CN104277917B - A kind of industrial hemp method of extraction of essential oil and its extraction equipment rich in cannabidiol - Google Patents
A kind of industrial hemp method of extraction of essential oil and its extraction equipment rich in cannabidiol Download PDFInfo
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- CN104277917B CN104277917B CN201410574240.2A CN201410574240A CN104277917B CN 104277917 B CN104277917 B CN 104277917B CN 201410574240 A CN201410574240 A CN 201410574240A CN 104277917 B CN104277917 B CN 104277917B
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/022—Refining
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
Abstract
The invention discloses a kind of industrial hemp method of extraction of essential oil and its extraction equipment rich in cannabidiol, by using screening washer, oven, the fermentation vat that pipeline is sequentially connected, Rotary Evaporators, tank is stirred by ultrasonic, butterfly centrifugal machine, first climbing film evaporator, proportioning tank, pressurization chromatographic silica gel post, wash out flow container, second climbing film evaporator, Rotary Evaporators, the equipment such as finished pot and solvent recovery tank is progressively screened to industrial hemp, baking, extraction, reprocessing, filtering, monitoring, loading, chromatography, concentration and the operating procedure of finished product, finally extract the industrial hemp essential oil rich in active ingredient cannabidiol.Instant invention overcomes the shortcomings that the efficiency in traditional handicraft is low, consumption is big and is not easy to large-scale production, and the semi-finished product containing THC are legal, safe efficient without artificial contact and circulation in processing; process is simple, and product purity is high, and active ingredient is complete; cost is cheap, is easy to promote.
Description
Technical field
The present invention relates to field of plant extraction, more particularly to a kind of extraction of the industrial hemp essential oil rich in cannabidiol
Method, also relate to the extraction equipment used during industrial hemp extraction of essential oil of the manufacture rich in cannabidiol.
Background technology
At present, the extracting method of industrial hemp essential oil is mainly using the extracting mode of organic solvent immersion, due to extract
Composition is included in its histocyte, and the periphery of cell is the cell of the material compositions such as one layer of cellulose, hemicellulose and pectin
Wall, it is plasm in cell membrane, being operated by heating, ultrasound etc. in preprocessing process, destroys plasmic physiology work(
Can, make the active ingredient in industrial hemp cell and other solable matters penetrated into outside cell, then, it is to be separated go out we
Required active ingredient, it is necessary to further by the method for chromatography, obtain the industrial hemp essential oil rich in cannabidiol；Due to work
Sparetime university's sack contains drug ingredient THC so that it is each that the extraction process and flow of industrial hemp essential oil have to comply with China
Item provisions of laws and regulations, and under the supervision of relevant departments fairly develop and utilize；
Existing extracting method is mostly open now, all different degrees of presence artificially contact and interference, is unfavorable for work
The security development of sparetime university fiber crops and utilization, and extraction efficiency is low, and power consumption is big, is also unfavorable for the large-scale production of industrial hemp and big
Scope is promoted.
The content of the invention
The present invention solves the technical problem of provide a kind of industrial hemp method of extraction of essential oil rich in cannabidiol
And its extraction equipment, effectively, safely, sufficiently resource can be carried out by the setting of the multiple movable valves of use in a device
Recycle, also reduce the possibility of artificial contact product in process of production, it is safe efficient.
