CN112939745A - Separation system and separation method of cannabidiol - Google Patents
Separation system and separation method of cannabidiol Download PDFInfo
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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
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
-
- 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
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
- C07C37/72—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by liquid-liquid treatment
-
- 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
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
- C07C37/82—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by solid-liquid treatment; by chemisorption
-
- 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
- C07C37/68—Purification; separation; Use of additives, e.g. for stabilisation
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
- C07C37/84—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by crystallisation
Abstract
The invention relates to a cannabidiol separation system and a cannabidiol separation method, and belongs to the technical field of cannabidiol separation and purification. A method for separating cannabidiol, comprising the steps of: drying flowers and leaves of industrial hemp, then crushing to obtain crushed slag, adding an extraction solvent, and carrying out countercurrent extraction to obtain an extracting solution; concentrating the extracting solution, adding water for dilution to obtain a diluent, adsorbing the diluent by using a resin column, and eluting by using an eluting solvent to obtain an eluent; concentrating the eluate to obtain crude extract; carrying out reverse chromatography gradient elution on the crude paste to obtain a semi-finished product liquid; concentrating the semi-finished product liquid to obtain a crude product; recrystallizing the crude product, filtering to obtain a filter cake, and drying to obtain the finished product, namely the cannabidiol. The invention also provides a cannabidiol separation system. The separation method has the advantages of simple and convenient operation, mild process conditions, high production efficiency and low production cost.
Description
Technical Field
The invention belongs to the technical field of cannabidiol separation and purification, and particularly relates to a cannabidiol separation system and a cannabidiol separation method.
Background
Cannabidiol (CBD) is the main chemical component in medicinal plant cannabis sativa, is a non-addictive component in cannabis sativa, and has a series of pharmacological actions such as spasm resistance, anxiety resistance, insomnia resistance, vomiting resistance, inflammation resistance, tumor resistance and the like. The FDA has approved its use for the treatment of intractable epilepsy in 2018, and its market demand must be further expanded with the further development of cannabidiol in the fields of medicine, health care, food, cosmetics, etc. in countries around the world.
The production process of cannabidiol is divided into two types of chemical synthesis and natural extraction. Cannabidiol is produced by natural extraction, which mainly uses branches and leaves of cannabis as raw materials, and obtains crude products by different extraction methods after drying and crushing, and then obtains finished products by solvent crystallization, chromatographic separation or other methods for a plurality of times.
Because of the complex components of cannabinol in the cannabis, the purity and yield of the finished products obtained by different methods are different. The tetrahydrocannabinol with side effects can generate certain side effects if the tetrahydrocannabinol with side effects can not be completely removed, so the requirement on the preparation and purification process of cannabidiol is higher.
At present, the existing preparation methods in China are mostly methods in laboratories, and most of the technologies involve the problems of complex process, large equipment investment, high production cost and the like.
For example, a method for purifying cannabidiol by crystallization, which takes a certain content of cannabidiol crude product as raw material, although the purity of the obtained final product is more than 99.5 percent, the content of tetrahydrocannabinol is not more than 0.1 percent, the tetrahydrocannabinol can not be completely removed, so the specific side effect can not meet the requirement.
The method adopts a supercritical argon extraction method to extract hemp branches and leaves, then adopts a molecular distillation method to carry out primary separation, and finally adopts an argon supercritical fluid chromatographic separation method to carry out separation and purification, although the purity of the obtained final product is more than 99.8%, the total yield is more than 94.0%, and the tetrahydrocannabinol is not detected, the method adopts an ultrahigh pressure process, has high requirements on process equipment, needs great equipment cost for enterprises, and has low economic benefit.
For example, a method for extracting purified cannabidiol from hemp. The method adopts supercritical CO2The extraction technology is used for extracting the branches and leaves of the hemp, the cannabidiol extract is further purified by utilizing the macroporous adsorption resin and the rapid purification system, although the content of the obtained final product exceeds 98 percent and the final product does not contain tetrahydrocannabinol, the method also adopts an ultrahigh pressure process, and the purification process adopts forward chromatographic separation with silica gel as a stationary phase, the silica gel is disposable, the cost is high, the requirement on process equipment is high, huge equipment cost is required for enterprises, and the economic benefit is low.
For example, a method for separating and purifying cannabidiol from industrial cannabis sativa leaves. The method adopts an extraction method to extract the hemp branches and leaves, then adopts macroporous resin for adsorption and elution, then adopts silica gel column for forward separation, and finally obtains the final product through preparative chromatography, wherein the purity of the product is over 95 percent. But the product purity is not high, and meanwhile, the process steps are more, the operation is complex, and the practicability is not strong.
Disclosure of Invention
The present invention provides a cannabidiol separation system and a cannabidiol separation method for solving the above technical problems.
In order to solve the above problems, the present invention provides a method for separating cannabidiol.
The technical scheme for solving the technical problems is as follows: a method of separating cannabidiol comprising the steps of:
s1, drying flowers and leaves of industrial hemp, then crushing to obtain crushed slag, and adding an extraction solvent for countercurrent extraction to obtain an extracting solution;
s2, firstly concentrating the extracting solution obtained in the step S1, then adding water for dilution to obtain a diluent, adsorbing the diluent by using a resin column, and then eluting by using an elution solvent to obtain an eluent;
s3, concentrating the eluent obtained in the step S2 to obtain a crude paste;
s4, carrying out reverse chromatography gradient elution on the crude paste obtained in the step S3 to obtain a semi-finished product liquid;
s5, concentrating the semi-finished product liquid obtained in the step S4 to obtain a crude product;
s6, recrystallizing the crude product obtained in the step S5, filtering to obtain a filter cake, and drying to obtain a finished product, namely the cannabidiol.
