CN109554229A - A kind of method of extraction of essential oil and device of high-content linalool - Google Patents
A kind of method of extraction of essential oil and device of high-content linalool Download PDFInfo
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- CN109554229A CN109554229A CN201811374054.9A CN201811374054A CN109554229A CN 109554229 A CN109554229 A CN 109554229A CN 201811374054 A CN201811374054 A CN 201811374054A CN 109554229 A CN109554229 A CN 109554229A
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Classifications
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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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- 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
Abstract
The present invention provides a kind of method of extraction of essential oil of high-content linalool, include the following steps: that (1) will distill in the distillation section in linalool type Huang camphor tree, fragrant camphor tree leaf and water adding apparatus, vapo(u)rizing temperature is 100 DEG C, the vapor of distillation is introduced into leaf, it mixes the essential oil steam of leaf material with vapor, obtains oil mixing with water air-flow；(2) oil mixing with water air-flow is condensed through multi-reflow, the essential oil component of liquid that is collecting different batches and being separated from water, collects essential oil component, stops heating.The present invention also provides a kind of for extracting the essential oil extracting device of high-content linalool.
Description
Technical field
The invention belongs to technical field of fine, and in particular to a kind of method of extraction of essential oil of high-content linalool and
Device.
Background technique
Linalool (Linalool) also known as linalool, molecular formula C10H18O is colourless liquid, is monoterpenes compound, has
Similar to the lily of the valley or lily floral scent.Main chemical compositions are left-handed linalool in fragrant camphor tree essential oil, in linalool type Huang camphor tree essential oil
Main chemical compositions are dextrorotation linalool.Natural linalool is generally by extraction by steam distillation Huang camphor tree, fragrant camphor tree leaf essential oil
It is made, and the height of the percentage contents of natural linalool is to determine the most important factor of essential oil quality in essential oil.With current
Linalool percentage contents are every from the point of view of the market price, in essential oil increases by 1%, and the market price per ton increase accordingly 2000 yuan.
Therefore, the essential oil for obtaining high-content linalool is particularly critical.
Yellow camphor tree, camphor tree branches and leaves are usually placed in distillation still, with certain material ratio by the preparation method of natural linalool
It is heated after water is added, after heating generation vapor directs or through control certain pressure, will be rich in leaf oil cell
Essential oil steam, and obtain essential oil by condensation, after water-oil separating.
In the extracting method of the existing essential oil containing linalool, reflux ratio when discharging will not be controlled, it is primary only with essential oil
Property the method collected, the content of linalool is lower in gained essential oil.
Summary of the invention
The present invention is intended to provide a kind of method of extraction of essential oil of high-content linalool, was extracted by changing steam distillation
Discharging time, discharging speed in journey, discharging reflux ratio extract the yellow camphor tree of high-content linalool, fragrant chapter essential oil.
Another object of the present invention be provide it is a kind of for extracting the extraction element of the essential oil of high-content linalool, by this
Device can control discharging reflux ratio, to obtain the essential oil containing high-content linalool.
Technical scheme is as follows:
A kind of method of extraction of essential oil of high-content linalool, includes the following steps:
(1) it will be distilled in the distillation container in linalool type Huang camphor tree, fragrant camphor tree leaf and water adding apparatus, vapo(u)rizing temperature 100
DEG C, the vapor of distillation is introduced into leaf, mixes the essential oil steam of leaf material with vapor, obtains oil mixing with water air-flow；
(2) oil mixing with water air-flow is condensed through the reflux component multi-reflow of device, obtain different batches and with moisture
From liquid essential oil component, and through essential oil collection vessel collect essential oil component, stop heating.
Further, in the method for extraction of essential oil of the high-content linalool, the linalool type being added in step (1) is yellow
The mass ratio of camphor tree, fragrant camphor tree leaf and water is 1: 4-1: 20.
