CN104277917A - Extraction method and extraction device for cannabidiol-enriched industrial hemp essential oil - Google Patents
Extraction method and extraction device for cannabidiol-enriched industrial hemp essential oil Download PDFInfo
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- CN104277917A CN104277917A CN201410574240.2A CN201410574240A CN104277917A CN 104277917 A CN104277917 A CN 104277917A CN 201410574240 A CN201410574240 A CN 201410574240A CN 104277917 A CN104277917 A CN 104277917A
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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
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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
- C11B9/025—Recovery by solvent extraction
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Abstract
The invention discloses an extraction method and an extraction device for cannabidiol-enriched industrial hemp essential oil. By adopting devices such as a screening machine, an oven, a soaking tank, a rotary evaporator, an ultrasonic agitation tank, a butterfly centrifuge, a first climbing-film evaporator, a proportioning tank, a pressurized chromatography silica gel column, an eluate tank, a second climbing-film evaporator, a rotary evaporator, a finished product tank and a solvent recovery tank which are sequentially connected by virtue of pipelines, industrial hemps are stepwise subjected to the operation steps comprising screening, baking, extracting, re-treating, filtering, monitoring, sampling, chromatography and concentrating to obtain the finished product and the effective component cannabidiol-enriched industrial hemp essential oil is finally extracted. By virtue of the extraction device disclosed by the invention, the defects of low efficiency, large consumption and inconvenience in scale production of the conventional process are overcome, the semi-finished product containing tetrahydrocannabinol in the processing does not artificially contact and flow, is legal, safe and efficient, the process method is simple and can be easily promoted and the product has high purity, complete active ingredients and low cost.
Description
Technical field
The present invention relates to field of plant extraction, particularly relate to a kind of extracting method being rich in the industrial hemp essential oil of cannabidiol, also relate to manufacturing simultaneously and be rich in the extraction equipment used in the industrial hemp extraction of essential oil process of cannabidiol.
Background technology
At present, the extracting mode that the extracting method of industrial hemp essential oil mainly adopts organic solvent to soak, because extract component is included in its histocyte, the periphery of cell is one deck Mierocrystalline cellulose, the cell walls of the material such as hemicellulose and pectin composition, it is protoplasma in cell walls, passing through in preprocessing process is heated, operation such as ultrasonic grade, destroy plasmic physiological function, the effective constituent in industrial hemp cell and other soluble substance is made to penetrate into outside cell, so, isolate the effective constituent needed for us, must further by the method for chromatography, obtain the industrial hemp essential oil being rich in cannabidiol, because industrial hemp includes drug ingredient tetrahydrocannabinol, make the extraction process of industrial hemp essential oil and flow process must meet the every provisions of laws and regulations of China, and carry out fairly development and utilization under the supervision of relevant departments,
Existing extracting method mostly is open now, and existence all in various degree artificially contacts and disturbs, and be unfavorable for security development and the utilization of industrial hemp, and extraction efficiency is low, and power consumption is large, is also unfavorable for the large-scale production of industrial hemp and promotes on a large scale.
Summary of the invention
The technical problem that the present invention mainly solves is to provide a kind of the industrial hemp method of extraction of essential oil and the extraction equipment thereof that are rich in cannabidiol, by adopt in a device multiple movable valve arrange can effectively, safety, fully recycle is carried out to resource, also the possibility of artificial contact product is in process of production reduced, safely, efficiently.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is: provide a kind of industrial hemp method of extraction of essential oil being rich in cannabidiol, comprise following extraction step:
1) screen: the industrial hemp floral leaf chosen is screened, wherein mouldy, rotten part is chosen, carry out playing powder, dedusting, form industrial hemp floral leaf raw material;
2) toast: the industrial hemp floral leaf raw material after screening is laid in baking pan, put into baking oven baking, roasting temperature: 160 DEG C, toast 30 minutes, the raw material moisture after oven dry is lower than 8%;