The separation method of the invention has the beneficial effects that: (1) the separation method has simple operation, mild process conditions, high production efficiency and low production cost;
(2) the yield of cannabidiol prepared by reverse chromatography gradient elution in the separation method is high, the obtained cannabidiol has high purity, and does not contain tetrahydrocannabinol by-products;
(3) the separation method can realize the industrial production of the cannabidiol, can obtain the cannabidiol with high yield, and the annual yield can reach more than 2000 kg.
On the basis of the technical scheme, the invention can be further improved as follows.
Further, in step S1, the drying temperature is 100-200 ℃, and the drying time is 2-6 h; the mesh number of the crushed slag is 5-100 meshes; the temperature of the countercurrent extraction is 30-80 ℃; the extraction solvent is a mixture of any one of methanol, ethanol, petroleum ether and ethyl acetate and water in any proportion; the mass volume ratio of the slag to the solvent is 1: (3-10).
The beneficial effect of adopting the further scheme is that: is beneficial to the extraction operation of the branches and leaves of the hemp and is beneficial to the extraction of effective components.
Further, in step S2, the concentration is performed by vacuum concentration using a vacuum concentration tank; the flow rate of the diluent in the adsorption is 300-1000 ml/min; the elution solvent is ethyl acetate or hexane; the stationary phase in the resin column is one or more of macroporous resin D101, macroporous resin H-103, macroporous resin DM-130, macroporous resin X-5 and macroporous resin XAD-16.
The beneficial effect of adopting the further scheme is that: can improve the purity of the extracted effective components.
Further, in step S3, the concentration is performed by vacuum concentration using a vacuum concentration tank.
The beneficial effect of adopting the further scheme is that: the concentration effect is good.
Further, in step S4, the subjecting the crude paste to reverse chromatography gradient elution comprises the steps of:
s41, adding a solvent into the crude paste for dissolving, adding a stationary phase, uniformly stirring, concentrating to obtain a solid, adding water according to the mass volume ratio of 1 (1-2) to the solid, uniformly stirring, and filling into a column to obtain a separation column;
s42, standing the separation column obtained in the step 41 for 2-6 hours, performing gradient elution by using an eluent, and collecting liquid to obtain semi-finished liquid.
The beneficial effect of adopting the further scheme is that: the cannabidiol is easy to separate and obtain.
Further, in step S41, the adding amount of the stationary phase is 5-20kg per separation column, and the stationary phase is one of macroporous resin PRP-4, macroporous resin PRP-5, macroporous resin PRP-6 and macroporous resin PRP-7.
The beneficial effect of adopting the further scheme is that: the cannabidiol can be eluted easily.
Further, in step S42, the conditions of the reverse chromatography gradient elution are: the eluent is a mixture of water and one of organic solvents of methanol, ethanol, acetone and acetonitrile; the elution gradient was: the volume of the organic solvent of the first gradient accounts for 30-60% of the mixture, the volume of the organic solvent of the second gradient accounts for 60-90% of the mixture, and the volume of the organic solvent of the third gradient accounts for 90-100% of the mixture; the elution volumes were: the first gradient is 2-6 column volumes; the second gradient is 6-10 column volumes; the third gradient is 1-2 column volumes.
The beneficial effect of adopting the further scheme is that: the cannabidiol can be eluted easily.
Further, in step S5, the concentration is performed by vacuum concentration using a vacuum concentration tank.
The beneficial effect of adopting the further scheme is that: can improve the purity of cannabidiol.
Further, in step S6, the solvent used for recrystallization is one of n-hexane, petroleum ether, ethyl acetate and acetonitrile, the dissolving temperature is 30-60 ℃, and the addition amount of the solvent is such that the mass-to-volume ratio of the solvent to the crude product is 1: (10-30); in step S6, the crystallization temperature is-20 ℃ to 5 ℃, and the crystallization time is 4 to 24 hours; in step S6, the drying pressure is-0.05-0.09 Mpa, the drying temperature is 30-60 ℃, and the drying time is 6-24 h.
The beneficial effect of adopting the further scheme is that: the adoption of recrystallization leads to higher purity of cannabidiol.
Secondly, the present invention provides a cannabidiol separation system to solve the above technical problems.
The technical scheme for solving the technical problems is as follows: a cannabidiol separation system comprises a countercurrent extraction device, an elution tower, a chromatographic separation system, a recrystallization tank, a drying device and a finished product tank;
the utility model discloses a drying device, including countercurrent extraction device, elution tower, chromatographic separation system, recrystallization jar, drying device, be equipped with the feed inlet on the countercurrent extraction device, countercurrent extraction device's output with the input of elution tower is connected, the output of elution tower with chromatographic separation system's input is connected, chromatographic separation system's output with the input of recrystallization jar is connected, the output of recrystallization jar with drying device's input is connected, drying device's output with the finished product jar is connected.
The separation system of the invention has the advantages that: (1) the separation system can realize the industrial production of the cannabidiol, can obtain the cannabidiol with high yield, and the annual yield can reach more than 2000 kg;
(2) the cannabidiol produced by the separation system does not have a byproduct of tetrahydrocannabinol, so that the generation of side effects is avoided, and the obtained cannabidiol has high purity and high yield;
(3) the separation system has low equipment manufacturing cost and low cost requirement on enterprises, and is suitable for enterprise application.