In order to solve the above technical problems, one aspect of the present invention is：There is provided a kind of rich in cannabidiol
Industrial hemp method of extraction of essential oil, including following extraction step：
1) screen：The industrial hemp floral leaf of selection is screened, wherein mouldy, rotten part is chosen, beaten
Powder, dedusting, form industrial hemp floral leaf raw material；
2) toast：Industrial hemp floral leaf raw material after screening is laid in baking pan, oven baking is put into, bakes temperature：
160 DEG C, toast 30 minutes, the raw material moisture after drying is less than 8%；
3）Extraction：Industrial hemp floral leaf raw material after drying is put into fermentation vat by pipeline, is 1 by weight ratio:1
Raw material and solvent mixing, are sufficiently stirred, at room temperature constant temperature extracting at least two hour, obtain industrial hemp raw material leaching liquor, extract
Liquid enters the first solvent cell by solvent outlet B, and the pipeline that leaching liquor is set by the first solvent cell bottom enters the second solvent
Pond, evaporative removal solvent, obtain semifluid leaching liquor；In addition, solvent passes through in the first solvent cell and the second solvent cell top
The solvent vapo(u)r outlet A1 and A2 not set is exported, and pass sequentially through condensation reservoir and volatile oil solvent tank reclaimed again it is sharp
With；
4）Reprocessing：By semifluid leaching liquor by pipeline to tank is stirred by ultrasonic, heating-up temperature is the boiling point of solvent
Temperature, minute time 10-15, then add diluent, solid-liquid ratio 1:5, in mass, the hemp leaching liquor diluted,
The hemp leaching liquor of dilution is shaken using ultrasonic agitation tank, the time is 15-30 minutes, supersonic frequency 40KHz, is obtained
Industrial hemp leaching liquor rich in active ingredient；
5）Filtering：Industrial hemp leaching liquor is transmitted to butterfly centrifugal machine by pipeline, filtered at room temperature, rotating speed 8000r/
Min, transmitted after filtering by pipeline into the first climbing film evaporator, remove diluent, it is primary to obtain on-line industry hemp essential oil
Product；
6）Monitoring：On-line industry hemp essential oil primary product is detected by on-line measuring device, will after detection is qualified
Proportioning tank enters step 7 before it is delivered to loading, otherwise return to step 5；
7）Loading：Add elution dilution agent, solid-liquid ratio 1:1, in mass, elute and obtain loading eluent, dilute
Top loading of the loading eluent afterwards by pipeline to chromatographic silica gel post of pressurizeing；
8）Chromatography：By the suction-operated for chromatographic silica gel post of pressurizeing, isocratic elution obtains product dilution after 10 hours, will
Product dilution is transmitted to corresponding fluid reservoir by pipeline；The eluant, eluent separated in chromatography is transmitted to successively by pipeline
One solvent tank and the second solvent tank are recycled；
9）Elution：Isocratic elution is carried out to the loading material in pillar using the eluent matched, produced after elution
Product dilution, by carrying out online HPLC detections, according to testing result by product dilution difference fraction collection to accordingly it is molten
In agent tank, wherein, detect qualified product dilution and enter the second climbing film evaporator 13, otherwise, it is dilute to detect underproof product
Release liquid and enter solvent recovery proportioning tank 12, carry out concentration and isocratic elution again successively, solvent recovery recycles；
10）Concentration：In the second climbing film evaporator, temperature 60 C carries out initial concentration, and the product dilution after concentration leads to
Piping is delivered to Rotary Evaporators, and temperature is 60-80 DEG C, and operating pressure 0.01MPa-0.03MPa, operating pressure is when draining
0.06-0.08MPa, eluant, eluent is removed completely and obtains the industrial hemp essential oil crude product rich in cannabidiol；
11）Finished product：The industrial hemp essential oil crude product of cannabidiol be will be enriched in by pipeline to finished pot, add examination
Agent, the removal of impurity is gone by high pressure elution device, after detection is qualified, labeling, storage, obtain finished product.
In a preferred embodiment of the present invention, the step（7）In, the eluant, eluent be petroleum ether and dichloromethane with
Mass ratio is 6:1 washing lotion mixed, 10 hours of elution time.
In a preferred embodiment of the present invention, step（10）In, liter film is provided with second climbing film evaporator and is steamed
Circulation pipe is sent out, the circulating condensing coolant-temperature gage in the climbing-film evaporation circulation pipe is 10 DEG C, washing in second climbing film evaporator
De- liquid recovered liquid carries out circulation concentration by the climbing-film evaporation circulation pipe, the eluant, eluent recovery in second climbing film evaporator
Liquid is recycled by pipeline to solvent recovery proportioning tank；Rotary evaporation is provided with the Rotary Evaporators to follow
Endless tube, caused eluant, eluent recovered liquid is delivered to the solvent recovery tank by rotary evaporation circulation pipe in the Rotary Evaporators
In.
In a preferred embodiment of the present invention, step（11）In, the reagent is in n-hexane, ethyl acetate and methanol
At least one.
In a preferred embodiment of the present invention, step（3）Described in solvent be any one in petroleum ether or 6# solvent naphthas
Kind.
In a preferred embodiment of the present invention, step（4）Described in diluent be methanol or absolute ethyl alcohol.
