling water is controlled to be about 20 ℃, and the consumption of the cooling water is 1.0T/h; adjusting a vent valve of the distillation kettle to keep the temperature of the outlet water of the condenser at about 35 ℃ and the temperature of the distilled water at 40 ℃;
(3) controlling the steam speed at the steam outlet to enable the oil-water mixture to flow out as soon as possible, and distilling for 2.5 hours;
step three, separation and refining
In order to ensure that the separation is more complete, a two-stage separation mode is adopted, two oil-water separators are connected in series, the retention time of essential oil is prolonged, the oil and the water are completely separated, and the essential oil floating on the upper layer is taken out for drying and filtering to obtain the essential oil of the dropwort.
The oil yields of examples 2-4 were counted and the results are shown in Table 4.
TABLE 4
| Item | Oil yield (%) |
| Example 2 | 0.4 |
| Example 3 | 0.42 |
| Example 4 | 0.43 |
| Comparative example (existing extraction method) | 0.3 |
As can be seen from the data in the table, the essential oil of Filipendula esculenta is extracted by the extraction method, and the oil yield is as follows: 0.4 percent.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (1)
1. The method for extracting the essential oil of the Filipendula ulmaria is characterized by comprising the following steps of:
step one, raw material pretreatment
When 70% of flowers of the Filipendula esculenta are open in 6-7 months, harvesting the Filipendula esculenta raw material, and removing withered leaves and thick stalks on the lower part;
step two, canning
Weighing raw materials, putting into a distillation kettle, uniformly and uniformly charging, compacting the periphery, and matching leaves and stems in a staggered manner; tightly sealing the tank opening, checking whether a gas leakage place exists or not, and closing a sewage discharge valve;
step three, distillation
(1) Setting the pressure of a steam boiler to be 0.25MPa, introducing steam into the distillation kettle, and opening an air release valve to carry out distillation;
(2) opening a cooling water valve of the condenser, introducing cooling water into the condenser, controlling the temperature of the cooling water to be 20 ℃, controlling the consumption of the cooling water to be 1.0T/h, and adjusting a vent valve of the distillation kettle to keep the temperature of outlet water of the condenser to be 35 ℃ and the temperature of distillate water to be 40 ℃;
(3) controlling the steam speed to enable the oil-water mixture to flow out, and distilling for 2-2.5 hours;
step three, separation and refining
And (3) connecting two oil-water separators in series by adopting a two-stage separation mode, prolonging the retention time of the essential oil to completely separate the oil from the water, taking out the essential oil floating on the upper layer, drying and filtering to obtain the essential oil of the dropwort.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103387879A (en) * | 2013-08-13 | 2013-11-13 | 甘肃省检验检疫科学技术研究院 | Distillation equipment of rose essential oil and preparation method of rose essential oil |
| CN105647646A (en) * | 2015-12-30 | 2016-06-08 | 安徽银丰药业股份有限公司 | Mint leaf extraction technology |
| CN106350230A (en) * | 2016-12-05 | 2017-01-25 | 永州山香香料有限公司 | Litsea cubeba oil distillation separation equipment and technology |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103387879A (en) * | 2013-08-13 | 2013-11-13 | 甘肃省检验检疫科学技术研究院 | Distillation equipment of rose essential oil and preparation method of rose essential oil |
| CN105647646A (en) * | 2015-12-30 | 2016-06-08 | 安徽银丰药业股份有限公司 | Mint leaf extraction technology |
| CN106350230A (en) * | 2016-12-05 | 2017-01-25 | 永州山香香料有限公司 | Litsea cubeba oil distillation separation equipment and technology |
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Effective date of registration: 20221118 Address after: 134300 Room 201, Unit 4, 246-36, Hongqi Street, Hunjiang District, Baishan City, Jilin Province Patentee after: Baishan Heitu Agricultural Technology Co.,Ltd. Address before: 134300 No.228, Hunjiang street, Hunjiang District, Baishan City, Jilin Province Patentee before: BAISHAN SCIENCE AND TECHNOLOGY Research Institute |