Drawings
FIG. 1 is a schematic diagram of the separation system of the present invention.
In the drawings, the components represented by the respective reference numerals are listed below:
1. a countercurrent extraction device; 2. a feed inlet; 3. a first delivery pump; 4. a first concentration tank; 5. an elution column; 6. a second delivery pump; 7. a third delivery pump; 8. preparing a material tank; 9. a fourth delivery pump; 10. a chromatographic separation column; 11. a fifth delivery pump; 12. a second concentration tank; 13. a sixth delivery pump; 14. a recrystallization tank; 15. a seventh delivery pump; 16. a drying device; 17. an eighth delivery pump; 18. a finished product tank; 19. a solvent storage tank; 20. a ninth delivery pump; 21. a liquid mixing tank; 22. a tenth transfer pump; 23. a head tank.
Detailed Description
The principles and features of this invention are described below in conjunction with the following drawings, which are set forth by way of illustration only and are not intended to limit the scope of the invention.
Example 1
As shown in fig. 1, the present embodiment provides a cannabidiol separation system, which includes a countercurrent extraction apparatus 1, an elution column 5, a chromatographic separation system, a recrystallization tank 14, a drying apparatus 16, and a finished product tank 18;
the countercurrent extraction device 1 is provided with a feed inlet 2, the output end of the countercurrent extraction device 1 is connected with the input end of an elution tower 5, the output end of the elution tower 5 is connected with the input end of a chromatographic separation system, the output end of the chromatographic separation system is connected with the input end of a recrystallization tank 14, the output end of the recrystallization tank 14 is connected with the input end of a drying device 16, and the output end of the drying device 16 is connected with a finished product tank 18.
Wherein, the countercurrent extraction device 1 is used for countercurrent extraction to extract the components in the hemp. The elution tower 5 is used for eluting the effective components and improving the yield. The extracted effective components are separated by a chromatographic separation system, and then the needed cannabidiol is separated, so that only cannabidiol is obtained, and tetrahydrocannabinol is not existed. The recrystallization is realized through the arranged recrystallization tank 14, the obtained cannabidiol can be purified, and the purity of the cannabidiol is improved. The drying device 16 is used for drying to obtain dried cannabidiol. Wherein the production capacity of the countercurrent extraction device 1 is 500-2000L/h. The production capacity of the chromatographic separation system was 5-15 kg/batch and 36 h/batch. The recrystallization tank 14 is a device with the volume of 1000-3000L and the operation temperature of-20-100 ℃ with stirring. The drying device 16 is a device with the volume of 500-1000L and the operation temperature of 20-100 ℃ with vacuum.
The technical scheme of the embodiment has the beneficial effects that the separation system can realize industrial production of cannabidiol, can obtain cannabidiol with high yield, and the annual yield can reach more than 2000 kg. The cannabidiol produced by the separation system does not have a byproduct of tetrahydrocannabinol, so that the generation of side effects is avoided, and the obtained cannabidiol has high purity and high yield. The separation system has low equipment manufacturing cost and low cost requirement on enterprises, and is suitable for enterprise application. The invention adopts styrene-divinylbenzene as a framework, different modification groups and macroporous resin with different particle sizes as a single component or a composition as the stationary phase, and water-soluble acetone, methanol and ethanol as a solvent, so that cannabidiol can be effectively separated, and the obtained cannabidiol has high purity.
Preferably, in this embodiment, a first concentration tank 4 is further disposed between the countercurrent extraction device 1 and the elution column 5, an output end of the countercurrent extraction device 1 is connected with an input end of the first concentration tank 4, and an output end of the first concentration tank 4 is connected with an input end of the elution column 5. The obtained extract can be concentrated by the first concentration tank 4. Wherein the first concentrating tank 4 is a vacuum concentrating tank.
Wherein, be equipped with first delivery pump 3 between countercurrent extraction device 1 and the first concentrated jar 4, the input of first delivery pump 3 and the output intercommunication of countercurrent extraction device 1, the output of first delivery pump 3 and the input intercommunication of first concentrated jar 4 can carry the extract in the countercurrent extraction device 1 to first concentrated jar 4 through first delivery pump 3. Be equipped with second delivery pump 6 between first concentrated jar 4 and the elution tower 5, the input of second delivery pump 6 and the output intercommunication of first concentrated jar 4, the output of second delivery pump 6 and the input intercommunication of elution tower 5 can carry the concentrated solution in the first concentrated jar 4 to elution tower 5 through second delivery pump 6 in, elute.
Preferably, in the present embodiment, a plurality of resin columns are disposed in the elution column 5, and the volume of the plurality of resin columns is 500-3000L. The resin column is filled with a stationary phase which is one or more of macroporous resin D101, macroporous resin H-103, macroporous resin DM-130, macroporous resin X-5 and macroporous resin XAD-16.
Preferably, in the present embodiment, the chromatographic separation column 10 includes a preparation tank 8, a chromatographic separation column 10 and a second concentration tank 12, an input end of the preparation tank 8 is connected with an output end of the elution column 5, an output end of the preparation tank 8 is connected with an input end of the chromatographic separation column 10, an output end of the chromatographic separation column 10 is connected with an input end of the second concentration tank 12, and an output end of the second concentration tank 12 is connected with an input end of the recrystallization tank 14.
Wherein the volume of the material preparation tank 8 is 500-1000L, and the material preparation tank is a vacuum reduced pressure concentration tank. The material preparing tank 8 is used for preparing materials to be separated. Wherein the chromatographic separation column 10 has a separation device with an elution function, and can separate and extract the desired cannabidiol. The second concentration tank 12 is used to concentrate the obtained separated liquid to obtain an active ingredient.