A kind of extraction equipment is also provided, including：Screening washer, oven, the fermentation vat being sequentially connected by pipeline, the first solvent
Proportioning tank, pressurization chromatographic silica gel before pond, the second solvent cell, ultrasonic agitation tank, butterfly centrifugal machine, the first climbing film evaporator, loading
Post, elution flow container, solvent recovery proportioning tank, the second climbing film evaporator, Rotary Evaporators and finished pot, in addition to solvent recovery
Tank, the first solvent tank, the second solvent tank, condensation reservoir and volatile oil solvent tank, the fermentation vat include the solvent that top is set and entered
Mouthful, floral leaf be put into mouth, solvent vapour outlet A1 and its bottom set solvent outlet B and its side wall set steam (vapor) outlet,
Steam inlet, floral leaf discharging opening, the fermentation vat are described by solvent outlet B successively external first solvent cell, the second solvent cell
Second solvent cell is internally provided with heating and evaporating unit, and second solvent cell is provided with solvent vapo(u)r outlet A2 at the top of it
And leaching liquor outlet is provided with its bottom, and the input of solvent vapo(u)r outlet A2 connection condensation reservoirs, the output of condensation reservoir
The input of end connection solvent tank, the output end of the solvent tank connect the colvent inlet end of the fermentation vat, the fermentation vat
Solvent vapour outlet A1 connection condensation reservoirs input, the top setting recovered liquid output end of the pressurization chromatographic silica gel post is simultaneously
Be provided with chromatographic solution output end in its bottom, the recovered liquid output end connect respectively the first solvent tank and the second solvent tank and
Corresponding movable valve is provided with connecting pipe, the chromatographic solution output end connects the elution flow container, first solvent
Top between tank and the second solvent tank is connected by the pipeline with movable valve of setting, the top of first solvent tank
Connected with the top of the input of the second climbing film evaporator by the pipeline with movable valve of setting, second liter of film steams
The bottom for sending out the output end of device connects solvent recovery proportioning tank by pipeline.
In a preferred embodiment of the present invention, it is described ultrasonic agitation tank, butterfly centrifugal machine, the first climbing film evaporator, plus
Movable valve, the pressure level are provided with the input pipeline of pressure silica gel chromatography post, the first solvent tank and the second solvent tank
Analyse and be provided with movable valve at the pipeline at output of silicagel column, elution flow container, fluid reservoir and the second climbing film evaporator.
In a preferred embodiment of the present invention, the dress post device interior of the silica gel pressurizing chromatographic column is provided with stirring dress
Put, the agitating device is made up of agitating shaft and stirring vane two parts, and the upper end of the agitating shaft is provided with motor, the electricity
The control terminal of machine is connected with air pump, and the stirring vane is installed vertically in the rotary shaft of the agitating shaft.
In a preferred embodiment of the present invention, the solvent recovery proportioning tank has been arranged in parallel metering and has regarded pipe, and described the
The output end of one climbing film evaporator is provided with on-line measuring device, and the output end of the silica gel pressurizing chromatographic column is provided with online
HPLC detection devices, the evaporation rate of first climbing film evaporator and the second climbing film evaporator is the 10 of common evaporator
Times.
The beneficial effects of the invention are as follows：A kind of industrial hemp method of extraction of essential oil rich in cannabidiol of the present invention and its carry
Flower that taking equipment is discarded by using hemp, leaf be primary raw material, and supporting special extraction equipment to hemp progress effectively into
The abundant extraction divided, extraction equipment used are disposed as pipeline at the import and export of each production link, and are provided with corresponding
Movable valve control, thoroughly prevent artificially to participate in, it is ensured that the whole technique of the industrial hemp extraction of essential oil rich in cannabidiol
The security of flow and it is normative while, also improve the purity of product.
Brief description of the drawings
Technical scheme in order to illustrate the embodiments of the present invention more clearly, make required in being described below to embodiment
Accompanying drawing is briefly described, it should be apparent that, drawings in the following description are only some embodiments of the present invention, for
For those of ordinary skill in the art, on the premise of not paying creative work, it can also be obtained according to these accompanying drawings other
Accompanying drawing, wherein：
Fig. 1 is the present invention a kind of industrial hemp method of extraction of essential oil and its extraction equipment and its equipment rich in cannabidiol
A preferred embodiment process flow diagram；
Fig. 2 is the process flow diagram of leach step in the present invention.
The mark of each part is as follows in accompanying drawing：1st, condensation reservoir, 2, volatile oil solvent tank, 3, fermentation vat, the 4, first solvent cell,
5th, the second solvent cell, 6, ultrasonic agitation tank, 7, butterfly centrifugal machine, the 8, first climbing film evaporator, 9, proportioning tank before loading, 10 plus
Pressure silica gel chromatography post, 11, elution flow container, 12, solvent recovery proportioning tank, the 13, second climbing film evaporator, 14, Rotary Evaporators,
15th, finished pot, 16, solvent recovery tank, the 17, first solvent tank, the 18, second solvent tank.