Further, in the method for extraction of essential oil of the high-content linalool, linalool type Huang camphor tree described in step (1),
Fragrant camphor tree leaf be selected from fresh picking and removed shredded or be crushed to broken leaf after blade surface impurity can be by the fresh of 40-60 mesh
The leaf that leaf or the fresh leaf of fresh picking are weighed immediately after removal surface impurity and moisture, and are sealed under low temperature
Material.
Further, reflux condensation mode and collection in the method for extraction of essential oil of the high-content linalool, in step (2)
Process includes the following steps；
(1) when the oil reservoir that the component that flows back begins with liquid occurs and oil reservoir can be collected container collection, reflux portion is controlled
The discharging reflux ratio of part is within the scope of 0%-50%, reflux cycle divides the essence of 1-3 batch collection liquid within the scope of 10-60s
Oil ingredient, until the ratio between the linalool type Huang camphor tree of total reservoir volume and addition containing linalool, fragrant camphor tree leaf gross mass exists
When in 0.3%-1.0% (mL/g) range, first time essential oil component is obtained；
(2) control again reflux component discharging reflux ratio within the scope of 50-80%, reflux cycle within the scope of 10-40s,
And 1-3 batch is divided to collect essential oil component, until the linalool type Huang camphor tree of total reservoir volume and addition containing linalool, the total matter of fragrant camphor tree leaf
When ratio between amount is in 0.5%-1.8% (mL/g) range, second of essential oil component is obtained；
(3) continue the discharging reflux ratio of control reflux component within the scope of 80%-90%, reflux cycle is in 10-60s range
It is interior, essential oil component is collected, until can stop heating when the essential oil volume steamed no longer changes, obtains third time essential oil component.
Each essential oil component that the present invention obtains can carry out further component point by measurements such as GC, GC-MS, optical activities
Class.
The present invention also provides a kind of essential oil extracting device of high-content linalool, which includes for grease mixed airflow
The reflux component of reflux, and can be received with the distillation section of the essential oil steam of an initiation leaf material of reflux component connection, one respectively
The collecting part of oil liquid after collection reflux.
Specifically, essential oil extracting device of the invention includes a distillation section, reflux component and essential oil collecting part, is steamed
Evaporating component includes cucurbit and distillation cascade, and the periphery of cucurbit is equipped with a heating device, and cucurbit is equipped with material mouth, the mouth of a river,
Top is equipped with gas outlet, gas outlet and distillation cascade one end connection, and the return pipe a in the distillation cascade other end and the reflux component joins
Logical, the reflux component includes return pipe a and return pipe b, and the upper and lower part on the side wall of return pipe a is respectively equipped with branch mouth a
With branch mouth b, branch mouth a and branch mouth b are joined by the steam port a and steam port b that are equipped on the pipeline and return pipe b that valve controls respectively
Logical, the periphery on the top return pipe b is arranged with condenser pipe, the upper and lower part of condenser pipe side wall extend through equipped with hydrothermal solution outlet and
Cold liquid inlet extends through above and below the side wall of the lower part return pipe b equipped with steam port a, steam port b, is located at return pipe b
Interior and be located between steam port a and condensation bottom of the tube and be equipped with a reflux ratio controller, the bottom end of return pipe b is equipped with oil outlet, out
The receiving flask connection of hydraulic fluid port lower part and the collecting part, the collecting part include a receiving flask.
Further, in the essential oil extracting device of the high-content linalool, the top opening of the return pipe a of the reflux component
Portion is equipped with a temperature detector.
Further, in the essential oil extracting device of the high-content linalool, the distillation bottom of the tube in the distillation section
Inside be equipped with net-like spacer.
Further, in the essential oil extracting device of the high-content linalool, the collecting part further includes one and collection
The essential oil volume measurement device of bottle and oil outlet difference connection.