Preferably, in the present embodiment, a plurality of separation columns are disposed in the chromatographic separation column 10, and the volume of the plurality of separation columns is 100-200L. The separation column is filled with a separation stationary phase which is any one of macroporous resins PRP-4, PRP-5, PRP-6 and PRP-7. The styrene-divinylbenzene crosslinked copolymer is used as a skeleton, and a monomer or a mixture formed by adding functional groups is added, wherein the particle size is different from 100 meshes to 800 meshes.
Preferably, in the embodiment, a solvent supply system for supplying the solvent to the preparation tank 8 and the chromatographic separation column 10 is further included, and the output end of the solvent supply system is respectively communicated with the preparation tank 8 and the chromatographic separation column 10. The solvent can be supplied to the material preparation tank 8 and the chromatographic separation column 10 by the provided solvent supply system.
Preferably, in the present embodiment, the solvent supply system comprises a solution tank 21 and a head tank 23, an output end of the solution tank 21 is respectively communicated with an input end of the head tank 23 and an input end of the preparation tank 8, and an output end of the head tank 23 is communicated with an input end of the chromatographic separation column 10. The solvent can be mixed by the liquid preparation tank 21, the ratio of the solvent to water can be adjusted, and the device is suitable for targeted elution and separation. The high-level tank 23 is arranged to facilitate the solvent to enter the chromatographic separation tower 10 for separation.
Preferably, a plurality of solvent storage tanks 19 are further included, and output ends of the plurality of solvent storage tanks 19 are respectively connected with input ends of the solution mixing tanks 21. The plurality of solvent tanks 19 are used to store different solvents, and are used as needed.
Wherein, be equipped with third delivery pump 7 between elution tower 5 and the system material jar 8, the input of third delivery pump 7 and the output intercommunication of elution tower 5, the output of third delivery pump 7 and the input intercommunication of the system material jar 8. A fourth delivery pump 9 is arranged between the material preparation tank 8 and the chromatographic separation tower 10, the input end of the fourth delivery pump 9 is communicated with the output end of the material preparation tank 8, and the output end of the fourth delivery pump 9 is communicated with the input end of the chromatographic separation tower 10. And a fifth delivery pump 11 is arranged between the chromatographic separation tower 10 and the second concentration tank 12, the input end of the fifth delivery pump 11 is communicated with the output end of the distribution separation tower, and the output end of the fifth delivery pump 11 is communicated with the input end of the second concentration tank 12. A sixth delivery pump 13 is arranged between the second concentration tank 12 and the recrystallization tank 14, the input end of the sixth delivery pump 13 is communicated with the output end of the second concentration tank 12, and the output end of the sixth delivery pump 13 is communicated with the input end of the recrystallization tank 14. A seventh delivery pump 15 is arranged between the recrystallization tank 14 and the drying device 16, the input end of the seventh delivery pump 15 is communicated with the output end of the recrystallization tank 14, and the output end of the seventh delivery pump 15 is communicated with the input end of the drying device 16. An eighth delivery pump 17 is arranged between the drying device 16 and the finished product tank 18, the input end of the eighth delivery pump 17 is communicated with the output end of the drying device 16, and the output end of the eighth delivery pump 17 is communicated with the finished product tank 18. A ninth delivery pump 20 is arranged between the solvent storage tank 19 and the liquid mixing tank 21, the input end of the ninth delivery pump 20 is communicated with the output end of the solvent storage tank 19, and the output end of the ninth delivery pump 20 is communicated with the input end of the liquid mixing tank 21. A tenth delivery pump 22 is arranged between the liquid mixing tank 21 and the high-level tank 23, the input end of the tenth delivery pump 22 is communicated with the output end of the liquid mixing tank 21, and the output end of the tenth delivery pump 22 is communicated with the input end of the high-level tank 23.
Example 2
This example provides a cannabidiol separation method, which is carried out in practice by using the separation system of example 1 and using the species of branches and leaves as "yunnan 7". In the yunnan 7, the content of CBD (cannabidiol) is 7500ppm, and the content of THC (tetrahydrocannabinol) is 1100 ppm. The separation method comprises the following steps:
s1, taking 100kg of Yuma No. 7 flowers and leaves, drying the flowers and leaves for 2 hours at 150 ℃ by using a hot air circulation oven, then crushing by using an industrial crusher to obtain crushed slag, sieving the crushed slag with a sieve mesh number of 10 meshes to obtain 750g of dried crushed slag, wherein the mass-volume ratio of the dried crushed slag to the solvent is 1: 4, adding 300L of ethanol, and performing countercurrent extraction at 45 deg.C for 2h to obtain extractive solution.
And S2, concentrating the extracting solution obtained in the step S1 in a vacuum concentration tank under reduced pressure, adding 60L of water after the solvent is completely volatilized, stirring and diluting to obtain a diluent, wherein the volatilized solvent can be reused. Then adsorbing by using a resin column with the fixed phase of macroporous resin D101, wherein the specification of the resin column is 300mm in diameter and 1500mm in height, the flow rate of diluent in adsorption is 300ml/min, pre-washing by using 60L of 12% ethanol, and then eluting by using ethyl acetate until no product exists, thereby obtaining 150L of eluent.
S3, concentrating the eluent obtained in the step S2 under reduced pressure by adopting a vacuum concentration tank to obtain 731.5g of crude paste.