Embodiment
The technical scheme in the embodiment of the present invention will be clearly and completely described below, it is clear that described implementation
Example is only the part of the embodiment of the present invention, rather than whole embodiments.It is common based on the embodiment in the present invention, this area
All other embodiment that technical staff is obtained under the premise of creative work is not made, belong to the model that the present invention protects
Enclose.
Fig. 1 and Fig. 2 are referred to, the embodiment of the present invention includes：
A kind of industrial hemp method of extraction of essential oil rich in cannabidiol, including following extraction step：
1) screen：The industrial hemp floral leaf of selection is screened, wherein mouldy, rotten part is chosen, beaten
Powder, dedusting, form industrial hemp floral leaf raw material；
2) toast：Industrial hemp floral leaf raw material after screening is laid in baking pan, oven baking is put into, bakes temperature：
160 DEG C, toast 30 minutes, the raw material moisture after drying is less than 8%.
3）Extraction：Industrial hemp floral leaf raw material after drying is put into fermentation vat 3 by pipeline, is 1 by weight ratio:1
Raw material and solvent mixing, are sufficiently stirred, at room temperature constant temperature extracting at least two hour, obtain industrial hemp raw material leaching liquor, extract
Liquid enters the first solvent cell 4 by solvent outlet B, and it is molten that the pipeline that leaching liquor is set by the bottom of the first solvent cell 4 enters second
Agent pond 5, evaporative removal solvent, obtain semifluid leaching liquor；In addition, solvent in the first solvent cell 4 and the second solvent cell 5 by pushing up
The solvent vapo(u)r outlet A1 and A2 that portion is set respectively is exported, and is returned according to this by condensation reservoir 1 and volatile oil solvent tank 2
Receive and recycle；The solvent is petroleum ether or 6# solvent naphthas；
4）Reprocessing：By semifluid leaching liquor by pipeline to ultrasonic agitation tank 6, heating-up temperature is the boiling point of solvent
Temperature, minute time 10-15, then add diluent, solid-liquid ratio 1:5, in mass, the hemp leaching liquor diluted,
The hemp leaching liquor of dilution is shaken using ultrasonic agitation tank 6, the time is 15-30 minutes, supersonic frequency 40KHz, is obtained
To the industrial hemp leaching liquor rich in active ingredient；The diluent is methanol or absolute ethyl alcohol；
5）Filtering：Industrial hemp leaching liquor is transmitted to butterfly centrifugal machine 7 by pipeline, filtered at room temperature, rotating speed
8000r/min, transmitted after filtering by pipeline into the first climbing film evaporator 8, remove diluent, obtain on-line industry hemp essence
Oily primary product；
6）Monitoring：On-line industry hemp essential oil primary product is detected by on-line measuring device, will after detection is qualified
Proportioning tank 9 enters step 7 before it is delivered to loading, otherwise return to step 5；
7）Loading：Add elution dilution agent, solid-liquid ratio 1:1, in mass, sample obtains sample solution after being completely dissolved,
Top loading by pipeline to chromatographic silica gel post 10 of pressurizeing；
8）Chromatography：By the suction-operated for chromatographic silica gel post 10 of pressurizeing, isocratic elution obtains chromatographic solution in 10 hours, will chromatograph
Liquid is transmitted to flow container 11 is eluted by pipeline, and the eluant, eluent isolated in chromatography is transmitted to the first solvent tank 17 successively by pipeline
Recycled with the second solvent tank 18；The eluant, eluent is petroleum ether and dichloromethane using mass ratio as 6:1 is mixed
Washing lotion, 10 hours of elution time；
9）Elution：Isocratic elution is carried out to the loading material in pillar using the eluent matched, produced after elution
Product dilution, online HPLC detections are carried out, product dilution is distinguished to corresponding solvent tank by fraction collection according to testing result
In, wherein, detect qualified product dilution and enter the second climbing film evaporator 13, otherwise, detect underproof product dilution
Into solvent recovery proportioning tank 12, concentration and isocratic elution again are carried out successively, and solvent recovery recycles；
10）Concentration：In the inside of the second climbing film evaporator 13, temperature 60 C carries out initial concentration, and the product after concentration is dilute
Liquid is released by pipeline to Rotary Evaporators 14, temperature is 60-80 DEG C, operating pressure 0.01MPa-0.03MPa, work when draining
It is 0.06-0.08MPa to make pressure, removes eluant, eluent completely and obtains the industrial hemp essential oil crude product rich in cannabidiol；Described
It is provided with climbing-film evaporation circulation pipe in two climbing film evaporators 13, the circulating condensing coolant-temperature gage in the climbing-film evaporation circulation pipe is 10
DEG C, the eluent recovered liquid in second climbing film evaporator 13 carries out circulation concentration, institute by the climbing-film evaporation circulation pipe
The eluant, eluent recovered liquid stated in the second climbing film evaporator 13 is recycled by pipeline to solvent recovery proportioning tank 12；
It is provided with rotary evaporation circulation pipe in the Rotary Evaporators 14, caused eluant, eluent recovered liquid in the Rotary Evaporators 14
It is delivered to by rotary evaporation circulation pipe in the solvent recovery tank 16；
11）Finished product：The industrial hemp essential oil crude product of cannabidiol be will be enriched in by pipeline to finished pot 15, add examination
Agent, the removal of impurity is gone by high pressure elution device, after detection is qualified, labeling, storage, obtain finished product；The reagent is n-hexane, second
At least one of acetoacetic ester and methanol.
