CN109646992A - The method of cannabidiol enriched substance is extracted from industrial hemp - Google Patents
The method of cannabidiol enriched substance is extracted from industrial hemp Download PDFInfo
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- CN109646992A CN109646992A CN201910077932.9A CN201910077932A CN109646992A CN 109646992 A CN109646992 A CN 109646992A CN 201910077932 A CN201910077932 A CN 201910077932A CN 109646992 A CN109646992 A CN 109646992A
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- cannabidiol
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0292—Treatment of the solvent
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C37/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring
- C07C37/004—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by obtaining phenols from plant material or from animal material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/005—Selection of auxiliary, e.g. for control of crystallisation nuclei, of crystal growth, of adherence to walls; Arrangements for introduction thereof
- B01D9/0054—Use of anti-solvent
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- Life Sciences & Earth Sciences (AREA)
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Abstract
The present invention discloses a kind of method that cannabidiol enriched substance is extracted from industrial hemp, comprising the following steps: lye extracts, acid precipitating and organic solvent are extracted.Consumption of organic solvent of the present invention is only about the 5% of existing extracting method, and solvent consumption and energy consumption are greatly reduced, relevant device factory investment is greatly decreased, without investing the means of supercritical extraction equipment of large-scale solvent reclaimer facility and workshop or investment price valuableness.The method of the present invention extracts cannabidiol enriched substance, and not only investment cost is few, and operating cost is low, and cannabidiol content height, tetrahydrocannabinol removal rate are high in enriched substance.
Description
Technical field
The present invention relates to a kind of methods for extracting cannabidiol enriched substance, especially a kind of that hemp is extracted from industrial hemp
The method of diphenol enriched substance further relates to the cannabidiol enriched substance that the extracting method obtains, belongs to biological chemical field.
Background technique
Research data show can to obtain from the floral leaf of hemp plant cannabidiol (CBD), tetrahydrocannabinol (THC),
Native compounds, these substances such as cannabinol (CBN), cannabigerol (CBG), cannabichromene (CBC) and terpene all have
Very high medicinal and health value, it is especially the most extensive to the research of cannabidiol, and in safety and effect
Property aspect obtained sufficient affirmative.At present cannabidiol and the cannabis oil rich in cannabidiol have been widely used for drug,
Health care product, cosmetics and food etc., market prospects are boundless, and supply falls short of demand for industrial hemp extract.
The extracting method of cannabidiol has ethanol extraction method, petroleum ether extraction method, supercritical carbon dioxide extraction method at present
With subcritical butane extraction method etc..These methods are primarily present following drawback: 1. equipment purchase costs height, workshop building scale
Greatly, investment cost is high；2. organic solvent consumption is big, energy consumption is high, operating cost is high；3. in crude extract cannabidiol content it is low, four
Hydrogen hemp phenol content removal rate is low, further purifies that difficulty of processing is big, low efficiency.
Summary of the invention
In order to solve the above-mentioned technical problems, the present invention provides a kind of to extract cannabidiol enriched substance from industrial hemp
Method, the method for the present invention investment cost is few, and operating cost is low, and cannabidiol content height, tetrahydrocannabinol content are low in enriched substance.
The present invention is realized by following steps:
A method of extracting cannabidiol enriched substance from industrial hemp, comprising the following steps:
Step (1) lye extracts:
Dry industrial hemp floral leaf raw material is ground into the particle of 8 ~ 100 mesh, with 6~15 times of PH=11 (V/W) of particle quality
~13.5 alkaline aqueous solution extracts 0.5~5 hour, and filtering obtains extracting solution A；
Step (2) acid precipitating:
The acid adding in the extracting solution A of step (1) makes its pH value up to 2.5~5, and precipitating is precipitated, is separated by solid-liquid separation, it is deposited in 100~
It is dried under the conditions of 160 DEG C, obtains precipitating dry product；
Step (3) organic solvent extracts:
The precipitating dry product of step (2) is extracted with the organic solvent of 10~30 times (V/W) of precipitating dry product quality, is obtained extracting solution B, is mentioned
It takes liquid B concentrated, obtains medicinal extract, i.e. cannabidiol enriched substance.