S4, carrying out reverse chromatography gradient elution on the crude paste obtained in the step S3 to obtain a semi-finished product liquid.
Wherein the reverse chromatographic gradient elution of the crude paste comprises the following steps:
s41, putting the crude paste into a material preparation tank, adding 30L of acetone for dissolving, adding 8kg of PRP-6 stationary phase into each separation column, uniformly stirring, concentrating under reduced pressure to obtain a solid, adding water according to the mass volume of 1:1 of the solid, uniformly stirring, filling the column, wherein the specification of the separation column adopts a diameter of 200mm and a height of 2000mm, and filling and sealing to obtain the separation column.
And S42, standing the separation column obtained in the step 41 for 4 hours, opening a pump body, performing gradient elution by using eluent at the flow rate of 400ml/min, and collecting liquid to obtain semi-finished liquid.
Wherein the gradient elution conditions are as follows: the eluent is a mixture of acetone and water; the elution gradient was: the proportion of the acetone in the first gradient is 55% by volume, the proportion of the acetone in the second gradient is 70% by volume, and the proportion of the acetone in the third gradient is 100% by volume; the elution volumes were: the first gradient is 2-6 column volumes; the second gradient is 6-10 column volumes; the third gradient is 1-2 column volumes. Specifically, 200L of the first gradient elution is carried out, and the collected liquid in the first stage is used as waste liquid and acetone is recycled. And (5) performing second gradient elution for 200L, and performing next treatment on the second-stage collected liquid as a semi-finished product liquid. And (3) performing gradient elution for 60L in the third stage, wherein the collected liquid in the third stage is used as an impurity-containing section, and is used as a leftover material after being concentrated.
S5, concentrating the 200L semi-finished product liquid obtained in the step S42 under reduced pressure by adopting a vacuum concentration tank, and standing for 6 hours at-4 ℃ to obtain 705.6g of crude product.
S6, flowing the crude product obtained in the step S5 into a crystallization tank, adding 3.5L of n-hexane solvent, dissolving at 45 ℃, standing at-4 ℃ for crystallization for 6 hours, and performing suction filtration to obtain a filter cake. And (3) putting the filter flask into a vacuum drying oven, and drying for 6 hours under the conditions that the pressure is 0.09Mpa and the temperature is 45 ℃ to obtain 679g of finished products, namely the cannabidiol.
Detecting whether the obtained finished product contains tetrahydrocannabinol by adopting the following liquid chromatography: the instrument comprises the following steps: agilent 2100, column: c18 Agilent Eclipse XDB-C184.6X 150mm, mobile phase: methanol: water 78: 22, flow rate: 1.0ml/min, detection wavelength: 220nm, column temperature: 25 ℃, control source: shanghai Michelin Biochemical technology Ltd, at concentrations of 0.04mg/ml, 0.08mg/ml, 0.16mg/ml, 0.32mg/ml, 0.4 mg/ml. No tetrahydrocannabinol was detected.
Accounting for cannabidiol yield
The crude paste is obtained from branches and leaves through countercurrent extraction and resin column treatment, and the yield is 97.5%. In particular, the mass of the coarse paste is divided by the mass of the dry slag.
The crude paste is separated by chromatography and crystallized, and the purity is more than 99%. The yield thereof was found to be 90.5%. In particular, the quality of the finished product is divided by the quality of the dry slag.
Example 3
This example provides a cannabidiol separation method, which is carried out in practice by using the separation system of example 1 and using the species of branches and leaves as "yunnan 7". In the yunnan 7, the content of CBD (cannabidiol) is 7500ppm, and the content of THC (tetrahydrocannabinol) is 1100 ppm. The separation method comprises the following steps:
s1, taking 100kg of Yuma No. 7 flowers and leaves, drying the flowers and leaves for 6 hours at 100 ℃ by using a hot air circulation oven, then crushing the flowers and leaves by using an industrial crusher to obtain crushed slag, sieving the crushed slag with a sieve mesh number of 20 meshes to obtain 750g of dried crushed slag, wherein the mass-to-volume ratio of the dried crushed slag to the solvent is 1: 4, adding 300L of ethanol, and extracting at 45 deg.C under countercurrent for 3 hr to obtain extractive solution.
And S2, concentrating the extracting solution obtained in the step S1 in a vacuum concentration tank under reduced pressure, adding 70L of water after the solvent is completely volatilized, stirring and diluting to obtain a diluent, wherein the volatilized solvent can be reused. Then, a stationary phase is adopted to be adsorbed by a macroporous resin X-5 resin column, the specification of the resin column is 300mm in diameter and 1500mm in height, the flow rate of diluent in adsorption is 300ml/min, 60L of 12% ethanol is used for pre-washing, and then ethyl acetate is used for eluting until no product exists, so that 180L of eluent is obtained.
S3, concentrating the eluent obtained in the step S2 under reduced pressure by adopting a vacuum concentration tank to obtain 725g of crude paste.
S4, carrying out reverse chromatography gradient elution on the crude paste obtained in the step S3 to obtain a semi-finished product liquid.
Wherein the reverse chromatographic gradient elution of the crude paste comprises the following steps:
s41, putting the crude paste into a material preparation tank, adding 30L of acetone for dissolving, adding 7.8kg of PRP-6 stationary phase into each separation column, uniformly stirring, concentrating under reduced pressure to obtain a solid, adding water according to the mass volume of 1:1 of the solid, uniformly stirring, filling the column, wherein the specification of the separation column adopts a diameter of 200mm multiplied by 2000mm in height, and filling and sealing to obtain the separation column.