A kind of extraction equipment is also provided, including：Screening washer, oven, the fermentation vat 3, first that is sequentially connected by pipeline are molten
Proportioning tank 9, pressurization before agent pond 4, the second solvent cell 5, ultrasonic agitation tank 6, butterfly centrifugal machine 7, the first climbing film evaporator 8, loading
Chromatographic silica gel post 10, elution flow container 11, solvent recovery proportioning tank 12, the second climbing film evaporator 13, Rotary Evaporators 14 and finished product
Tank 15, in addition to solvent recovery tank 16, the first solvent tank 17, the second solvent tank 18, condensation reservoir 1 and volatile oil solvent tank 2.
The fermentation vat 3 includes the colvent inlet of top setting, floral leaf is put into mouth, solvent vapour outlet A1 and its bottom are set
Steam (vapor) outlet, steam inlet, the floral leaf discharging opening that the solvent outlet B put and its side wall are set, the fermentation vat 3 pass through solvent
External first solvent cell 4, the second solvent cell 5, second solvent cell 5 are internally provided with heating and evaporating unit to outlet B successively,
Second solvent cell 5 is provided with solvent vapo(u)r outlet A2 at the top of it and leaching liquor outlet is provided with its bottom, described molten
The input of agent steam (vapor) outlet A2 connections condensation reservoir 1, the input of the output end connection solvent tank of condensation reservoir 1, the solvent tank
Output end connect the colvent inlet end of the fermentation vat 3, the solvent vapour outlet A1 connections condensation reservoir 1 of the fermentation vat 3
Input, see Fig. 2.
The top of the pressurization chromatographic silica gel post 10 sets recovered liquid output end and chromatographic solution output is provided with its bottom
End, the recovered liquid output end connect the first solvent tank 17 and the second solvent tank 18 and are provided with connecting pipe correspondingly respectively
Movable valve, the chromatographic solution output end connection elution flow container 11, the solvent tank 18 of the first solvent tank 17 and second
Between top connected by pipeline of the setting with movable valve, the top of first solvent tank 17 and second liter of film steam
The top of the input of device 13 is sent out by pipeline connection of the setting with movable valve, second climbing film evaporator 13 it is defeated
The bottom for going out end connects solvent recovery proportioning tank 12 by pipeline, sees Fig. 1.
The ultrasonic agitation tank 6, butterfly centrifugal machine 7, the first climbing film evaporator 8, pressurization chromatographic silica gel post 10, the first solvent
Movable valve, the pressurization chromatographic silica gel post 10, eluent are provided with the input pipeline of the solvent tank 18 of tank 17 and second
Movable valve is provided with the pipeline at output of tank 11, fluid reservoir and the second climbing film evaporator 13.
The dress post device interior of the silica gel pressurizing chromatographic column is provided with agitating device, the agitating device by agitating shaft and
Stirring vane two parts form, and the upper end of the agitating shaft is provided with motor, and the control terminal of the motor is connected with air pump, described
Stirring vane is installed vertically in the rotary shaft of the agitating shaft.
The solvent recovery proportioning tank 12 has been arranged in parallel metering and has regarded pipe, and the output end of first climbing film evaporator 8 is set
It is equipped with on-line measuring device, the output end of the silica gel pressurizing chromatographic column is provided with online HPLC detection devices, described first liter
The evaporation rate of the climbing film evaporator 13 of film evaporator 8 and second is 10 times of common evaporator.