3) lixiviate: the industrial hemp floral leaf raw material after drying is dropped into fermentation vat by pipeline, be raw material and the solvent of 1:1 by weight ratio, abundant stirring, constant temperature extracting at least 2 hours under room temperature, obtain industrial hemp raw material vat liquor, vat liquor enters the first solvent cell by solvent outlet B, and vat liquor enters the second solvent cell by the pipeline arranged bottom the first solvent cell, evaporative removal solvent, obtains semi-fluid vat liquor; In addition, solvent is exported by solvent vapo(u)r outlet A1 and A2 arranged respectively at the first solvent cell and the second solvent cell top, and carries out recycling by condensation pond and volatile oil solvent tank successively;
4) reprocessing: by semi-fluid vat liquor by Cemented filling to ultrasonic agitation tank, Heating temperature is the boiling temperature of solvent, time 10-15 minute, then adds thinner, and solid-liquid ratio is 1:5, in mass, obtain the hemp vat liquor diluted, adopt ultrasonic agitation tank to shake the hemp vat liquor of dilution, the time is 15-30 minute, ultrasonic frequency is 40KHz, obtains the industrial hemp vat liquor being rich in effective constituent;
5) filter: industrial hemp vat liquor is transferred to butterfly centrifugal machine by pipeline, filtered at room temperature, rotating speed 8000r/min, transfer in the first climbing-film evaporator by pipeline after filtration, remove thinner, obtain on-line industry hemp essential oil primary product;
6) monitor: on-line industry hemp essential oil primary product is detected by on-line measuring device, detect qualified after be delivered to loading before proportioning tank enter step 7, otherwise return step 5;
7) loading: add eluent dilution, solid-liquid ratio is 1:1, and in mass, wash-out also obtains loading elutriant, the loading elutriant after dilution by Cemented filling to the top loading of pressurization chromatography silicagel column;
8) chromatography: by the adsorption of pressurization chromatography silicagel column, isocratic elution obtained product diluent after 10 hours, and product diluent is transferred to corresponding container for storing liquid by pipeline; The eluent separated in chromatography transfers to the first solvent tank successively by pipeline and the second solvent tank is recycled;
9) wash-out: utilize the elutriant that proportioning is good to carry out isocratic elution to the loading material in pillar, product diluent is obtained after wash-out, by carrying out online HPLC detection, according to detected result, product diluent is distinguished fraction collection in corresponding solvent tank, wherein, detect qualified product diluent and enter the second climbing-film evaporator 13, otherwise, detect underproof product diluent and enter solvent recuperation proportioning tank 12, carry out concentrated and again isocratic elution successively, solvent recuperation recycles;
10) concentrated: in the second climbing-film evaporator, temperature 60 C, carry out initial concentration, product diluent after concentrated by Cemented filling to Rotary Evaporators, temperature is 60-80 DEG C, operating pressure 0.01MPa-0.03MPa, when draining, operating pressure is 0.06-0.08MPa, removes eluent completely and obtains the industrial hemp essential oil crude product being rich in cannabidiol;
11) finished product: by be rich in cannabidiol industrial hemp essential oil crude product by Cemented filling to finished pot, add reagent, remove impurity by high pressure elution device, detect qualified after, labeling, warehouse-in, obtain finished product.
In a preferred embodiment of the present invention, in described step (7), described eluent is sherwood oil and methylene dichloride take mass ratio as the washing lotion that 6:1 carries out mixing, elution time 10 hours.
In a preferred embodiment of the present invention, in step (10), climbing-film evaporation circulation tube is provided with in described second climbing-film evaporator, circulating condensing water temp in described climbing-film evaporation circulation tube is 10 DEG C, elutriant Ethylene recov in described second climbing-film evaporator carries out circulation by described climbing-film evaporation circulation tube and concentrates, and the eluent Ethylene recov in described second climbing-film evaporator is recycled to solvent recuperation proportioning tank by Cemented filling; In described Rotary Evaporators, be provided with rotary evaporation circulation tube, the eluent Ethylene recov produced in described Rotary Evaporators is delivered in described solvent recovery tank by rotary evaporation circulation tube.
In a preferred embodiment of the present invention, in step (11), described reagent is at least one in normal hexane, ethyl acetate and methyl alcohol.
In a preferred embodiment of the present invention, solvent described in step (3) be in sherwood oil or 6# solvent oil any one.
In a preferred embodiment of the present invention, described in step (4), thinner is methyl alcohol or dehydrated alcohol.
