CN109897730A - A kind of Du Xiang refined volatile oil refinement method - Google Patents
A kind of Du Xiang refined volatile oil refinement method Download PDFInfo
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- CN109897730A CN109897730A CN201910202547.2A CN201910202547A CN109897730A CN 109897730 A CN109897730 A CN 109897730A CN 201910202547 A CN201910202547 A CN 201910202547A CN 109897730 A CN109897730 A CN 109897730A
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Abstract
The invention belongs to plant refinement technique field, in particular a kind of Du Xiang refined volatile oil refinement method and device.This method can not only extract Du Xiang volatile oil by Soxhlet extraction step and steam distillation step two-step pretreatment, can also obtain the medicinal extract of Du Xiang extraction, improve profit margin；Simultaneously, a kind of Du Xiang refined volatile oil refinement is provided, the device includes preprocessing module, refining module and collection module, and the collection module includes reverse osmosis membrane separation device and collection device, which may be implemented the effective quick separating and consecutive production of Du Xiang volatile oil refinement.
Description
Technical field
The invention belongs to plant refinement technique fields, are related to the method for ESSENTIAL OIL refinement, in particular a kind of Du
Fragrant refined volatile oil refinement method.
Background technique
Du Xiang (Ledum palustre L.) is that Angiospermae Ericaceae Du Xiang belongs to evergreen shrubs, is Chinese tradition
Du Xiangcai is also important spice berry.Du Xiang platymiscium is distributed temperate zone or cool temperature zone on the Northern Hemisphere, such as middle part in Europe, north
Portion, America and Northern Asia are distributed mainly on Xing'anling mountains and Changbai Mountain area in China, are mainly grown in wet
Mossery, depression etc..The compounds such as Du Xiang platymiscium volatile oil rich in, flavonoids and terpene.The branch of Du Xiang, leaf,
The extractable volatile oil fragrant out of colored and fruit, wherein flower, fruit oil yield are higher.The effect of Du Xiang volatile oil component, has been employed
In fields such as daily life, medical treatment, production of flavor, as Du Xiang volatile oil can expand blood vessel, reduce blood pressure, antitussive and antiasthmatic, control
Gastric ulcer and irregular menstruation are treated, while also having significant therapeutic effect in terms of sterilization, treating beriberi and treatment.
Du Xiang volatile oil frequently with extracting method have steam distillation (SD), ethanol ether extraction, CO2 it is overcritical
(SFE) and solid phase microextraction (SPME) etc. when, but present Du Xiang volatile oil is refined, continuity is bad, and energy consumption is high, entirely
Process is longer, thus causes the utilization rate of Du Xiang and yield to reduce, increases production cost, be unfavorable for carrying out large batch of
Production, and profit margin is low.
Summary of the invention
To solve the problems mentioned above in the background art.The present invention provides a kind of Du Xiang refined volatile oil refinement sides
Method, this method continuous production degree is high, raw material availability is high.
To achieve the above object, the invention provides the following technical scheme:
A kind of Du Xiang refined volatile oil refinement method, preparation process are as follows:
S1: after disintegrating apparatus crushing is added in Du Xiang plant, it is mixed with solvent；
S2: broken wall equipment carries out broken wall treatment；
S3: after broken wall treatment, Soxhlet extraction is carried out by Soxhlet reflux unit, obtains extracting solution；
S4: extracting solution is transferred in steam distillation device, carry out steam distillation, obtain steam distillation efflux and
Liquid Residue is extracted, the Du Xiang medicinal extract of Liquid Residue concentration will be extracted；
S5: steam distillation efflux is passed through reverse osmosis membrane separation device and is concentrated to get Du Xiang refined volatile oil.
Preferably, the Du Xiang plant pulverized particles size is 100~200 mesh.
The solvent is organic solvent, including but not limited to methanol, ethyl alcohol, acetone, ether, ethyl acetate, alkane etc..
Preferably, the Soxhlet extraction time 0.5h~8h.It is furthermore preferred that the Soxhlet extraction time is 2h~4h.
Preferably, the steam distillation time 0.5h~4h.
Preferably, the concentration condition are as follows: concentration flow velocity is 40~50L/h, pressure is 15~25kg/ in reverse osmosis membrane
m2, the outer vacuum degree of reverse osmosis membrane is 0~-0.1MPa.
In order to realize above-mentioned Du Xiang refined volatile oil refinement method, the present invention also provides a kind of Du Xiang refined volatile oils to mention
Refining system: including preprocessing module, refining module and collection module, the preprocessing module includes pulverizing unit, solvent addition
Unit and broken wall unit, the solvent that the pulverizing unit exports the output of solvent adding unit described in the Du Xiangyu crushed are defeated after mixing
Enter into the broken wall unit and carry out broken wall treatment, the refining module includes at least two in parallel Soxhlet reflux units and extremely
Few two distillation units, the output end of the Soxhlet reflux unit are connected in the distillation unit, and the collection module includes
Reverse osmosis membrane separation device and the collection device for being connected to the reverse osmosis membrane separation device output end, the distillation unit
Distillation substrate is separated by the reverse osmosis membrane separation device.
