CN108504460A - A kind of extracting method of palmate meadowsweet essential oil - Google Patents
A kind of extracting method of palmate meadowsweet essential oil Download PDFInfo
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- CN108504460A CN108504460A CN201810586548.7A CN201810586548A CN108504460A CN 108504460 A CN108504460 A CN 108504460A CN 201810586548 A CN201810586548 A CN 201810586548A CN 108504460 A CN108504460 A CN 108504460A
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- essential oil
- palmate meadowsweet
- palmate
- meadowsweet
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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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- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Fats And Perfumes (AREA)
Abstract
A kind of extracting method of palmate meadowsweet essential oil, is related to palmate meadowsweet manufacture field, solves the problems, such as that oil yield existing for the extracting method of existing palmate meadowsweet essential oil is low.The present invention includes：Pretreatment of raw material；Tinning；Distillation；Separation refines；Using the second-order separation mode, two oil water separators are together in series, extends the essential oil residence time, You Heshui is made to be kept completely separate, the essential oil that taking-up swims in upper layer is dried, filters to get palmate meadowsweet essential oil.Gained palmate meadowsweet essential oil of the invention through fragrance industry expert and perfumer carries out that perfume (or spice), expert is commented to think：The palmate meadowsweet essential oil that the present invention is extracted warms up sweet tea, caramel, micro- green, micro- medicinal herbs, has vanilla type, delicate fragrance type, rose scent, medicinal herbs type, entire fragrance is pure and fresh, naturally strong, is a novel perfume material in daily use chemicals blending.Present invention process and equipment is simple, small investment, does not waste raw material, at low cost, essential oil is high-quality and yield is high, and essential oil yield can reach 0.40%.
Description
Technical field
The present invention relates to palmate meadowsweet processing technique fields, and in particular to a kind of extracting method of palmate meadowsweet essential oil.
Background technology
Palmate meadowsweet is the rose family (Rosaceae) palmate meadowsweet category (Filipendula) herbaceos perennial, is grown on more
Hillside, riparian wetland, grassy marshland and border.It is 1~1.4 meter high.Rhizome is sturdy, it is horizontal walk, fibrous root is more.Diameter is upright, sturdy, there is thin rib,
Smoothly, sepia.Leaf alternate, pinnate compound leaf or be intermittent pinnate compound leaf；Basal leaf and lower part stem leaf have long handle；The food value of leaf
It is thick；Top leaflet is especially big, 7~9 drastic crack of palmate, 8~13 centimetres long.12~15 centimetres wide, the wide lanceolar of sliver or long round shape are draped over one's shoulders
Aciculiform, apex is tapering or length is tapering, and leaf margin has irregular rough sawn tooth.It is green above, below dense white fluff, vein protrusion；
A pair of of leaflet of side life, normal 3 split；Stipule is big, and half is heart-shaped, umbrella room shape panicle, basidixed, greatly；Spend small, majority；4 fissure of calyx；Flower
Valve 5, white, round or subcircular are 3 millimeters long；Stamen is most, longer than petal；Carpel 6~8.Achene has handle, semilune, edge
Ciliation, style and persistent calyx.Calyx reflexed, 6~July of florescence, 7~September of fruiting period.It is born in patana, riparian wetland, grass
Pasture and border.It is distributed in Northeast China, North China, Korea, Japan is northern, Mongolia, Soviet Union Siberia and the Far East Area.
Since palmate meadowsweet florescence fragrance is pleasant, the strong quiet and tastefully laid out fragrance being integrated with clear, fresh, sweet tea, therefore mosquito are constituted
Sub- grass is widely used in fragrance processing.
Currently, the palmate meadowsweet essential oil oil yield extracted using traditional method of extraction of essential oil is about 0.3%, oil yield compared with
Low, serious waste raw material, cost increases.
Invention content
In order to solve the problems, such as that oil yield existing for the extracting method of existing palmate meadowsweet essential oil is low, the present invention provides a kind of mosquito
The extracting method of sub- grass essential oil.