Further, in step (1), the alkaline aqueous solution includes sodium hydroxide, potassium hydroxide, barium hydroxide and ammonium hydroxide
Solution.
Further, in step (1), the extraction, which refers to, impregnates at normal temperature or is stirred in soaking process, mentions
Take the time 0.5~5 hour, speed of agitator is 30 ~ 300r/min.
Further, in step (1), the industrial hemp floral leaf raw material of the drying is the industry dry through natural drying
Cannabis leaf raw material.
Further, in step (2), the acid includes hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, glacial acetic acid, oxalic acid and citric acid
One of or it is a variety of.
Further, in step (3), the organic solvent includes ethyl alcohol, methanol, ethyl acetate, normal hexane and petroleum ether
One of or two kinds or more of mixture.
Further, in step (3), described extract includes diacolation, immersion, stirring or heat reflux, wherein diacolation: flow velocity
Dry product is precipitated for 20 ~ 50ml/min/1kg, the time is 5 ~ 10h；Impregnate: room temperature lower extraction time is not less than 10h；Stirring auxiliary mentions
Take: speed of agitator is 60 ~ 300r/min, and the time is 4 ~ 8h；Circumfluence distillation: the time is 15 ~ 60min.
Compared with prior art, beneficial effects of the present invention are specific as follows:
(1) prior art generally first will carry out sufficiently dry and decarboxylation to raw material, need barn and drying equipment, substantially will
100 DEG C or more dryings, energy consumption is very high.Industrial hemp floral leaf raw material of the invention need only natural drying it is dry, do not generate the above phase
Close investment and operating cost.
(2) solvent for use is expensive during the extraction process for the prior art, and consumption is big, and solvent recovery energy consumption is high, is concentrated back
Receiving unit facility and factory investment are big.The present invention first passes through lye extraction, precipitates using acid, then with minimal amount of organic solvent
It extracts.Consumption of organic solvent is only about the 5% of existing extracting method, and solvent consumption and energy consumption are greatly reduced, are extensive without investment
Solvent reclaimer facility and workshop or investment price valuableness means of supercritical extraction equipment, relevant device factory investment is substantially
It reduces.
(3) the crude extract impurity content of the prior art is high, and cannabidiol content is low, and only 15 ~ 22%, column chromatographs low efficiency,
Need to consume a large amount of eluant, eluents.The method of the present invention extracts cannabidiol enriched substance, and not only investment cost is few, operating cost is low, enrichment
Cannabidiol content is up to 40 ~ 50% in object, and tetrahydrocannabinol is largely removed, and greatly reduces in separating-purifying mistake
The difficulty of tetrahydrocannabinol separation removal in journey.The dosage for greatly reducing eluant, eluent simultaneously improves column chromatography efficiency.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to
Limit the present invention.In the examples where no specific technique or condition is specified, described technology or item according to the literature in the art
Part is carried out according to product description.Reagents or instruments used without specified manufacturer is that can be obtained by purchase
Conventional products.