And S42, standing the separation column obtained in the step 41 for 6 hours, opening a pump body, performing gradient elution by using eluent at the flow rate of 400ml/min, and collecting liquid to obtain semi-finished liquid.
Wherein the gradient elution conditions are as follows: the eluent is a mixture of acetone and water; the elution gradient was: the proportion of the acetone in the first gradient is 55% by volume, the proportion of the acetone in the second gradient is 70% by volume, and the proportion of the acetone in the third gradient is 100% by volume; the elution volumes were: the first gradient is 2-6 column volumes; the second gradient is 6-10 column volumes; the third gradient is 1-2 column volumes. Specifically, 180L of the first gradient elution is carried out, and the collected liquid in the first stage is used as waste liquid and acetone is recycled. And (4) performing second gradient elution for 180L, and performing next treatment on the second-stage collected liquid as a semi-finished product liquid. And (3) performing gradient elution for 50L in the third stage, wherein the collected liquid in the third stage is used as an impurity-containing section, and is used as a leftover material after being concentrated.
S5, concentrating the 180L semi-finished product liquid obtained in the step S42 under reduced pressure by using a vacuum concentration tank, and standing for 6 hours at-4 ℃ to obtain 688g of a crude product.
S6, flowing the crude product obtained in the step S5 into a crystallization tank, adding 2.9L of n-hexane solvent, dissolving at 50 ℃, standing at 0 ℃ for crystallization for 12 hours, and performing suction filtration to obtain a filter cake. And (3) putting the filter flask into a vacuum drying oven, and drying for 8 hours under the conditions that the pressure is 0.09Mpa and the temperature is 45 ℃ to obtain 660g of finished products, namely the cannabidiol.
Detecting whether the obtained finished product contains tetrahydrocannabinol by adopting the following liquid chromatography: the instrument comprises the following steps: agilent 2100, column: c18 Agilent Eclipse XDB-C184.6X 150mm, mobile phase: methanol: water 78: 22, flow rate: 1.0ml/min, detection wavelength: 220nm, column temperature: 25 ℃, control source: shanghai Michelin Biochemical technology Ltd, at concentrations of 0.04mg/ml, 0.08mg/ml, 0.16mg/ml, 0.32mg/ml, 0.4 mg/ml. No tetrahydrocannabinol was detected.
Accounting for cannabidiol yield
Countercurrent extraction and resin column treatment are carried out on branches and leaves to obtain crude paste, and the yield is 96.7%. In particular, the mass of the coarse paste is divided by the mass of the dry slag.
The crude paste is separated by chromatography and crystallized, and the purity is more than 99%. The yield thereof was found to be 88%. In particular, the quality of the finished product is divided by the quality of the dry slag.
Example 4
This example provides a cannabidiol separation method, which is carried out in practice by using the separation system of example 1 and using the species of branches and leaves as "yunnan 7". In the yunnan 7, the content of CBD (cannabidiol) is 7500ppm, and the content of THC (tetrahydrocannabinol) is 1100 ppm. The separation method comprises the following steps:
s1, taking 100kg of Yuma No. 7 flowers and leaves, drying the flowers and leaves for 2 hours at 200 ℃ by using a hot air circulation oven, then crushing the flowers and leaves by using an industrial crusher to obtain crushed slag, sieving the crushed slag with a sieve mesh number of 10 meshes to obtain 750g of dried crushed slag, wherein the mass-to-volume ratio of the dried crushed slag to the solvent is 1: 4, adding 300L of ethanol, and performing countercurrent extraction at 45 deg.C for 4h to obtain extractive solution.
And S2, concentrating the extracting solution obtained in the step S1 in a vacuum concentration tank under reduced pressure, adding 60L of water after the solvent is completely volatilized, stirring and diluting to obtain a diluent, wherein the volatilized solvent can be reused. Then, a stationary phase is used for macroporous resin H-103 for adsorption, the specification of the resin column is 300mm in diameter and 1500mm in height, the flow rate of diluent in adsorption is 300ml/min, 60L of 12% ethanol is used for pre-washing, and then ethyl acetate is used for eluting until no product exists, so that 180L of eluent is obtained.
S3, concentrating the eluent obtained in the step S2 under reduced pressure by a vacuum concentration tank to obtain 700g of crude paste.
S4, carrying out reverse chromatography gradient elution on the crude paste obtained in the step S3 to obtain a semi-finished product liquid.
Wherein the reverse chromatographic gradient elution of the crude paste comprises the following steps:
s41, putting the crude paste into a material preparation tank, adding 24L of acetone for dissolving, adding 7.5kg of PRP-4 stationary phase into each separation column, uniformly stirring, concentrating under reduced pressure to obtain a solid, adding water according to the mass volume of 1:1 of the solid, uniformly stirring, filling the column, wherein the specification of the separation column adopts a diameter of 200mm multiplied by 2000mm in height, and filling and sealing to obtain the separation column.
And S42, standing the separation column obtained in the step 41 for 4 hours, opening a pump body, performing gradient elution by using eluent at the flow rate of 400ml/min, and collecting liquid to obtain semi-finished liquid.