A kind of extraction equipment is also provided, comprises: screening washer, baking oven, by the fermentation vat that pipeline is connected successively, first solvent cell, second solvent cell, ultrasonic agitation tank, butterfly centrifugal machine, first climbing-film evaporator, proportioning tank before loading, pressurization chromatography silicagel column, wash-out flow container, solvent recuperation proportioning tank, second climbing-film evaporator, Rotary Evaporators and finished pot, also comprise solvent recovery tank, first solvent tank, second solvent tank, condensation pond and volatile oil solvent tank, described fermentation vat comprises the colvent inlet that top is arranged, floral leaf puts into mouth, the vapour outlet that solvent vapour outlet A1 and the solvent outlet B arranged bottom it and its sidewall are arranged, steam-in, floral leaf discharge port, described fermentation vat is by solvent outlet B external first solvent cell successively, second solvent cell, the inside of described second solvent cell is provided with heating and evaporating unit, described second solvent cell is provided with solvent vapo(u)r outlet A2 and bottom it, is provided with vat liquor outlet at its top, described solvent vapo(u)r outlet A2 connects the input terminus in condensation pond, the output terminal in condensation pond connects the input terminus of solvent tank, the output terminal of described solvent tank connects the colvent inlet end of described fermentation vat, the solvent vapour outlet A1 of described fermentation vat connects the input terminus in condensation pond, the top of described pressurization chromatography silicagel column arranges Ethylene recov output terminal and bottom it, is provided with chromatographic solution output terminal, described Ethylene recov output terminal connects the first solvent tank and the second solvent tank respectively and on connecting tube, is provided with corresponding movable valve, described chromatographic solution output terminal connects described wash-out flow container, top between described first solvent tank and the second solvent tank is connected by the pipeline with movable valve arranged, the top of described first solvent tank is connected by the pipeline with movable valve arranged with the top of the input terminus of the second climbing-film evaporator, the bottom of the output terminal of described second climbing-film evaporator connects solvent recuperation proportioning tank by pipeline.
In a preferred embodiment of the present invention, the input terminus pipeline place of described ultrasonic agitation tank, butterfly centrifugal machine, the first climbing-film evaporator, pressurize chromatography silicagel column, the first solvent tank and the second solvent tank is provided with movable valve, and the pipeline at output place of described pressurization chromatography silicagel column, wash-out flow container, container for storing liquid and the second climbing-film evaporator is provided with movable valve.
In a preferred embodiment of the present invention, the dress post device interior of described silica gel pressurizing chromatographic column is provided with whipping appts, described whipping appts is made up of stir shaft and agitating vane two portions, the upper end of described stir shaft is provided with motor, the control end of described motor is connected with air pump, and described agitating vane is installed vertically on the rotation axis of described stir shaft.
In a preferred embodiment of the present invention, described solvent recuperation proportioning tank has been arranged in parallel metering and has looked pipe, the output terminal of described first climbing-film evaporator is provided with on-line measuring device, the output terminal of described silica gel pressurizing chromatographic column is provided with online HPLC test set, and the vaporator rate of described first climbing-film evaporator and the second climbing-film evaporator is all 10 times of common vaporizer.
The invention has the beneficial effects as follows: a kind of industrial hemp method of extraction of essential oil and the flower of extraction equipment by utilizing hemp discarded thereof being rich in cannabidiol of the present invention, leaf is main raw material, and supporting special extraction equipment carries out the abundant extraction of effective constituent to hemp, extraction equipment used enters each production link, exit is all set to Cemented filling, and be provided with the control of corresponding movable valve, thoroughly stop artificial participation, while the security guaranteeing the whole technical process of the industrial hemp extraction of essential oil being rich in cannabidiol and standardization, also improve the purity of product.
Accompanying drawing explanation
In order to be illustrated more clearly in the technical scheme in the embodiment of the present invention, below the accompanying drawing used required in describing embodiment is briefly described, apparently, accompanying drawing in the following describes is only some embodiments of the present invention, for those of ordinary skill in the art, under the prerequisite not paying creative work, other accompanying drawing can also be obtained according to these accompanying drawings, wherein:
Fig. 1 is a kind of process flow diagram being rich in the industrial hemp method of extraction of essential oil of cannabidiol and a preferred embodiment of extraction equipment and equipment thereof thereof of the present invention;
Fig. 2 is the process flow diagram of lixiviate step in the present invention.
In accompanying drawing, the mark of each parts is as follows: 1, condensation pond, and 2, volatile oil solvent tank, 3, fermentation vat, 4, the first solvent cell, the 5, second solvent cell, 6, ultrasonic agitation tank, 7, butterfly centrifugal machine, the 8, first climbing-film evaporator, 9, proportioning tank before loading, 10, pressurize chromatography silicagel column, and 11, wash-out flow container, 12, solvent recuperation proportioning tank, 13, the second climbing-film evaporator, 14, Rotary Evaporators, 15, finished pot, 16, solvent recovery tank, the 17, first solvent tank, the 18, second solvent tank.