Embodiment 1
The method that cannabidiol enriched substance is extracted in the slave industrial hemp of the present embodiment, is carried out as follows:
Dry industrial hemp floral leaf raw material is ground into the particle of 50 mesh, 20kg is weighed, is placed in extractor.Addition NaOH
The alkaline solution 160L of the PH of preparation=11.5 is extracted 1 hour under room temperature with 150 r/min stirring, extracting solution is put into acid-regulating tank,
It is slowly added into sulfuric acid under stirring, makes PH=3, is precipitated by centrifuge separation, is dried, obtain under the conditions of being deposited in 60 DEG C
Precipitate dry product 637g.Dry product 7L dehydrated alcohol seepage pressure effects are precipitated, flow velocity 30ml/min/1kg is precipitated under dry product, extraction 5 ~
10h, extracting solution is concentrated, obtains cannabidiol enriched substance 358g.Enriched substance contains cannabidiol 41.3%, only has containing tetrahydrocannabinol
1.41%。
Embodiment 2
The method that cannabidiol enriched substance is extracted in the slave industrial hemp of the present embodiment, is carried out as follows:
Dry industrial hemp floral leaf raw material is ground into the particle of 100 mesh, 20kg is weighed, is placed in extractor.Addition Ba
(OH) extracting solution is put into acid-regulating tank, is stirring soak extraction 3 hours under room temperature by the 2 alkaline solution 200L of PH=12.5 prepared
It is slowly added into glacial acetic acid under state, makes PH=3.5, is centrifuged and is precipitated, is dried under the conditions of being deposited in 100 DEG C, must be precipitated
Dry product 679g.Precipitating dry product, circumfluence distillation, each extraction time are 45min in three times with petroleum ether 13L.Extracting solution passes through
Filter, concentration, obtain cannabidiol enriched substance 326g.Enriched substance contains cannabidiol 42.6%, only has 1.48% containing tetrahydrocannabinol.
Embodiment 3
The method that cannabidiol enriched substance is extracted in the slave industrial hemp of the present embodiment, is carried out as follows:
Dry industrial hemp floral leaf raw material is ground into the particle of 20 mesh, 20kg is weighed, is placed in extractor.Addition KOH
Extracting solution is put into acid-regulating tank by the alkaline solution 280L of the PH of preparation=13 soak extraction 5 hours under room temperature, is delayed under stirring
It is slow that glacial acetic acid is added, make PH=4, is precipitated by centrifuge separation.It is dried under the conditions of being deposited in 150 DEG C, obtains precipitating dry product
852g.Precipitating dry product stirs extraction without ethyl acetate with 10L in three times, and each speed of agitator is 100r/min, extraction time
For 5h, extracting solution is filtered, is concentrated, and obtains cannabidiol enriched substance 349g.Enriched substance contains cannabidiol 43.2%, hemp containing tetrahydro
Phenol only has 1.52%.
Reference examples
Reference examples select ethanol extraction method more mature at present, are carried out as follows:
Industrial hemp floral leaf raw material is 1 hour dry under the conditions of 130 DEG C, it is ground into the particle of 10 ~ 80 mesh, weighs 20kg, is set
In extractor.160L dehydrated alcohol is added, impregnates 4 hours, releases extracting solution, when being concentrated into specific gravity of about 1.08,5L is added
Purified water carries out water and sinks, stands 12 hours, be centrifugated out and precipitate, precipitate drying, obtain medicinal extract 943g after being sufficiently stirred.Leaching
Cream contains cannabidiol 16.2%, contains tetrahydrocannabinol 1.96%.
As it can be seen that the present processes can be obviously improved the content of cannabidiol.
Embodiments of the present invention are not restricted to the described embodiments, other any not violate technical principle of the invention
Changes, modifications, substitutions, combinations, simplifications, it is within the scope of the present invention.
Claims (7)
1. a kind of method for extracting cannabidiol enriched substance from industrial hemp, it is characterised in that: the following steps are included:
Step (1) lye extracts:
Dry industrial hemp floral leaf raw material is ground into the particle of 8 ~ 100 mesh, with 6~15 times of PH=11 (V/W) of particle quality
~13.5 alkaline aqueous solution extracts 0.5~5 hour, and filtering obtains extracting solution A；
Step (2) acid precipitating:
The acid adding in the extracting solution A of step (1) makes its pH value up to 2.5~5, and precipitating is precipitated, is separated by solid-liquid separation, it is deposited in 100~
It is dried under the conditions of 160 DEG C, obtains precipitating dry product；
Step (3) organic solvent extracts:
The precipitating dry product of step (2) is extracted with the organic solvent of 10~30 times (V/W) of precipitating dry product quality, is obtained extracting solution B, is mentioned
It takes liquid B concentrated, obtains medicinal extract, i.e. cannabidiol enriched substance.