The present invention is that technical scheme applied to solve the technical problem is as follows：
A kind of extracting method of palmate meadowsweet essential oil of the present invention, includes the following steps：
Step 1: pretreatment of raw material
6~July when the flower of palmate meadowsweet has 70% opening, gathers in palmate meadowsweet raw material, removes lower part and withers leaf and coarse
Stalk；
Step 2: tinning
It weighs raw material to be packed into distillation still, it is desirable that charging uniformity, surrounding compacting, leaf are staggeredly arranged in pairs or groups with stalk；It is tamping
Tank mouth checks whether there is the place of gas leakage, closes blowdown water valve；
Step 3: distillation
(1) it sets steam boiler pressure to 0.2~0.35MPa, steam is passed through into distillation still, open vent valve, into
Row distillation；
(2) condenser cooling water valve to be opened, cooling water is passed through into condenser, cooling water temperature is controlled at 10~30 DEG C,
Cooling water amount is 1.0T/h, adjusts distillation still vent valve, so that cooling water outlet temperature is maintained at 30~40 DEG C, distillate coolant-temperature gage
It is maintained at 30~40 DEG C；
(3) vapor (steam) velocity is controlled so that oil water mixture flows out, and distills 2~2.5 hours；
Step 3: detaching, being refined
Using the second-order separation mode, two oil water separators are together in series, extends the essential oil residence time, keeps You Heshui complete
Fully separating, the essential oil that taking-up swims in upper layer is dried, filters to get palmate meadowsweet essential oil.
As preferred embodiment, in step 3, the pressure of steam boiler is set as 0.25MPa.
As preferred embodiment, in step 3, cooling water temperature is controlled at 20 DEG C.
As preferred embodiment, in step 3, leaving condenser water temperature is maintained at 35 DEG C.
As preferred embodiment, in step 3, distillates coolant-temperature gage and be maintained at 40 DEG C.
The beneficial effects of the invention are as follows：The present invention extracts palmate meadowsweet essential oil using compressed steam distillation technique, to mosquito
The extraction process of careless essential oil is studied, its steam pressure, distillation time, separate mode (part is dissolved in water), essence are studied
The influence of oil refining, different parts essential oil content measurement, palmate meadowsweet collecting time etc. to oil yield, carries out products obtained therefrom
Comment it is fragrant identify and application test, for Instructing manufacture provide scientific basis.
Gained palmate meadowsweet essential oil of the invention through fragrance industry expert and perfumer carries out that perfume (or spice), expert is commented to think：Institute of the present invention
The palmate meadowsweet essential oil of extraction warms up sweet tea, caramel, micro- green, micro- medicinal herbs, has a vanilla type, delicate fragrance type, rose scent, medicinal herbs type, entirely
Fragrance is pure and fresh, naturally strong, is a novel perfume material in daily use chemicals blending.
The present invention extracts palmate meadowsweet essential oil using compressed steam distillation technique, and technique and equipment is simple, small investment, not unrestrained
Take raw material, at low cost, essential oil is high-quality and yield is high, and essential oil yield can reach 0.40%.
Description of the drawings
Fig. 1 is a kind of flow chart of the extracting method of palmate meadowsweet essential oil of the present invention.
Specific implementation mode
As shown in Figure 1, a kind of extracting method of palmate meadowsweet essential oil of the present invention, is realized particular by following steps：
Step 1: pretreatment of raw material
6~July when the flower of palmate meadowsweet has 70% opening, gathers in palmate meadowsweet raw material, removes lower part and withers leaf and coarse
Stalk.