Embodiment
Be clearly and completely described to the technical scheme in the embodiment of the present invention below, obviously, described embodiment is only a part of embodiment of the present invention, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making other embodiments all obtained under creative work prerequisite, belong to the scope of protection of the invention.
Refer to Fig. 1 and Fig. 2, the embodiment of the present invention comprises:
Be rich in an industrial hemp method of extraction of essential oil for cannabidiol, comprise following extraction step:
1) screen: the industrial hemp floral leaf chosen is screened, wherein mouldy, rotten part is chosen, carry out playing powder, dedusting, form industrial hemp floral leaf raw material;
2) toast: the industrial hemp floral leaf raw material after screening is laid in baking pan, put into baking oven baking, roasting temperature: 160 DEG C, toast 30 minutes, the raw material moisture after oven dry is lower than 8%.
3) lixiviate: the industrial hemp floral leaf raw material after drying is dropped into fermentation vat 3 by pipeline, be raw material and the solvent of 1:1 by weight ratio, abundant stirring, constant temperature extracting at least 2 hours under room temperature, obtain industrial hemp raw material vat liquor, vat liquor enters the first solvent cell 4 by solvent outlet B, and vat liquor enters the second solvent cell 5 by the pipeline arranged bottom the first solvent cell 4, evaporative removal solvent, obtains semi-fluid vat liquor; In addition, solvent is exported by solvent vapo(u)r outlet A1 and A2 arranged respectively at the first solvent cell 4 and the second solvent cell 5 top, and carries out recycling by condensation pond 1 and volatile oil solvent tank 2 according to this; Described solvent is sherwood oil or 6# solvent oil;
4) reprocessing: by semi-fluid vat liquor by Cemented filling to ultrasonic agitation tank 6, Heating temperature is the boiling temperature of solvent, time 10-15 minute, then adds thinner, and solid-liquid ratio is 1:5, in mass, obtain the hemp vat liquor diluted, adopt ultrasonic agitation tank 6 to shake the hemp vat liquor of dilution, the time is 15-30 minute, ultrasonic frequency is 40KHz, obtains the industrial hemp vat liquor being rich in effective constituent; Described thinner is methyl alcohol or dehydrated alcohol;
5) filter: industrial hemp vat liquor is transferred to butterfly centrifugal machine 7 by pipeline, filtered at room temperature, rotating speed 8000r/min, transfer in the first climbing-film evaporator 8 by pipeline after filtration, remove thinner, obtain on-line industry hemp essential oil primary product;
6) monitor: on-line industry hemp essential oil primary product is detected by on-line measuring device, detect qualified after be delivered to loading before proportioning tank 9 enter step 7, otherwise return step 5;
7) loading: add eluent dilution, solid-liquid ratio is 1:1, in mass, obtains sample solution after sample dissolves completely, the top loading of the chromatography silicagel column 10 that extremely pressurizeed by Cemented filling;
8) chromatography: by the adsorption of pressurization chromatography silicagel column 10, isocratic elution obtains chromatographic solution in 10 hours, chromatographic solution is transferred to wash-out flow container 11 by pipeline, and in chromatography, isolated eluent transfers to the first solvent tank 17 successively by pipeline and the second solvent tank 18 is recycled; Described eluent is sherwood oil and methylene dichloride take mass ratio as the washing lotion that 6:1 carries out mixing, elution time 10 hours;
9) wash-out: utilize the elutriant that proportioning is good to carry out isocratic elution to the loading material in pillar, product diluent is obtained after wash-out, carry out online HPLC detection, according to detected result, product diluent is distinguished fraction collection in corresponding solvent tank, wherein, detect qualified product diluent and enter the second climbing-film evaporator 13, otherwise, detect underproof product diluent and enter solvent recuperation proportioning tank 12, carry out concentrated and again isocratic elution successively, solvent recuperation recycles;
10) concentrated: in the inside of the second climbing-film evaporator 13, temperature 60 C, carry out initial concentration, product diluent after concentrated by Cemented filling to Rotary Evaporators 14, temperature is 60-80 DEG C, operating pressure 0.01MPa-0.03MPa, when draining, operating pressure is 0.06-0.08MPa, removes eluent completely and obtains the industrial hemp essential oil crude product being rich in cannabidiol; Climbing-film evaporation circulation tube is provided with in described second climbing-film evaporator 13, circulating condensing water temp in described climbing-film evaporation circulation tube is 10 DEG C, elutriant Ethylene recov in described second climbing-film evaporator 13 carries out circulation by described climbing-film evaporation circulation tube and concentrates, and the eluent Ethylene recov in described second climbing-film evaporator 13 is recycled to solvent recuperation proportioning tank 12 by Cemented filling; In described Rotary Evaporators 14, be provided with rotary evaporation circulation tube, the eluent Ethylene recov produced in described Rotary Evaporators 14 is delivered in described solvent recovery tank 16 by rotary evaporation circulation tube;
11) finished product: by be rich in cannabidiol industrial hemp essential oil crude product by Cemented filling to finished pot 15, add reagent, remove impurity by high pressure elution device, detect qualified after, labeling, warehouse-in, obtain finished product; Described reagent is at least one in normal hexane, ethyl acetate and methyl alcohol.