The present invention is compared to the existing method of extraction of essential oil containing linalool, the beneficial effect is that:
1, the first time that the method for the present invention obtains, the content of the linalool in second of essential oil component are higher, more traditional work
0.5%-8.0% is higher by under skill and appointed condition
2, the linalool essential oil for the principal component higher amount that the method for the present invention obtains, essential oil quality more preferably, can be reduced subsequent
Principal component purifying process advantageously reduces the post processing costs such as rectifying, distillation.
3, extraction element provided by the invention, the linalool essential oil suitable for extraction by steam distillation high-content.
Detailed description of the invention
Fig. 1 is the structural schematic diagram of the essential oil extracting device of embodiment 1, wherein 1 cucurbit, 2 distillation cascades, and 3 mouth b, 4
Return pipe a, 5 mouth b, 6 heating devices, 7 temperature detectors, 8 cold liquid inlets, 9 steam port a, 10 return pipe b, 11 steam port b,
12 condenser pipes, the outlet of 13 hydrothermal solutions, 14 reflux ratio controllers, 15 oil outlets, 16 receiving flasks.
Fig. 2 is the structural schematic diagram of the essential oil extracting device of comparative example 1, wherein 1 heating device, 2 cucurbits, 3 reflux
Pipe, 4 receiving flasks.
Specific embodiment
The contents of the present invention are further described by the following examples.
1 essential oil extracting device of embodiment
As shown in Figure 1, building essential oil extracting device, wherein the device includes a distillation section, reflux component and essential oil
Collecting part, distillation section include cucurbit 1 and distillation cascade 2, and the periphery of cucurbit 1 is equipped with a heating device 6, cucurbit 1
Be equipped with material mouth, the mouth of a river, top is equipped with gas outlet, gas outlet and 2 one end connection of distillation cascade, 2 other end of distillation cascade with described time
The inside of return pipe a4 connection in stream unit, 2 bottom of distillation cascade is equipped with net-like spacer, for blocking the fresh leaf on distillation cascade 2
It falls into cucurbit 1；The reflux component includes return pipe a4 and return pipe b10, and the top opening portion of return pipe a4 is equipped with a temperature
Detector 15, for the vapo(u)rizing temperature during Detection and Extraction；Upper and lower part on the side wall of return pipe a4 is respectively equipped with branch
Mouth a5 and branch mouth b3, branch mouth a5 and branch mouth b3 pass through the pipeline for being equipped with valve control and the steam port a9 on return pipe b10 respectively
With steam port b11 connection, the upper periphery of return pipe b10 is arranged with condenser pipe 12, the upper and lower part point of 12 side wall of condenser pipe
Not She You hydrothermal solution outlet 9 and cold liquid inlet 8, the side wall of the lower part return pipe b10 is equipped with steam port a9, steam port b11, is located at
A reflux ratio controller 14, the bottom end return pipe b10 are equipped in return pipe b10 and between 12 bottom steam port a9 and condenser pipe
Equipped with oil outlet 15, oil outlet lower part 13 and essential oil volume measurement device import connection, essential oil volume measurement device exports and institute
16 connection of receiving flask of collecting part is stated, the collecting part includes a receiving flask 13.
The aqueous vapor generated after heating cucurbit 1 enters the leaf material in distillation cascade 2, so that the essential oil steam and vapor of leaf material
It is mixed into mixed vapour air-flow, and enters return pipe a4, cold liquid inlet 8 and the hydrothermal solution outlet 9 of return pipe b10 is followed for being passed through
The cooling water of ring passes through the valve on the pipeline of the steam port a9 connection on the branch mouth a5 and return pipe b10 on control return pipe a4
Valve on the pipeline of the steam port b11 connection on branch mouth b3 and return pipe b10 on door, return pipe a4, so that constantly generating
Mixed vapour air-flow circulation is realized in the condenser pipe 12 in return pipe a4 and return pipe b10, by control oil outlet on
Reflux ratio controller 15, the reflux ratio of control device realize the extraction of the essential oil of high-content linalool.