Step 2: tinning
(1) raw material is packed into distillation still (hereinafter referred to as tank), it is desirable that charging uniformity, surrounding compacting, leaf and stalk
It staggeredly arranges in pairs or groups, is conducive to the Liu Chang that ventilates；
(2) it is tamping tank mouth, checks whether there is the place of gas leakage, closes blowdown water valve；
Step 3: distillation
(1) it sets steam boiler pressure to 0.2~0.35MPa, the steam valve of steam boiler is opened, into distillation still
It is passed through steam, vent valve is opened, is distilled；
(2) condenser cooling water valve is opened, cooling water is passed through into condenser, cooling water temperature controls on 10~30 DEG C of left sides
The right side, cooling water amount 1.0T/h；Distillation still vent valve is adjusted, so that leaving condenser water temperature is maintained at 30~40 DEG C or so, evaporates
Leaving water temperature is maintained at 30~40 DEG C；
(3) venthole vapor (steam) velocity is controlled so that oil water mixture flows out as early as possible, distills 2~2.5 hours；
Step 3: detaching and refining
In order to keep separation more thorough, using the second-order separation mode, two oil water separators are together in series, extend essential oil
Residence time makes You Heshui reach and is kept completely separate, and the essential oil that taking-up swims in upper layer is dried, filters to get palmate meadowsweet essence
Oil.
The determination of 1 optimum test condition of embodiment
One, device therefor is produced
(1) distillation still (stainless steel is made, 2.5 cubic metres of dischargeable capacity)；
(2) condenser (aluminum coiled pipe, 2.5 cubic metres of film-cooled heat)；
(3) steam boiler (0.5T/h)；
(4) oil water separator (galvanized iron sheet is made)；
(5) drier (50 liters of porcelain enamel barrels are made)；
(6) various connecting pipes.
Two, experiment content
Distillation still top charging door is opened, raw material is packed into distillation still, is uniformly sealed after having peace of mind, opens steam valve
Door opens condenser water valve when pressure gauge reaches authorized pressure on kettle, slowly opens top gas outlet valve.At this time every one section
Time by taking oil with graduated cylinder on oil water separator, calculates by weight oil yield.The residual water in bottom is exhausted after distillation, opens discharging
Mouth takes out residue and is pushed into spoil area.
(1) influence of distillation pressure and time to oil yield
According to many years of experience, the extraction pressure of draft class essential oil is to influence the important link of essential oil aroma quality, pressure mistake
High essential oil, which has, is charred smell, and control steam pressure is the key that extraction essential oil.Budding the later stage according to the selection of aforesaid operations condition
The herb of the palmate meadowsweet aerial part of harvesting carries out tinning extraction.Distillation test is carried out under the conditions of different pressures, by setting
Period carries out extraction of essential oil (being shown in Table 1).
Table 1
By the data in table 1 it is found that when distillation time is identical, increase distillation pressure, essential oil yield increased, and work as steaming
Pressure yield highest 0.43% in 0.1~0.2MPa is evaporated, but is compared by fragrance, acquisition essential oil fragrance, which carries, is charred breath,
Then think that distillation pressure is undesirable in 0.1~0.2MPa.The essence that essential oil is obtained with pressure 0.05MPa is obtained by comparing normal pressure
Oil is not different on fragrance, and yield is also to meet desired value 0.40%.Essential oil has steamed 90% when distilling 2 hours
More than, then it is assumed that can be set to distillation time 2~2.5 hours is advisable.
(2) different parts essential oil content measures
1) experiment purpose：Different parts essential oil content is measured by experiment.
2) experimental method：Four growth phases are designed, carry out volatile oil extracting respectively.
3) experiment content：It chooses mosquito blade of grass, flower, stem, complete stool and carries out volatile oil extracting respectively.
4) experimental result is shown in Table 2.
2 different parts yield table containing essential oil of table
Compared by data in table 2 it is found that essential oil content to spend highest, leaf to take second place, stem it is minimum.Thus in extraction,
The coarse cane in part can be removed to increase economic efficiency to improve essential oil content.
(3) determination of collecting time
1) experiment purpose：Best collecting time is determined by testing, and is obtained highest and is extracted yield.
2) experimental method：Three growth phases are designed, carry out volatile oil extracting respectively.
3) experiment content：Dividing growth phase is：It blooms early period, florescence, fruiting period.
4) experimental result is shown in Table 3.
3 Different Harvesting Time essential oil content of table is tested
By the data in table 3 it is found that the collecting time florescence extracts essential oil yield highest, therefore, palmate meadowsweet raw material is best
It is harvested at the florescence.