A kind of extraction equipment is also provided, comprise: proportioning tank 9, pressurization chromatography silicagel column 10, wash-out flow container 11, solvent recuperation proportioning tank 12, second climbing-film evaporator 13, Rotary Evaporators 14 and finished pot 15 before screening washer, baking oven, fermentation vat 3, first solvent cell 4, second solvent cell 5 be connected successively by pipeline, ultrasonic agitation tank 6, butterfly centrifugal machine 7, first climbing-film evaporator 8, loading, also comprise solvent recovery tank 16, first solvent tank 17, second solvent tank 18, condensation pond 1 and volatile oil solvent tank 2.
Described fermentation vat 3 comprises the colvent inlet that top is arranged, floral leaf puts into mouth, the vapour outlet that solvent vapour outlet A1 and the solvent outlet B arranged bottom it and its sidewall are arranged, steam-in, floral leaf discharge port, described fermentation vat 3 is by solvent outlet B external first solvent cell 4 successively, second solvent cell 5, the inside of described second solvent cell 5 is provided with heating and evaporating unit, described second solvent cell 5 is provided with solvent vapo(u)r outlet A2 and bottom it, is provided with vat liquor outlet at its top, described solvent vapo(u)r outlet A2 connects the input terminus in condensation pond 1, the output terminal in condensation pond 1 connects the input terminus of solvent tank, the output terminal of described solvent tank connects the colvent inlet end of described fermentation vat 3, the solvent vapour outlet A1 of described fermentation vat 3 connects the input terminus in condensation pond 1, see Fig. 2.
The top of described pressurization chromatography silicagel column 10 arranges Ethylene recov output terminal and bottom it, is provided with chromatographic solution output terminal, described Ethylene recov output terminal connects the first solvent tank 17 and the second solvent tank 18 respectively and on connecting tube, is provided with corresponding movable valve, described chromatographic solution output terminal connects described wash-out flow container 11, top between described first solvent tank 17 and the second solvent tank 18 is connected by the pipeline with movable valve arranged, the top of described first solvent tank 17 is connected by the pipeline with movable valve arranged with the top of the input terminus of the second climbing-film evaporator 13, the bottom of the output terminal of described second climbing-film evaporator 13 connects solvent recuperation proportioning tank 12 by pipeline, see Fig. 1.
The input terminus pipeline place of described ultrasonic agitation tank 6, butterfly centrifugal machine 7, first climbing-film evaporator 8, pressurize chromatography silicagel column 10, first solvent tank 17 and the second solvent tank 18 is provided with movable valve, and the pipeline at output place of described pressurization chromatography silicagel column 10, wash-out flow container 11, container for storing liquid and the second climbing-film evaporator 13 is provided with movable valve.
The dress post device interior of described silica gel pressurizing chromatographic column is provided with whipping appts, described whipping appts is made up of stir shaft and agitating vane two portions, the upper end of described stir shaft is provided with motor, the control end of described motor is connected with air pump, and described agitating vane is installed vertically on the rotation axis of described stir shaft.
Described solvent recuperation proportioning tank 12 has been arranged in parallel metering and has looked pipe, the output terminal of described first climbing-film evaporator 8 is provided with on-line measuring device, the output terminal of described silica gel pressurizing chromatographic column is provided with online HPLC test set, and the vaporator rate of described first climbing-film evaporator 8 and the second climbing-film evaporator 13 is all 10 times of common vaporizer.