Wherein the gradient elution conditions are as follows: the eluent is a mixture of acetone and water; the elution gradient was: the volume of the ethanol in the first gradient accounts for 55% of the mixture, the volume of the ethanol in the second gradient accounts for 70% of the mixture, and the volume of the ethanol in the third gradient accounts for 100% of the mixture; the elution volumes were: the first gradient is 2-6 column volumes; the second gradient is 6-10 column volumes; the third gradient is 1-2 column volumes. Specifically, 180L of the first gradient elution is carried out, and the collected liquid in the first stage is used as waste liquid and acetone is recycled. And (4) performing second gradient elution for 180L, and performing next treatment on the second-stage collected liquid as a semi-finished product liquid. And (3) performing gradient elution for 50L in the third stage, wherein the collected liquid in the third stage is used as an impurity-containing section, and is used as a leftover material after being concentrated.
S5, concentrating the 180L semi-finished product liquid obtained in the step S42 under reduced pressure by using a vacuum concentration tank, and standing for 6 hours at-4 ℃ to obtain 664g of crude product.
S6, flowing the crude product obtained in the step S5 into a crystallization tank, adding 2.5L of n-hexane solvent, dissolving at 50 ℃, standing at 0 ℃ for crystallization for 12 hours, and performing suction filtration to obtain a filter cake. And (3) putting the filter flask into a vacuum drying oven, and drying for 8 hours under the conditions that the pressure is 0.06Mpa and the temperature is 45 ℃ to obtain 610g of finished product, namely the cannabidiol.
Detecting whether the obtained finished product contains tetrahydrocannabinol by adopting the following liquid chromatography: the instrument comprises the following steps: agilent 2100, column: c18 Agilent Eclipse XDB-C184.6X 150mm, mobile phase: methanol: water 78: 22, flow rate: 1.0ml/min, detection wavelength: 220nm, column temperature: 25 ℃, control source: shanghai Michelin Biochemical technology Ltd, at concentrations of 0.04mg/ml, 0.08mg/ml, 0.16mg/ml, 0.32mg/ml, 0.4 mg/ml. No tetrahydrocannabinol was detected.
Accounting for cannabidiol yield
The crude paste was obtained from branches and leaves by countercurrent extraction and resin column treatment with a yield of 93.3%. In particular, the mass of the coarse paste is divided by the mass of the dry slag.
The crude paste is separated by chromatography and crystallized, and the purity is more than 99%. The yield thereof was found to be 81.3%. In particular, the quality of the finished product is divided by the quality of the dry slag.
Example 5
This example provides a cannabidiol separation method, which is carried out in practice by using the separation system of example 1 and using the species of branches and leaves as "yunnan 7". In the yunnan 7, the content of CBD (cannabidiol) is 7500ppm, and the content of THC (tetrahydrocannabinol) is 1100 ppm. The separation method comprises the following steps:
s1, taking 100kg of Yuma No. 7 flowers and leaves, drying the flowers and leaves for 3 hours at 150 ℃ by using a hot air circulation oven, then crushing the flowers and leaves by using an industrial crusher to obtain crushed slag, sieving the crushed slag with a sieve mesh number of 10 meshes to obtain 750g of dried crushed slag, wherein the mass-to-volume ratio of the dried crushed slag to the solvent is 1: 4, adding 300L of ethanol, and extracting at 45 deg.C under countercurrent for 3 hr to obtain extractive solution.
And S2, concentrating the extracting solution obtained in the step S1 in a vacuum concentration tank under reduced pressure, adding 60L of water after the solvent is completely volatilized, stirring and diluting to obtain a diluent, wherein the volatilized solvent can be reused. Then adsorbing by using a resin column with the fixed phase of macroporous resin DM-130, wherein the specification of the resin column is 300mm in diameter and 1500mm in height, the flow rate of diluent in adsorption is 300ml/min, pre-washing by using 60L of 12% ethanol, and then eluting by using ethyl acetate until no product exists, thereby obtaining 200L of eluent.
S3, concentrating the eluent obtained in the step S2 under reduced pressure by a vacuum concentration tank to obtain 710g of crude paste.
S4, carrying out reverse chromatography gradient elution on the crude paste obtained in the step S3 to obtain a semi-finished product liquid.
Wherein the reverse chromatographic gradient elution of the crude paste comprises the following steps:
s41, putting the crude paste into a material preparation tank, adding 24L of acetone for dissolving, adding 8kg of PRP-6 stationary phase into each separation column, uniformly stirring, concentrating under reduced pressure to obtain a solid, adding water according to the mass volume of 1:1 of the solid, uniformly stirring, filling the column, wherein the specification of the separation column adopts a diameter of 200mm and a height of 2000mm, and filling and sealing to obtain the separation column.
And S42, standing the separation column obtained in the step 41 for 4 hours, opening a pump body, performing gradient elution by using eluent at the flow rate of 400ml/min, and collecting liquid to obtain semi-finished liquid.
Wherein the gradient elution conditions are as follows: the eluent is a mixture of acetone and water; the elution gradient was: the volume of the ethanol in the first gradient accounts for 55% of the mixture, the volume of the ethanol in the second gradient accounts for 70% of the mixture, and the volume of the ethanol in the third gradient accounts for 100% of the mixture; the elution volumes were: the first gradient is 2-6 column volumes; the second gradient is 6-10 column volumes; the third gradient is 1-2 column volumes. Specifically, 200L of the first gradient elution is carried out, and the collected liquid in the first stage is used as waste liquid and acetone is recycled. And (5) performing second gradient elution for 200L, and performing next treatment on the second-stage collected liquid as a semi-finished product liquid. And (3) performing gradient elution for 60L in the third stage, wherein the collected liquid in the third stage is used as an impurity-containing section, and is used as a leftover material after being concentrated.