Specific embodiment：
Go out leaching liquor flow：（See Fig. 2）
Industrial hemp floral leaf raw material after baking enters fermentation vat 3 by dog-house, and fermentation vat 3 is added by its colvent inlet
6# solvent naphtha dosage, soak at room temperature more than 2 hours, the first solvent cell 4 and second is sequentially entered by solvent outlet B as defined in entering
Solvent cell 5, most of 6# solvent naphthas are removed using steam-heated method in the second solvent cell 5, obtain industrial hemp raw material
Leaching liquor, 6# solvent naphthas pass sequentially through condensation reservoir 1 and volatile oil solvent tank 2 is reclaimed and recycled, and can input immersion repeatedly
Used in pond 3.
Go out industrial hemp essential oil flow chart：（See Fig. 1）
Industrial hemp raw material leaching liquor enters ultrasonic agitation tank 6 by leaching liquor entrance, and heating removes remaining 6# solvents,
Absolute ethyl alcohol is added, ultrasonic oscillation is handled more than 15 minutes, and the work rich in active ingredient is filtrated to get using butterfly centrifugal machine 7
Sparetime university's fiber crops extract solution, extract solution enter climbing film evaporator by pipeline, then on-line industry hemp essential oil primary product is obtained after concentrating,
This primary product, into proportioning tank 9 before loading, after being matched according to actual applied sample amount, passes through pipeline to the chromatography that pressurizes by pipeline
In silicagel column 10, isocratic elution is carried out to loading material using the eluent matched, passes through the absorption and desorption of silica gel
Effect affords product dilution；Product dilution is by HPLC on-line checkings, according to testing result, by product dilution point
Other fraction collection into corresponding solvent tank, wherein, detect qualified product dilution and be fed sequentially into second liter by pipeline
Film evaporator 13, otherwise, detect underproof product dilution and be delivered to solvent recovery proportioning tank 12, carry out successively concentration and again
Secondary isocratic elution；
In the second climbing film evaporator 13, temperature 60 C carries out initial concentration, and the product dilution after concentration passes through pipeline
Rotary Evaporators 14 are delivered to, temperature is 70 DEG C or so, operating pressure 0.02MPa or so, and operating pressure is 0.07MPa when draining
Left and right, eluant, eluent is removed completely and obtains the industrial hemp essential oil crude product rich in cannabidiol；Industrial hemp essential oil crude product passes through pipe
Road is delivered to finished pot 15, adds reagent, removes THC by high pressure elution device, after detection is qualified, labels, enters
Storehouse, obtain finished product；
Wherein, the eluant, eluent isolated is transmitted separately to the by pipeline in the chromatography process of pressurization chromatographic silica gel post 10
One solvent tank 17 and the second solvent tank 18 are recycled；Obtained eluant, eluent condensation is evaporated in the second climbing film evaporator 13
And transmitted by pipeline to the first solvent tank 17, it can recycle again.
In summary, hair of the deep processing of the extract of the industrial hemp rich in cannabidiol to China's industrial hemp industry
Exhibition has immeasurable effect, can further improve the added value of this pollution-free industry of China's industrial hemp；Use industrial hemp
Discarded flower and leaf makees raw material, using modern science and technology technology, turns waste into wealth, benefits common people；Plant standardized extract is fusion
The new high-tech product of modern pharmaceutical technology and biochemical technology, and new varieties of occupying inter-national market in recent years,
Processing stage is higher with scientific and technological content；Industrial hemp essential oil is by the life science, health science, Nutriology Dept. of the development mankind
Learn, medical science generation far-reaching influence, and common people pursue, international economy development new highlight；The exploitation of industrial hemp will fill
Divide and utilize resources advantage, using scientific and technological new technology, and produced in the case where meeting GAP, GMP requirement, while using above-mentioned advanced
Technique and quality detection technology so that the active ingredient of industrial hemp floral leaf extract maximizes, THC content symbol
Close and be less than 0.3% as defined in country and European Union；Industrial hemp essential oil is the deep processing to industrial hemp resource, and there is exploitation to throw
Enter advantage and the features such as less, with high content of technology, added value of product is big, international market is extensive.
A kind of beneficial effect of industrial hemp method of extraction of essential oil and its extraction equipment rich in cannabidiol of the present invention is：
First, the beneficial effects of the invention are as follows：Whole totally closed operation is realized in whole technological process, is avoided to greatest extent
Artificially participate in and disturb in production process, ensure raw material in whole production process into and out of all realizing mechanization, it is ensured that industry
The fairly development and utilization of hemp, links meet every provisions of laws and regulations of China and the world；
2nd, compared with common contaminated soil improvement and recovery technique, the technological process apparatus are advanced, efficient, safe, pole
The earth improves the content of active ingredient in industrial hemp floral leaf raw material, and active ingredient is complete after extraction, secondly whole production
Technique is clear and coherent, smooth, efficiency high, and equipment is obtained and is relatively easy to, is easy to promote.