Specific embodiment:
Go out vat liquor flow process: (see figure 2)
Industrial hemp floral leaf raw material after baking enters fermentation vat 3 by dog-house, fermentation vat 3 adds the 6# solvent oil dosage of regulation by its colvent inlet, soak at room temperature more than 2 hours, the first solvent cell 4 and the second solvent cell 5 is entered successively by solvent outlet B, in the second solvent cell 5, utilize steam-heated method to remove most of 6# solvent oil, obtain industrial hemp raw material vat liquor, 6# solvent oil is reclaimed and recycle by condensation pond 1 and volatile oil solvent tank 2 successively, repeatedly can input in fermentation vat 3 and use.
Go out industrial hemp essential oil schema: (see figure 1)
Industrial hemp raw material vat liquor enters ultrasonic agitation tank 6 by vat liquor entrance, add the remaining 6# solvent of heat abstraction, add dehydrated alcohol, ultrasonic oscillation process more than 15 minutes, butterfly centrifugal machine 7 is utilized to filter the industrial hemp extracting solution obtaining being rich in effective constituent, extracting solution enters climbing-film evaporator by pipeline, on-line industry hemp essential oil primary product is obtained after reconcentration, this primary product enters proportioning tank 9 before loading by pipeline, after actual applied sample amount proportioning, by Cemented filling in pressurization chromatography silicagel column 10, the elutriant that proportioning is good is utilized to carry out isocratic elution to loading material, product diluent is obtained by the sorption and desorption effect wash-out of silica gel, product diluent is by HPLC on-line checkingi, according to detected result, by product diluent difference fraction collection in corresponding solvent tank, wherein, detect qualified product diluent and be transported to the second climbing-film evaporator 13 successively by pipeline, otherwise, detect underproof product diluent and be delivered to solvent recuperation proportioning tank 12, carry out concentrated and isocratic elution again successively,
In the second climbing-film evaporator 13, temperature 60 C, carry out initial concentration, product diluent after concentrated by Cemented filling to Rotary Evaporators 14, temperature is about 70 DEG C, about operating pressure 0.02MPa, when draining, operating pressure is about 0.07MPa, removes eluent completely and obtains the industrial hemp essential oil crude product being rich in cannabidiol; Industrial hemp essential oil crude product to finished pot 15, adds reagent by Cemented filling, by high pressure elution device remove tetrahydrocannabinol, detect qualified after, labeling, warehouse-in, obtain finished product;
Wherein, in the chromatography process of pressurization chromatography silicagel column 10, isolated eluent transfers to the first solvent tank 17 respectively by pipeline and the second solvent tank 18 is recycled; In the second climbing-film evaporator 13, evaporate the eluent condensation obtained and transfer to the first solvent tank 17 by pipeline, can recycle again.
In sum, the development of deep processing to China's industrial hemp industry of being rich in the extract of the industrial hemp of cannabidiol has immeasurable effect, can improve the added value of China's this pollution-free industry of industrial hemp further; The flower discarded with industrial hemp and leaf make raw material, adopt modern science and technology technology, turn waste into wealth, benefit common people; Plant standardized extract is the novel high-tech product having merged modern pharmaceutical technology and biochemical technology, is also the new variety of occupying inter-national market in recent years, processing stage and scientific and technological content higher; Life science to the development mankind, health science, nutrition science, medical science are produced far-reaching influence by industrial hemp essential oil, are also that common people pursue, international economy development new highlight; The exploitation of industrial hemp will make full use of resources advantage, adopt scientific and technological new technology, and meet GAP, GMP require under produce, adopt technique and the quality detection technology of above-mentioned advanced person simultaneously, the effective constituent of industrial hemp floral leaf extract is maximized, tetrahydrocannabinol content meet country and European Union regulation be less than 0.3%; Industrial hemp essential oil is the deep processing to industrial hemp resource, has exploitation advantage and the features such as less input, with high content of technology, added value of product is large, world market is extensive.
The beneficial effect of the present invention a kind of the industrial hemp method of extraction of essential oil and extraction equipment thereof that are rich in cannabidiol is:
One, the invention has the beneficial effects as follows: whole technical process realizes omnidistance totally closed operation, avoid artificial in production process participation and interference to greatest extent, ensure whole production process Raw into and out of all realizing mechanize, guarantee the fairly development and utilization of industrial hemp, links all meets every provisions of laws and regulations of China and the world;
Two, administer with common contaminated soil and compare with recovery technique, this technological process apparatus is advanced, efficient, safety, drastically increase the content of effective constituent in industrial hemp floral leaf raw material, and effective constituent is complete after extracting, secondly whole production technique is clear and coherent, smooth, efficiency is high, equipment obtains comparatively easy, is convenient to promote.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every utilize description of the present invention to do equivalent structure or equivalent flow process conversion; or be directly or indirectly used in other relevant technical field, be all in like manner included in scope of patent protection of the present invention.