2. according to the method described in claim 1, it is characterized by: the alkaline aqueous solution includes hydroxide in step (1)
Sodium, potassium hydroxide, lithium hydroxide, barium hydroxide and ammonia spirit.
3. according to the method described in claim 1, it is characterized by: in step (1), the extraction refer to impregnate at normal temperature or
It is stirred in soaking process, extraction time 0.5~5 hour, speed of agitator is 30 ~ 300r/min.
4. according to the method described in claim 1, it is characterized by: the industrial hemp floral leaf of the drying is former in step (1)
Material is the industrial hemp floral leaf raw material dry through natural drying.
5. according to the method described in claim 1, it is characterized by: in step (2), the acid include hydrochloric acid, sulfuric acid, nitric acid,
One of phosphoric acid, glacial acetic acid, oxalic acid and citric acid are a variety of.
6. according to the method described in claim 1, it is characterized by: in step (3), the organic solvent include ethyl alcohol, methanol,
The mixture of one of ethyl acetate, normal hexane and petroleum ether or two kinds or more.
7. according to the method described in claim 1, it is characterized by: described extract includes diacolation, immersion, stirring in step (3)
Or heat reflux, wherein diacolation: flow velocity is that 20 ~ 50ml/min/1kg precipitates dry product, and the time is 5 ~ 10h；It impregnates: being extracted under room temperature
Time is not less than 10h；Stir assisted extraction: speed of agitator is 60 ~ 300r/min, and the time is 4 ~ 8h；Circumfluence distillation: the time is
15~60min。
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110038251A (en) * | 2019-05-30 | 2019-07-23 | 汉义生物科技（北京）有限公司 | A method of degradation cannboid |
| CN110251987A (en) * | 2019-06-19 | 2019-09-20 | 中国农业科学院麻类研究所 | A kind of extracting method improving cannabidiol content |
| CN111018675A (en) * | 2019-12-10 | 2020-04-17 | 云南罗瑞生物科技有限公司 | Method for efficiently and incrementally extracting cannabidiol |
| WO2020220852A1 (en) * | 2019-04-30 | 2020-11-05 | 云南汉盟制药有限公司 | Method for extracting cannabidiol from cannabis sativa l. |
| WO2020238642A1 (en) * | 2019-05-30 | 2020-12-03 | 汉义生物科技（北京）有限公司 | Inclusion compound containing non-psychoactive cannabinoid and method for preparation thereof |
| WO2021055886A1 (en) * | 2019-09-20 | 2021-03-25 | Beaker Intellectual, Llc | Isolation of cannabinoids from aqueous-extracted phytocannabinoid precipitates |
| CN114680369A (en) * | 2020-12-28 | 2022-07-01 | 云南汉盟制药有限公司 | Industrial hemp extract, preparation method and application |
| CN115504864A (en) * | 2021-06-07 | 2022-12-23 | 南通新世元生物科技有限公司 | Method for obtaining high-purity cannabidiol from industrial cannabis sativa |
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Cited By (9)
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| WO2020220852A1 (en) * | 2019-04-30 | 2020-11-05 | 云南汉盟制药有限公司 | Method for extracting cannabidiol from cannabis sativa l. |
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| CN111018675A (en) * | 2019-12-10 | 2020-04-17 | 云南罗瑞生物科技有限公司 | Method for efficiently and incrementally extracting cannabidiol |
| CN114680369A (en) * | 2020-12-28 | 2022-07-01 | 云南汉盟制药有限公司 | Industrial hemp extract, preparation method and application |
| CN115504864A (en) * | 2021-06-07 | 2022-12-23 | 南通新世元生物科技有限公司 | Method for obtaining high-purity cannabidiol from industrial cannabis sativa |
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