In above-mentioned apparatus, heating device 6 selects electric furnace, 1 leaf sample treating capacity 100g-500g of cucurbit, reflux ratio controller
15 (can be sold for market) regulatable return-flows when reflux cycle.
1 essential oil extracting device of comparative example
As shown in Fig. 2, building essential oil extracting device, wherein the device includes cucurbit 2, and the periphery of cucurbit 2, which is equipped with, to be added
The bottleneck of thermal 1, cucurbit 1 is equipped with branch mouth, the import connection of branch mouth and a return pipe 3, the side wall top and the bottom of return pipe 3
It is respectively equipped with cold liquid inlet and hydrothermal solution outlet, the outlet of return pipe 3 passes through 4 connection of an adapter tube and a receiving flask.
In above-mentioned apparatus, heating device 1 selects electric furnace (same as Example 1), has a thermometer to be inserted into from 2 mouthfuls of cucurbit
Liquid to cucurbit 1, cucurbit 2 select 1000mL flask.
2 method of extraction of essential oil of embodiment
(1) material leaf processing: clean, anhydrous fragrant camphor tree fresh leaf is acquired, mixes well and is crushed to 40-60 mesh, be uniformly divided into two
Part, every part of each 100.0g is placed in closed preservation under low temperature；
(2) by the distillation cascade in the essential oil extracting device of a copy of it fresh leaf filling embodiment 1, water is put into cucurbit,
Fresh leaf and water solid-liquid mass ratio 1: 4-1: 20 open heating device, so that water is heated to 100 DEG C and maintain the vapo(u)rizing temperature, will steam
The vapor evaporated is introduced into fresh leaf, mixes the essential oil steam of leaf material with vapor, obtains oil mixing with water air-flow；
(3) the return pipe a in essential oil extracting device of the oil mixing with water air-flow successively through embodiment 1, the branch pipe on return pipe a
A, the steam port a of the condenser pipe a in return pipe b, steam port b, the branch pipe b on return pipe a, form reflux condensation mode circulation path,
When beginning with essential oil discharging in receiving flask, reflux ratio control will be discharged in 0%-50% by control reflux ratio controller, returned
Period 10-60s is flowed, is during which collected essential oil component 3 times, number 1-3, until the fresh leaf of total reservoir volume and addition containing linalool
Ratio 0.3%-1.0% between gross mass；Pass through control discharging again and control discharging reflux ratio in 50%-80% than return channel,
During which reflux cycle 40s is collected essential oil component 2 times, number 4-5, until the fresh leaf of total reservoir volume and addition containing linalool is total
Ratio between quality is in 0.5%-1.8%.
After the extraction of essential oil of each batch, GC-MS detection is carried out respectively, the results are shown in Table 1.
Table 1
As shown in Table 1, the percentage contents of linalool are mentioned compared with conventional process conditions in number 1-5 essential oil component
It is high.
2 method of extraction of essential oil of comparative example
(1) material leaf processing: clean, anhydrous fragrant camphor tree fresh leaf is acquired, mixes well and is crushed to 40-60 mesh, be uniformly divided into two
Part, every part of each 100.0g is placed in closed preservation under low temperature；
(2) another fresh leaf and water is taken to be put into the cucurbit in the essential oil extracting device of comparative example 1, fresh leaf and water solid-liquid matter
Ratio 1: 4-1: 20 is measured, heating device is opened, so that water is heated to 100 DEG C and maintain the vapo(u)rizing temperature, the vapor of distillation is introduced
It in fresh leaf, mixes the essential oil steam of leaf material with vapor, obtains oil mixing with water air-flow；(3) oil mixing with water air-flow successively passes through pair
Return pipe in the essential oil extracting device of ratio 1 is passed through cold water in return pipe and is cooled down, and the essential oil condensed is through adapter tube
It instills in receiving flask, is controlled during reflux discharging without reflux, and essential oil is collected using disposable discharge method.