Claims (10)
1. be rich in an industrial hemp method of extraction of essential oil for cannabidiol, it is characterized in that, comprise following extraction step:
1 screening: screen the industrial hemp floral leaf chosen, chooses wherein mouldy, rotten part, carries out playing powder, dedusting, forms industrial hemp floral leaf raw material;
2 bakings: the industrial hemp floral leaf raw material after screening is laid in baking pan, put into baking oven baking, roasting temperature: 160 DEG C, toast 30 minutes, the raw material moisture after oven dry is lower than 8%;
3 lixiviates: the industrial hemp floral leaf raw material after drying is dropped into fermentation vat by pipeline, be raw material and the solvent of 1:1 by weight ratio, abundant stirring, constant temperature extracting at least 2 hours under room temperature, obtain industrial hemp raw material vat liquor, vat liquor enters the first solvent cell by solvent outlet B, and vat liquor enters the second solvent cell by the pipeline arranged bottom the first solvent cell, evaporative removal solvent, obtains semi-fluid vat liquor; In addition, solvent is exported by solvent vapo(u)r outlet A1 and A2 arranged respectively at the first solvent cell and the second solvent cell top, and carries out recycling by condensation pond and volatile oil solvent tank successively;
4 reprocessing: by semi-fluid vat liquor by Cemented filling to ultrasonic agitation tank, Heating temperature is the boiling temperature of solvent, time 10-15 minute, then adds thinner, and solid-liquid ratio is 1:5, in mass, obtain the hemp vat liquor diluted, adopt ultrasonic agitation tank to shake the hemp vat liquor of dilution, the time is 15-30 minute, ultrasonic frequency is 40KHz, obtains the industrial hemp vat liquor being rich in effective constituent;
5 filter: industrial hemp vat liquor is transferred to butterfly centrifugal machine by pipeline, filtered at room temperature, rotating speed 8000r/min, transfer in the first climbing-film evaporator after filtration by pipeline, remove thinner, obtain on-line industry hemp essential oil primary product;
6 monitorings: on-line industry hemp essential oil primary product is detected by on-line measuring device, detect qualified after be delivered to loading before proportioning tank enter step 7, otherwise return step 5;
7 loadings: add eluent dilution, solid-liquid ratio is 1:1, in mass, obtains sample solution after sample dissolves completely, the top loading of the chromatography silicagel column 10 that extremely pressurizeed by Cemented filling;
8 chromatographies: by the adsorption of pressurization chromatography silicagel column, isocratic elution obtained chromatographic solution after 10 hours, chromatographic solution is transferred to wash-out flow container by pipeline, and in chromatography, isolated eluent transfers to the first solvent tank successively by pipeline and the second solvent tank is recycled;
9 wash-outs: utilize the elutriant that proportioning is good to carry out isocratic elution to the loading material in pillar, product diluent is obtained after wash-out, carry out online HPLC detection, according to detected result, product diluent is distinguished fraction collection in corresponding solvent tank, wherein, detect qualified product diluent and enter the second climbing-film evaporator 13, otherwise, detect underproof product diluent and enter solvent recuperation proportioning tank 12, carry out concentrated and again isocratic elution successively, solvent recuperation recycles;
10 concentrate: in the second climbing-film evaporator, temperature 60 C, carry out initial concentration, product diluent after concentrated by Cemented filling to Rotary Evaporators, temperature is 60-80 DEG C, operating pressure 0.01MPa-0.03MPa, when draining, operating pressure is 0.06-0.08MPa, removes eluent completely and obtains the industrial hemp essential oil crude product being rich in cannabidiol;
11 finished products: by be rich in cannabidiol industrial hemp essential oil crude product by Cemented filling to finished pot, add reagent, remove impurity by high pressure elution device, detect qualified after, labeling, warehouse-in, obtain finished product.
2. according to the industrial hemp method of extraction of essential oil described in claim 1, it is characterized in that, in described step (7), described eluent is sherwood oil and methylene dichloride take mass ratio as the washing lotion that 6:1 carries out mixing, elution time 10 hours.