The extraction of 2 palmate meadowsweet essential oil of embodiment
Step 1: pretreatment of raw material
6~July when the flower of palmate meadowsweet has 70% opening, gathers in palmate meadowsweet raw material, removes lower part and withers leaf and coarse
Stalk；
Step 2: tinning
(1) it weighs 380kg palmate meadowsweet raw materials to be packed into distillation still (hereinafter referred to as tank), it is desirable that charging uniformity, surrounding
Compacting, leaf are staggeredly arranged in pairs or groups with stalk, are conducive to the Liu Chang that ventilates；
(2) it is tamping tank mouth, checks whether there is the place of gas leakage, closes blowdown water valve；
Step 3: distillation
(1) it sets steam boiler pressure to 0.2MPa, opens the steam valve of steam boiler, steaming is passed through into distillation still
Vapour, Steam pressure control is in 0.05MPa or so, after pressure reaches 0.03MPa, you can opens vent valve, is distilled；
(2) condenser cooling water valve to be opened, cooling water is passed through into condenser, cooling water temperature is controlled at 20 DEG C or so,
Cooling water amount is 1.0T/h；Distillation still vent valve is adjusted, so that leaving condenser water temperature is maintained at 35 DEG C or so, distillates coolant-temperature gage
It is maintained at 40 DEG C；
(3) venthole vapor (steam) velocity is controlled so that oil water mixture flows out as early as possible, distills 2 hours；
Step 3: detaching and refining
In order to keep separation more thorough, using the second-order separation mode, two oil water separators are together in series, extend essential oil
Residence time makes You Heshui reach and is kept completely separate, and the essential oil that taking-up swims in upper layer is dried, filters to get palmate meadowsweet essence
Oil.
The extraction of 3 palmate meadowsweet essential oil of embodiment
Step 1: pretreatment of raw material
6~July when the flower of palmate meadowsweet has 70% opening, gathers in palmate meadowsweet raw material, removes lower part and withers leaf and coarse
Stalk；
Step 2: tinning
(1) raw material for weighing 380kg is packed into distillation still (hereinafter referred to as tank), it is desirable that charging uniformity, surrounding compacting,
Leaf is staggeredly arranged in pairs or groups with stalk, is conducive to the Liu Chang that ventilates；
(2) it is tamping tank mouth, checks whether there is the place of gas leakage, closes blowdown water valve；
Step 3: distillation
(1) it sets steam boiler pressure to 0.25MPa, opens the steam valve of steam boiler, be passed through into distillation still
Steam, Steam pressure control is in 0.1MPa or so, after pressure reaches 0.05MPa, you can opens vent valve, is distilled；
(2) condenser cooling water valve to be opened, cooling water is passed through into condenser, cooling water temperature is controlled at 20 DEG C or so,
Cooling water amount is 1.0T/h；Distillation still vent valve is adjusted, so that leaving condenser water temperature is maintained at 35 DEG C or so, distillates coolant-temperature gage
It is maintained at 40 DEG C；
(3) venthole vapor (steam) velocity is controlled so that oil water mixture flows out as early as possible, distills 2.3 hours；
Step 3: detaching and refining
In order to keep separation more thorough, using the second-order separation mode, two oil water separators are together in series, extend essential oil
Residence time makes You Heshui reach and is kept completely separate, and the essential oil that taking-up swims in upper layer is dried, filters to get palmate meadowsweet essence
Oil.