After extraction of essential oil, 0.75ml essential oil is obtained in total, GC-MS detection is carried out to the component of the essential oil, wherein virtue
Camphor tree alcohol percentage contents are 88.10%, and the results are shown in Table 1.
Comparative example 2 and comparative example 2 are it is found that obtain high-content through extracting method provided by the invention and extraction element
The essential oil of linalool, more general water distill principal component content in the essential oil of extraction process and are higher by 1.03%-5.08%.
3 method of extraction of essential oil of embodiment
(1) material leaf processing: clean, the anhydrous dextrorotation linalool type Huang camphor tree fresh leaf of acquisition mixes well and is crushed to 40-60
Mesh mixes well and is divided into two parts, every part of leaf quality 200.0g, closed preservation under low temperature.
(2) by the distillation cascade in the essential oil extracting device of a copy of it fresh leaf filling embodiment 1, water is put into cucurbit,
Fresh leaf and water solid-liquid mass ratio 1:4-1:20 open heating device, so that water is heated to 100 DEG C and maintain the vapo(u)rizing temperature, will steam
The vapor evaporated is introduced into fresh leaf, mixes the essential oil steam of leaf material with vapor, obtains oil mixing with water air-flow；
(3) the return pipe a in essential oil extracting device of the oil mixing with water air-flow successively through embodiment 1, the branch pipe on return pipe a
A, the steam port a of the condenser pipe a in return pipe b, steam port b, the branch pipe b on return pipe a, form reflux condensation mode circulation path,
When beginning with essential oil discharging in receiving flask, reflux ratio control will be discharged in 0%-50% by control reflux ratio controller, returned
Period 10-60s is flowed, is during which collected essential oil component 2 times, number 1-2, until the fresh leaf of total reservoir volume and addition containing linalool is total
Ratio 0.3%-1.0% between quality；Reflux ratio control will be discharged in 50%-80% than return channel by control discharging again, returned
Period 40s is flowed, is during which collected essential oil component 1 time, number 3, until the fresh leaf gross mass of total reservoir volume and addition containing linalool
Between ratio in 0.5%-1.8%.
After extraction of essential oil, GC-MS detection is carried out, the results are shown in Table 2.
Table 2
As seen from the results in Table 2, linalool percentage contents are higher by compared with conventional process conditions in number 1-3 essential oil component
2.32%-6.60%.
Comparative example 3
Take a fresh leaf 200g, the linalool percentage composition with 2 same treatment of comparative example, in obtained essential oil in implementation 3
It is 90.74%.
Embodiment 3 and comparative example 3 compare, and obtain high-content virtue camphor tree through extracting method provided by the invention and extraction element
The essential oil of alcohol, more general water distill principal component content in the essential oil of extraction process and are higher by 2.32%-6.6%.
In conclusion the content of principal component linalool essential oil mentions significantly in the essential oil that the method for the present invention and device obtain
Height is worth being widely applied.
Claims (9)
1. a kind of method of extraction of essential oil of high-content linalool, which comprises the steps of:
(1) it will be distilled in the distillation container in linalool type Huang camphor tree, fragrant camphor tree leaf and water adding apparatus, vapo(u)rizing temperature is 100 DEG C, will
The vapor of distillation is introduced into leaf, mixes the essential oil steam of leaf material with vapor, obtains oil mixing with water air-flow；
(2) oil mixing with water air-flow is condensed through the reflux component multi-reflow of device, collect different batches and has been separated from water
The essential oil component of liquid stops heating.
2. a kind of method of extraction of essential oil of high-content linalool according to claim 1, which is characterized in that the high-content
In the method for extraction of essential oil of linalool, the mass ratio of the linalool type Huang camphor tree, fragrant camphor tree leaf and the water that are added in step (1) is 1: 4-1:
20。
3. a kind of method of extraction of essential oil of high-content linalool according to claim 1, which is characterized in that the high-content
In the method for extraction of essential oil of linalool, linalool type Huang camphor tree described in step (1), fragrant camphor tree leaf are selected from fresh picking and go disleaf
Being shredded or be crushed to broken leaf after piece surface impurity can gone by the fresh leaf of 40-60 mesh or the fresh leaf of fresh picking
Except the leaf material weighed after surface impurity and moisture, and be sealed under low temperature immediately.