Embodiments of the invention are the foregoing is only, are not intended to limit the scope of the invention, it is every to utilize this hair
The equivalent structure or equivalent flow conversion that bright description is made, or directly or indirectly it is used in other related technology necks
Domain, it is included within the scope of the present invention.
Claims (8)
1. a kind of industrial hemp method of extraction of essential oil rich in cannabidiol, it is characterised in that including following extraction step：
1) screen：The industrial hemp floral leaf of selection is screened, wherein mouldy, rotten part is chosen, beat powder,
Dedusting, form industrial hemp floral leaf raw material；
2) toast：Industrial hemp floral leaf raw material after screening is laid in baking pan, oven baking is put into, bakes temperature：160 DEG C,
Baking 30 minutes, the raw material moisture after drying are less than 8%；
3）Extraction：Industrial hemp floral leaf raw material after drying is put into fermentation vat by pipeline, is 1 by weight ratio:1 raw material
Mixed with solvent, be sufficiently stirred, at room temperature constant temperature extracting at least two hour, obtain industrial hemp raw material leaching liquor, leaching liquor leads to
Cross solvent outlet B and enter the first solvent cell, the pipeline that leaching liquor is set by the first solvent cell bottom enters the second solvent cell, steams
Hair removes solvent, obtains semifluid leaching liquor；In addition, solvent by setting respectively at the top of the first solvent cell and the second solvent cell
Solvent vapo(u)r outlet A1 and A2 exported, and pass sequentially through condensation reservoir and volatile oil solvent tank and carry out recycling；
4）Reprocessing：By semifluid leaching liquor by pipeline to tank is stirred by ultrasonic, heating-up temperature is the boiling temperature of solvent,
Minute time 10-15, then add diluent, solid-liquid ratio 1:5, in mass, the hemp leaching liquor diluted, it will dilute
Hemp leaching liquor shaken using ultrasonic agitation tank, the time be 15-30 minutes, supersonic frequency 40KHz, and obtaining being rich in has
Imitate the industrial hemp leaching liquor of composition；
5）Filtering：Industrial hemp leaching liquor is transmitted to butterfly centrifugal machine by pipeline, filtered at room temperature, rotating speed 8000r/min,
Transmitted after filtering by pipeline into the first climbing film evaporator, remove diluent, obtain on-line industry hemp essential oil primary product；
6）Monitoring：On-line industry hemp essential oil primary product is detected by on-line measuring device, it is after detection is qualified that its is defeated
Proportioning tank enters step 7 before delivering to loading, otherwise return to step 5；
7）Loading：Add elution dilution agent, solid-liquid ratio 1:1, in mass, sample obtains sample solution after being completely dissolved, and passes through
The top loading of pipeline extremely pressurization chromatographic silica gel post 10；
8）Chromatography：By the suction-operated for chromatographic silica gel post of pressurizeing, isocratic elution obtains chromatographic solution after 10 hours, and chromatographic solution is led to
Piping is transmitted to flow container is eluted, and the eluant, eluent isolated in chromatography is transmitted molten to the first solvent tank and second successively by pipeline
Agent tank is recycled；
9）Elution：Isocratic elution is carried out to the loading material in pillar using the eluent matched, it is dilute to obtain product after elution
Liquid is released, carries out online HPLC detections, product dilution is distinguished into corresponding solvent tank by Fraction collection according to testing result, its
In, detect qualified product dilution and enter the second climbing film evaporator（13）, otherwise, detect underproof product dilution and enter
Solvent recovery proportioning tank（12）, concentration and isocratic elution again are carried out successively, and solvent recovery recycles；
10）Concentration：In the second climbing film evaporator, temperature 60 C carries out initial concentration, and the product dilution after concentration passes through pipe
Road is delivered to Rotary Evaporators, and temperature is 60-80 DEG C, and operating pressure 0.01MPa-0.03MPa, operating pressure is when draining
0.06-0.08MPa, eluant, eluent is removed completely and obtains the industrial hemp essential oil crude product rich in cannabidiol；
Step（10）In, climbing-film evaporation circulation pipe is provided with second climbing film evaporator, in the climbing-film evaporation circulation pipe
Circulating condensing coolant-temperature gage be 10 DEG C, the eluent recovered liquid in second climbing film evaporator is circulated by the climbing-film evaporation
Pipe carries out circulation concentration, and the eluant, eluent recovered liquid in second climbing film evaporator passes through pipeline to solvent recovery proportioning tank
Recycled；It is provided with rotary evaporation circulation pipe in the Rotary Evaporators, is washed caused by the Rotary Evaporators
De- agent recovered liquid is delivered in solvent recovery tank by rotary evaporation circulation pipe；