3. the industrial hemp method of extraction of essential oil according to claim 1 or 2, it is characterized in that, in step (10), climbing-film evaporation circulation tube is provided with in described second climbing-film evaporator, circulating condensing water temp in described climbing-film evaporation circulation tube is 10 DEG C, elutriant Ethylene recov in described second climbing-film evaporator carries out circulation by described climbing-film evaporation circulation tube and concentrates, and the eluent Ethylene recov in described second climbing-film evaporator is recycled to solvent recuperation proportioning tank by Cemented filling; In described Rotary Evaporators, be provided with rotary evaporation circulation tube, the eluent Ethylene recov produced in described Rotary Evaporators is delivered in described solvent recovery tank by rotary evaporation circulation tube.
4. according to the industrial hemp method of extraction of essential oil described in claim 1, it is characterized in that, in step (11), described reagent is at least one in normal hexane, ethyl acetate and methyl alcohol.
5., according to the industrial hemp method of extraction of essential oil described in claim 1, it is characterized in that, solvent described in step (3) be in sherwood oil or 6# solvent oil any one.
6. according to the industrial hemp method of extraction of essential oil described in claim 1, it is characterized in that, described in step (4), thinner is methyl alcohol or dehydrated alcohol.
7. an extraction equipment, is characterized in that, comprising: screening washer, baking oven, by the fermentation vat that pipeline is connected successively, first solvent cell, second solvent cell, ultrasonic agitation tank, butterfly centrifugal machine, first climbing-film evaporator, proportioning tank before loading, pressurization chromatography silicagel column, wash-out flow container, solvent recuperation proportioning tank, second climbing-film evaporator, Rotary Evaporators and finished pot, also comprise solvent recovery tank, first solvent tank, second solvent tank, condensation pond and volatile oil solvent tank, described fermentation vat comprises the colvent inlet that top is arranged, floral leaf puts into mouth, the vapour outlet that solvent vapour outlet A1 and the solvent outlet B arranged bottom it and its sidewall are arranged, steam-in, floral leaf discharge port, described fermentation vat is by solvent outlet B external first solvent cell successively, second solvent cell, the inside of described second solvent cell is provided with heating and evaporating unit, described second solvent cell is provided with solvent vapo(u)r outlet A2 and bottom it, is provided with vat liquor outlet at its top, described solvent vapo(u)r outlet A2 connects the input terminus in condensation pond, the output terminal in condensation pond connects the input terminus of solvent tank, the output terminal of described solvent tank connects the colvent inlet end of described fermentation vat, the solvent vapour outlet A1 of described fermentation vat connects the input terminus in condensation pond, the top of described pressurization chromatography silicagel column arranges Ethylene recov output terminal and bottom it, is provided with chromatographic solution output terminal, described Ethylene recov output terminal connects the first solvent tank and the second solvent tank respectively and on connecting tube, is provided with corresponding movable valve, described chromatographic solution output terminal connects described wash-out flow container, top between described first solvent tank and the second solvent tank is connected by the pipeline with movable valve arranged, the top of described first solvent tank is connected by the pipeline with movable valve arranged with the top of the input terminus of the second climbing-film evaporator, the bottom of the output terminal of described second climbing-film evaporator connects solvent recuperation proportioning tank by pipeline.
8. extraction equipment according to claim 7, it is characterized in that, the input terminus pipeline place of described ultrasonic agitation tank, butterfly centrifugal machine, the first climbing-film evaporator, pressurize chromatography silicagel column, the first solvent tank and the second solvent tank is provided with movable valve, and the pipeline at output place of described pressurization chromatography silicagel column, wash-out flow container, container for storing liquid and the second climbing-film evaporator is provided with movable valve.
9. extraction equipment according to claim 7, it is characterized in that, the dress post device interior of described silica gel pressurizing chromatographic column is provided with whipping appts, described whipping appts is made up of stir shaft and agitating vane two portions, the upper end of described stir shaft is provided with motor, the control end of described motor is connected with air pump, and described agitating vane is installed vertically on the rotation axis of described stir shaft.
10. extraction equipment according to claim 7, it is characterized in that, described solvent recuperation proportioning tank has been arranged in parallel metering and has looked pipe, the output terminal of described first climbing-film evaporator is provided with On-line testing proofing unit, the output terminal of described silica gel pressurizing chromatographic column is provided with online HPLC test set, and the vaporator rate of described first climbing-film evaporator and the second climbing-film evaporator is all 10 times of common vaporizer.
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