Preferably, the distillation unit includes positive process distiller and inverse process distiller, and the positive process distiller is used
Steam distillation processing is carried out in the solution exported to the Soxhlet reflux unit, the inverse process distiller is used for described anti-
Filtered fluid in infiltration membrane separation device carries out distillation processing.
Preferably, the output end of the inverse process distiller have for steam condensation condenser, the condenser with
The condenser pipe series connection, and connect with cold water source.
Preferably, reverse osmosis membrane includes oleophilic drainage film and hydrophilic and oleophobic film in the reverse osmosis membrane separation device, described
Reverse osmosis membrane separation device includes three-port structure, and the oleophilic drainage film and the hydrophilic and oleophobic film are located at the threeway
Structure steam distillation efflux entrance two sides.
Compared with prior art, the beneficial effects of the present invention are:
1, the present invention is located in advance carrying out mixing by way of merga pass means for breaking walls is crushed with solvent to Du Xiang plant
Reason, can effectively increase the precipitation of cost-effectively in Du Xiang plant in this way, mention by Soxhlet reflux unit to Du Xiang
When taking, the time of Du Xiang extraction can also be reduced, shortens the whole refinement time, while increasing the recovery rate of Du Xiang volatile oil,
Improve profit margin.
2, by Soxhlet extraction step and steam distillation step, Du Xiang volatile oil can be not only extracted, can also be obtained
The medicinal extract that Du Xiang is extracted improves profit margin.
3, it is directed to the slower process for the treatment of process, the present invention is equipped with multiple Soxhlet reflux units, and Du Xiang puts into rope
Time in family name's reflux unit is different, thus can handle the Du Xiang of volume within the short time, and reduce interruption or keep away
Exempt from the intermittent time occur, improves the speed integrally produced.
4, the present invention is carrying out the waste liquid in reverse osmosis membrane separation device at distillation by the distiller in distillation unit
Reason, can be quickly obtained waste residue, also reduce the demand to water resource, reduce the secondary treatment problem of waste liquid, while and rope
In family name's reflux unit condenser pipe series connection, it is easy to produce in water route integration and circulation supply.
Detailed description of the invention
Attached drawing is used to provide further understanding of the present invention, and constitutes part of specification, with reality of the invention
It applies example to be used to explain the present invention together, not be construed as limiting the invention.In the accompanying drawings:
Fig. 1 is system block diagram of the invention；
Fig. 2 is that the water in the present invention recycles schematic diagram；
Fig. 3 is reverse osmosis membrane separation schematic device in the present invention.
In figure: 1, preprocessing module；11, pulverizing unit；12, solvent adding unit；13, broken wall unit；2, module is refined；
21, Soxhlet reflux unit；211, condenser；22, distillation unit；3, collection module；31, reverse osmosis membrane separation device；32, it collects
Device；311, oleophilic drainage film；312, hydrophilic and oleophobic film.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1
Fig. 1-3 is please referred to, the present invention is the following technical schemes are provided: a kind of refined volatile oil refines system, including pretreatment
Module 1, refining module 2 and collection module 3, preprocessing module 1 include pulverizing unit 11, solvent adding unit 12 and broken wall unit
13, it is input in broken wall unit 13 after the solvent mixing that the Du Xiangyu solvent adding unit 12 that the output of pulverizing unit 11 crushes exports
Broken wall treatment is carried out, refining module 2 includes at least two Soxhlet reflux units 21 and at least two distillation units 22 in parallel, rope
The output end of family name's reflux unit 21 is connected in distillation unit 22, and collection module 3 includes reverse osmosis membrane separation device 31 and connects
The collection device 32 in 31 output end of reverse osmosis membrane separation device is connect, the distillation substrate of distillation unit 22 passes through reverse osmosis membrane separation
Device 31 is separated.
Specifically, Soxhlet reflux unit 21 includes extraction flask, extraction tube and condenser pipe, extraction tube is for holding broken wall unit
The material of 13 outputs, and condenser pipe and extraction flask are located at the two sides up and down of extraction tube；Material is imported in extraction tube, is extracted
When, it by material packet in fat-free filter paper packet, is put into extraction tube, petroleum ether, heating extraction bottle, petroleum ether gas is added in extraction flask
Change, condenser is ascended by connecting tube, congeals into liquid and instill in extraction tube, extract the lipid material in sample, pipe to be extracted
Interior petroleum ether liquid level reach a certain height, and flows into extraction flask through siphon pipe dissolved with the petroleum ether of crude fat, flows into extraction flask
Petroleum ether continues to be heated gasification, rising, condensation, instills in extraction tube, loops back and forth like this, until extracting completely.