11）Finished product：The industrial hemp essential oil crude product of cannabidiol be will be enriched in by pipeline to finished pot, reagent is added, lead to
Cross high pressure elution device and go the removal of impurity, after detection is qualified, labeling, storage, obtain finished product；Extraction equipment, including：Screening washer, bake
Stove, the fermentation vat being sequentially connected by pipeline, the first solvent cell, the second solvent cell, ultrasonic agitation tank, butterfly centrifugal machine, first
Proportioning tank, pressurization chromatographic silica gel post, elution flow container, solvent recovery proportioning tank, the second climbing-film evaporation before climbing film evaporator, loading
Device, Rotary Evaporators and finished pot, in addition to solvent recovery tank, the first solvent tank, the second solvent tank, condensation reservoir and volatile oil are molten
Agent tank, colvent inlet of the fermentation vat including top setting, floral leaf are put into what mouth, solvent vapour outlet A1 and its bottom were set
Steam (vapor) outlet, steam inlet, the floral leaf discharging opening that solvent outlet B and its side wall are set, the fermentation vat pass through solvent outlet B
External first solvent cell, the second solvent cell successively, second solvent cell are internally provided with heating and evaporating unit, and described second
Solvent cell is provided with solvent vapo(u)r outlet A2 at the top of it and leaching liquor outlet is provided with its bottom, the solvent vapo(u)r outlet
The input of A2 connection condensation reservoirs, the input of the output end connection solvent tank of condensation reservoir, the output end connection of the solvent tank
The colvent inlet end of the fermentation vat, the input of the solvent vapour outlet A1 connection condensation reservoirs of the fermentation vat, the pressurization
The top of chromatographic silica gel post sets recovered liquid output end and chromatographic solution output end, the recovered liquid output end is provided with its bottom
The first solvent tank and the second solvent tank are connected respectively and corresponding movable valve is provided with connecting pipe, and the chromatographic solution is defeated
Go out end and connect the elution flow container, the top between first solvent tank and the second solvent tank carries moving valve by setting
Top the carrying by setting of the pipeline connection of door, the top of first solvent tank and the input of the second climbing film evaporator
The pipeline connection of movable valve, the bottom of the output end of second climbing film evaporator connect solvent recovery by pipeline and matched
Tank.
2. the industrial hemp method of extraction of essential oil according to claim 1, it is characterised in that the step（7）In, it is described
Eluant, eluent is petroleum ether and dichloromethane using mass ratio as 6:1 washing lotion mixed, 10 hours of elution time.
3. the industrial hemp method of extraction of essential oil according to claim 1, it is characterised in that step（11）In, the examination
Agent is at least one of n-hexane, ethyl acetate and methanol.
4. the industrial hemp method of extraction of essential oil according to claim 1, it is characterised in that step（3）Described in solvent
For petroleum ether or 6# solvent naphthas.
5. the industrial hemp method of extraction of essential oil according to claim 1, it is characterised in that step（4）Described in dilute
Agent is methanol or absolute ethyl alcohol.
6. industrial hemp method of extraction of essential oil according to claim 1, it is characterised in that the ultrasonic agitation tank, butterfly
Centrifuge, the first climbing film evaporator, pressurization chromatographic silica gel post, the first solvent tank and the second solvent tank input pipeline at be all provided with
Movable valve is equipped with, the pressurization chromatographic silica gel post, is eluted at the pipeline at output of flow container, fluid reservoir and the second climbing film evaporator
It is provided with movable valve.
7. industrial hemp method of extraction of essential oil according to claim 1, it is characterised in that the silica gel pressurizing chromatographic column
Dress post device interior is provided with agitating device, and the agitating device is made up of agitating shaft and stirring vane two parts, the stirring
The upper end of axle is provided with motor, and the control terminal of the motor is connected with air pump, and the stirring vane is installed vertically on the stirring
In the rotary shaft of axle.
8. industrial hemp method of extraction of essential oil according to claim 1, it is characterised in that the solvent recovery proportioning tank is simultaneously
Connection is provided with metering and regards pipe, and the output end of first climbing film evaporator is provided with On-line testing detection means, and the silica gel adds
The output end of pressure chromatographic column is provided with online HPLC detection devices, first climbing film evaporator and the second climbing film evaporator
Evaporation rate is 10 times of common evaporator.
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