The extraction of 4 palmate meadowsweet essential oil of embodiment
Step 1: pretreatment of raw material
6~July when the flower of palmate meadowsweet has 70% opening, gathers in palmate meadowsweet raw material, removes lower part and withers leaf and coarse
Stalk；
Step 2: tinning
(1) raw material for weighing 380kg is packed into distillation still (hereinafter referred to as tank), it is desirable that charging uniformity, surrounding compacting,
Leaf is staggeredly arranged in pairs or groups with stalk, is conducive to the Liu Chang that ventilates；
(2) it is tamping tank mouth, checks whether there is the place of gas leakage, closes blowdown water valve；
Step 3: distillation
(1) it sets steam boiler pressure to 0.35MPa, opens the steam valve of steam boiler, be passed through into distillation still
Steam, Steam pressure control is in 0.2MPa or so, after pressure reaches 0.15MPa, you can opens vent valve, is distilled；
(2) condenser cooling water valve to be opened, cooling water is passed through into condenser, cooling water temperature is controlled at 20 DEG C or so,
Cooling water amount is 1.0T/h；Distillation still vent valve is adjusted, so that leaving condenser water temperature is maintained at 35 DEG C or so, distillates coolant-temperature gage
It is maintained at 40 DEG C；
(3) venthole vapor (steam) velocity is controlled so that oil water mixture flows out as early as possible, distills 2.5 hours；
Step 3: detaching and refining
In order to keep separation more thorough, using the second-order separation mode, two oil water separators are together in series, extend essential oil
Residence time makes You Heshui reach and is kept completely separate, and the essential oil that taking-up swims in upper layer is dried, filters to get palmate meadowsweet essence
Oil.
The oil yield of embodiment 2-4 is counted, the results are shown in Table 4.
Table 4
| Project | Oil yield (%) |
| Embodiment 2 | 0.4 |
| Embodiment 3 | 0.42 |
| Embodiment 4 | 0.43 |
| Reference examples (existing extracting method) | 0.3 |
By data in table it is found that extracting method through the invention extracts palmate meadowsweet essential oil, oil yield is：
0.4%.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (5)
1. a kind of extracting method of palmate meadowsweet essential oil, which is characterized in that include the following steps：
Step 1: pretreatment of raw material
6~July when the flower of palmate meadowsweet has 70% opening, gathers in palmate meadowsweet raw material, removes the withered leaf in lower part and coarse stalk；
Step 2: tinning
It weighs raw material to be packed into distillation still, it is desirable that charging uniformity, surrounding compacting, leaf are staggeredly arranged in pairs or groups with stalk；Tank mouth is tamping,
The place of gas leakage is checked whether there is, blowdown water valve is closed；
Step 3: distillation
(1) it sets steam boiler pressure to 0.2~0.35MPa, steam is passed through into distillation still, open vent valve, steamed
It evaporates；
(2) condenser cooling water valve is opened, cooling water is passed through into condenser, cooling water temperature is controlled at 10~30 DEG C, cooling
Water consumption is 1.0T/h, adjusts distillation still vent valve, leaving condenser water temperature is made to be maintained at 30~40 DEG C, distillates coolant-temperature gage holding
At 30~40 DEG C；
(3) vapor (steam) velocity is controlled so that oil water mixture flows out, and distills 2~2.5 hours；
Step 3: detaching, being refined
Using the second-order separation mode, two oil water separators are together in series, extend the essential oil residence time, oil and water is made to divide completely
From the essential oil that taking-up swims in upper layer is dried, filters to get palmate meadowsweet essential oil.
2. a kind of extracting method of palmate meadowsweet essential oil according to claim 1, which is characterized in that in step 3, steam copper
The pressure of stove is set as 0.25MPa.
3. a kind of extracting method of palmate meadowsweet essential oil according to claim 1, which is characterized in that in step 3, cooling water
Temperature is controlled at 20 DEG C.
4. a kind of extracting method of palmate meadowsweet essential oil according to claim 1, which is characterized in that in step 3, condenser
Leaving water temperature is maintained at 35 DEG C.
5. a kind of extracting method of palmate meadowsweet essential oil according to claim 1, which is characterized in that in step 3, distillate water
Temperature is maintained at 40 DEG C.
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| CN201810586548.7A CN108504460B (en) | 2018-06-08 | 2018-06-08 | Method for extracting essential oil of Filipendula ulmaria |
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| CN201810586548.7A CN108504460B (en) | 2018-06-08 | 2018-06-08 | Method for extracting essential oil of Filipendula ulmaria |
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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 |
-
2018
- 2018-06-08 CN CN201810586548.7A patent/CN108504460B/en active Active
Patent 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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