Specifically, several extraction tubes are sequentially placed into the material exported in broken wall unit 13 according to regular hour sequence；
Due to being put into broken wall unit 13 according to regular hour sequence, can thus be produced to avoid when placing material next time
Production gap, therefore increase the continuity of production.
Specifically, distillation unit 22 includes positive process distiller and inverse process distiller, positive process distiller is used for rope
The solution that family name's reflux unit 21 exports carries out steam distillation processing, and inverse process distiller is used for reverse osmosis membrane separation device 31
In filtered fluid carry out distillation processing；The filtrate in reverse osmosis membrane separation device 31 can quickly be handled in this way, and
Available filter residue is purged, and reduces the storage of filtrate and the use of secondary treatment equipment.
Specifically, the output end of inverse process distiller have for steam condensation condenser 211, condenser 211 with it is cold
Solidifying pipe series connection, and connect with cold water source；Water route integration and circulation supply in easy to produce.
Specifically, one of the mode of reverse osmosis membrane separation device 31: quantity at least two, and it is both connected to distillation unit
22 output end；Two reverse osmosis membrane separation devices 31 use identical power source, give pressure to the material on reverse osmosis membrane,
The efficiency of permeability and separation in this way doubles.
Specifically, one of the another way of reverse osmosis membrane separation device 31 are as follows: reverse osmosis in reverse osmosis membrane separation device 31
Permeable membrane includes oleophilic drainage film 311 and hydrophilic and oleophobic film 312, and the reverse osmosis membrane separation device includes three-port structure, described
Oleophilic drainage film 311 and the hydrophilic and oleophobic film 312 are located at three-port structure steam distillation efflux entrance two sides.
The working principle and process for using of present system: Du Xiang is first placed into pulverizing unit and is crushed, according to
The type of Du Xiang is ground into different ranks, then will crush the Du Xiangyu solvent finished and mixes, is passed into broken wall later
Broken wall treatment is carried out in unit, mixes the active principle in Du Xiangcai sufficiently with solvent；Pass through multiple Soxhlet reflux units 21
It can guarantee the whole continuity of production, it, thus can be by the placement raw material being spaced in Soxhlet reflux unit 21
In the gap of blowing, still there are other Soxhlet reflux units 21 and continuing to produce, nonproductive time gap is filled out
It mends；Solution after Soxhlet reflux unit 21 and distillation unit 22 distill was carried out by reverse osmosis membrane separation device 31
Filter, then can be collected.
It should be noted that a kind of refined volatile oil provided by the invention refines system, it is not only applicable to the essence of Du Xiang
The refinement of volatile oil processed, the purification for applying also for the volatile oil such as other oil plants, Chinese medicine are refined.
Embodiment 2
A kind of Du Xiang refined volatile oil refinement method, preparation process are as follows:
S1: after the Du Xiang plant leaf blade 50kg disintegrating apparatus that pulverizing unit is added is crushed to 100 mesh, it is mixed with ethyl alcohol
It closes；
S2: the broken wall equipment of broken wall unit carries out broken wall treatment；
S3: after broken wall treatment, Soxhlet extraction 2h is carried out by Soxhlet reflux unit, obtains extracting solution；
S4: extracting solution is transferred in steam distillation device, carries out steam distillation 0.5h, obtains steam distillation outflow
Liquid and extraction Liquid Residue, will extract the Du Xiang medicinal extract of Liquid Residue concentration；
S5: steam distillation efflux is passed through the concentration of reverse osmosis membrane separation device, the concentration condition are as follows: concentration flow velocity
It is 15kg/m for pressure in 40L/h, reverse osmosis membrane2, the outer vacuum degree of reverse osmosis membrane is that -0.1MPa obtains Du Xiang purification volatilization
Oil.
The recovery rate of Du Xiang refined volatile oil: 0.541%.
Embodiment 3
A kind of Du Xiang refined volatile oil refinement method, preparation process are as follows:
S1: after Du Xiang plant leaf blade 50kg addition disintegrating apparatus is crushed to 200 mesh, it is mixed with acetone；
S2: broken wall equipment carries out broken wall treatment；
S3: after broken wall treatment, Soxhlet extraction 8h is carried out by different Soxhlet reflux units, obtains extracting solution；
S4: extracting solution is transferred in steam distillation device, is carried out steam distillation 4h, is obtained steam distillation efflux
With extraction Liquid Residue, the Du Xiang medicinal extract of Liquid Residue concentration will be extracted；
S5: steam distillation efflux is passed through the concentration of reverse osmosis membrane separation device, condition is concentrated are as follows: flow velocity, which is concentrated, is
Pressure is 25kg/m in 50L/h, reverse osmosis membrane2, the outer vacuum degree of reverse osmosis membrane is -0.08MPa, obtains Du Xiang purification volatilization
Oil.