4. a kind of method of extraction of essential oil of high-content linalool according to claim 1, which is characterized in that in step (2)
Reflux condensation mode and collect process include the following steps；
(1) when the oil reservoir that the component that flows back begins with liquid occurs and oil reservoir can be collected component collection, control discharging reflux ratio
Within the scope of 0%-50%, reflux cycle within the scope of 10-60s, and the essential oil component for dividing 1-3 batch to collect liquid, to containing fragrant
Ratio between the linalool type Huang camphor tree of the total reservoir volume of camphor tree alcohol and addition, fragrant camphor tree leaf gross mass is at 0.3%-1.0% (mL/g)
When in range, first time essential oil component is obtained；
(2) control again discharging reflux ratio within the scope of 50-80%, reflux cycle within the scope of 10-40s, and point 1-3 batches are received
Collect essential oil component, until the ratio between the linalool type Huang camphor tree of total reservoir volume and addition containing linalool, fragrant camphor tree leaf gross mass exists
When in 0.5%-1.8% (mL/g) range, second of essential oil component is obtained；
(3) continue control discharging reflux ratio within the scope of 80%-90%, reflux cycle collects essential oil group within the scope of 10-60s
Point, until can stop heating when the essential oil volume steamed no longer changes, obtain third time essential oil component.
5. a kind of essential oil extracting device of high-content linalool, which is characterized in that the device includes flowing back for grease mixed airflow
Reflux component, and respectively with reflux component connection one can cause leaf material essential oil steam and distillation section, one collect
The collecting part of oil liquid after reflux.
6. a kind of essential oil extracting device of high-content linalool according to claim 5, which is characterized in that including a distillation
Component, reflux component and essential oil collecting part, distillation section include cucurbit and distillation cascade, and the periphery of cucurbit is equipped with one
Heating device, cucurbit are equipped with material mouth, the mouth of a river, and napex is equipped with gas outlet, gas outlet and distillation cascade one end connection, and distillation cascade is another
Return pipe a connection in one end and the reflux component, the reflux component includes return pipe a and return pipe b, return pipe a's
Upper and lower part on side wall is respectively equipped with the pipeline that branch mouth a and branch mouth b, branch mouth a and branch mouth b are controlled by being equipped with valve respectively
With the steam port a and steam port b connection on return pipe b, the periphery on the top return pipe b is arranged with condenser pipe, condenser pipe side wall
Upper and lower part is extended through equipped with hydrothermal solution outlet and cold liquid inlet, is passed through above and below the side wall of the lower part return pipe b respectively
It is equipped with steam port a, steam port b, is located in return pipe b and is located between steam port a and condensation bottom of the tube and be equipped with a reflux ratio
The bottom end of controller, return pipe b is equipped with oil outlet, the receiving flask connection of oil outlet lower part and the collecting part, the collection
Component includes a receiving flask.
7. a kind of essential oil extracting device of high-content linalool according to claim 5, which is characterized in that the reflux portion
The top opening portion of the return pipe a of part is equipped with a temperature detector.
8. a kind of essential oil extracting device of high-content linalool according to claim 5, which is characterized in that the high-content
In the essential oil extracting device of linalool, several net-like spacers respectively are equipped in the distillation cascade in the distillation section.
9. a kind of essential oil extracting device of high-content linalool according to claim 5, which is characterized in that the collection portion
Part further includes the essential oil volume measurement device of one with receiving flask and oil outlet difference connection.
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| CN112179941A (en) * | 2019-07-05 | 2021-01-05 | 中粮生物化学（安徽）股份有限公司 | Method for measuring alcoholic strength |
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