The recovery rate of Du Xiang refined volatile oil: 0.525%.
Comparative example 1 (steam distillation)
S1: after Du Xiang plant leaf blade 50kg addition disintegrating apparatus is crushed to 200 mesh, it is mixed with acetone；
S2: steam distillation 4h obtains steam distillation efflux；
S3: Liquid liquid Separation obtains Du Xiang volatile oil.
The recovery rate of Du Xiang volatile oil: 0.382%.
As can be seen that carry out Du Xiang volatile oil extracting effect by the method for the invention has very than extraction by steam distillation rate
Using present device and continuous continual production may be implemented in big raising.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features.
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (10)
1. a kind of Du Xiang refined volatile oil refinement method, it is characterised in that: the following steps are included:
S1: after disintegrating apparatus crushing is added in Du Xiang plant, it is mixed with solvent；
S2: broken wall equipment carries out broken wall treatment；
S3: after broken wall treatment, Soxhlet extraction is carried out by Soxhlet reflux unit, obtains extracting solution；
S4: extracting solution is transferred in steam distillation device, is carried out steam distillation, is obtained steam distillation efflux and extraction
Liquid Residue will extract the Du Xiang medicinal extract of Liquid Residue concentration；
S5: steam distillation efflux is passed through reverse osmosis membrane separation device and is concentrated to get Du Xiang refined volatile oil.
2. a kind of Du Xiang refined volatile oil refinement method according to claim 1, it is characterised in that: the Du Xiang Plant Powder
Broken particle size is 100~200 mesh.
3. a kind of Du Xiang refined volatile oil refinement method according to claim 1, it is characterised in that: the solvent is organic
Solvent.
4. a kind of Du Xiang refined volatile oil refinement method according to claim 1, it is characterised in that: when the Soxhlet extraction
Between 0.5h~8h.
5. a kind of Du Xiang refined volatile oil refinement method according to claim 1, it is characterised in that: the steam distillation
Time 0.5h~4h.
6. a kind of Du Xiang refined volatile oil refinement method according to claim 1, it is characterised in that: the concentration condition
Are as follows: concentration flow velocity is 40~50L/h, pressure is 15~25kg/m in reverse osmosis membrane2, the outer vacuum degree of reverse osmosis membrane is 0~-
0.1MPa。
7. a kind of refinement system of Du Xiang refined volatile oil refinement method according to claim 1, it is characterised in that: including
Preprocessing module (1), refining module (2) and collection module (3), the preprocessing module (1) include pulverizing unit (11), solvent
Adding unit (12) and broken wall unit (13), the pulverizing unit (11) export solvent adding unit described in the Du Xiangyu crushed
(12) it is input in the broken wall unit (13) after the solvent mixing exported and carries out broken wall treatment, the refining module (2) includes
At least two in parallel Soxhlet reflux units (21) and at least two distillation units (22), the Soxhlet reflux unit (21) it is defeated
Outlet is connected in the distillation unit (22), and the collection module (3) includes reverse osmosis membrane separation device (31) and connection
In the collection device (32) of reverse osmosis membrane separation device (31) output end, the distillation substrate of the distillation unit (22) passes through
The reverse osmosis membrane separation device (31) is separated.
8. refinement system according to claim 7, it is characterised in that: the distillation unit (22) includes positive process distiller
With inverse process distiller, the solution that the positive process distiller is used to export the Soxhlet reflux unit (21) carries out vapor
Distillation processing, the inverse process distiller is for carrying out at distillation the filtered fluid in the reverse osmosis membrane separation device (31)
Reason.
9. refinement system according to claim 8, it is characterised in that: the output end of the inverse process distiller, which has, to be used for
The condenser (211) of steam condensation, the condenser (211) is connected with the condenser pipe, and connect with cold water source.
10. refinement system according to claim 7, it is characterised in that: reverse osmosis in the reverse osmosis membrane separation device (31)
Permeable membrane includes oleophilic drainage film (311) and hydrophilic and oleophobic film (312), and the reverse osmosis membrane separation device includes three-port structure,
The oleophilic drainage film (311) and the hydrophilic and oleophobic film (312) are located at the three-port structure steam distillation efflux
Entrance two sides.
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Cited By (1)
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| CN115322837A (en) * | 2022-08-17 | 2022-11-11 | 东北林业大学 | Refined ledum essential oil refining process and antibacterial application thereof |
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Application publication date: 20190618 |