S5, concentrating the 200L semi-finished product liquid obtained in the step S42 under reduced pressure by using a vacuum concentration tank, and standing for 6 hours at-4 ℃ to obtain 650g of crude product.
S6, flowing the crude product obtained in the step S5 into a crystallization tank, adding 2.5L of n-hexane solvent, dissolving at 50 ℃, standing at 0 ℃ for crystallization for 12 hours, and performing suction filtration to obtain a filter cake. And (3) putting the filter flask into a vacuum drying oven, and drying for 8 hours under the conditions that the pressure is 0.05Mpa and the temperature is 45 ℃ to obtain 628g of finished products, namely the cannabidiol.
Detecting whether the obtained finished product contains tetrahydrocannabinol by adopting the following liquid chromatography: the instrument comprises the following steps: agilent 2100, column: c18 Agilent Eclipse XDB-C184.6X 150mm, mobile phase: methanol: water 78: 22, flow rate: 1.0ml/min, detection wavelength: 220nm, column temperature: 25 ℃, control source: shanghai Michelin Biochemical technology Ltd, at concentrations of 0.04mg/ml, 0.08mg/ml, 0.16mg/ml, 0.32mg/ml, 0.4 mg/ml. No tetrahydrocannabinol was detected.
Accounting for cannabidiol yield
Countercurrent extraction and resin column treatment are carried out on branches and leaves to obtain crude paste, and the yield is 94.7%. In particular, the mass of the coarse paste is divided by the mass of the dry slag.
The crude paste is separated by chromatography and crystallized, and the purity is more than 99%. The yield thereof was found to be 83.7%. In particular, the quality of the finished product is divided by the quality of the dry slag.
Example 6
This example provides a cannabidiol separation method, which is carried out in practice by using the separation system of example 1 and using the species of branches and leaves as "yunnan 7". In the yunnan 7, the content of CBD (cannabidiol) is 7500ppm, and the content of THC (tetrahydrocannabinol) is 1100 ppm. The separation method comprises the following steps:
s1, taking 100kg of Yuma No. 7 flowers and leaves, drying the flowers and leaves for 5 hours at 100 ℃ by using a hot air circulation oven, then crushing by using an industrial crusher to obtain crushed slag, sieving the crushed slag with a sieve mesh number of 10 meshes to obtain 750g of dried crushed slag, wherein the mass-volume ratio of the dried crushed slag to the solvent is 1: 4, adding 300L of ethanol, and performing countercurrent extraction at 45 deg.C for 6h to obtain extractive solution.
And S2, concentrating the extracting solution obtained in the step S1 in a vacuum concentration tank under reduced pressure, adding 60L of water after the solvent is completely volatilized, stirring and diluting to obtain a diluent, wherein the volatilized solvent can be reused. Then adsorbing by using XAD-16 resin column with macroporous resin as stationary phase, wherein the specification of the resin column is 300mm in diameter and 1500mm in height, the flow rate of diluent in adsorption is 300ml/min, pre-washing by using 60L 12% ethanol, and eluting by using ethyl acetate until no product is produced, thereby obtaining 180L eluent.
S3, concentrating the eluent obtained in the step S2 under reduced pressure by a vacuum concentration tank to obtain 715g of crude paste.
S4, carrying out reverse chromatography gradient elution on the crude paste obtained in the step S3 to obtain a semi-finished product liquid.
Wherein the reverse chromatographic gradient elution of the crude paste comprises the following steps:
s41, putting the crude paste into a material preparation tank, adding 24L of acetone for dissolving, adding 7.5kg of PRP-4 stationary phase into each separation column, uniformly stirring, concentrating under reduced pressure to obtain a solid, adding water according to the mass volume of 1:1 of the solid, uniformly stirring, filling the column, wherein the specification of the separation column adopts a diameter of 200mm multiplied by 2000mm in height, and filling and sealing to obtain the separation column.
And S42, standing the separation column obtained in the step 41 for 6 hours, opening a pump body, performing gradient elution by using eluent at the flow rate of 400ml/min, and collecting liquid to obtain semi-finished liquid.
Wherein the gradient elution conditions are as follows: the eluent is a mixture of acetone and water; the elution gradient was: the volume of the ethanol in the first gradient accounts for 55% of the mixture, the volume of the ethanol in the second gradient accounts for 70% of the mixture, and the volume of the ethanol in the third gradient accounts for 100% of the mixture; the elution volumes were: the first gradient is 2-6 column volumes; the second gradient is 6-10 column volumes; the third gradient is 1-2 column volumes. Specifically, 200L of the first gradient elution is carried out, and the collected liquid in the first stage is used as waste liquid and acetone is recycled. And (5) performing second gradient elution for 200L, and performing next treatment on the second-stage collected liquid as a semi-finished product liquid. And (3) performing gradient elution for 60L in the third stage, wherein the collected liquid in the third stage is used as an impurity-containing section, and is used as a leftover material after being concentrated.
S5, concentrating the 200L semi-finished product liquid obtained in the step S42 under reduced pressure by using a vacuum concentration tank, and standing for 6 hours at-4 ℃ to obtain 648g of crude product.
S6, enabling the crude product obtained in the step S5 to flow into a crystallizing tank, adding 2L of ethyl acetate solvent, dissolving at 40 ℃, standing at 0 ℃ for crystallization for 12 hours, and performing suction filtration to obtain a filter cake. And (3) putting the filter flask into a vacuum drying oven, and drying for 8 hours under the conditions that the pressure is 0.06Mpa and the temperature is 45 ℃ to obtain 612g of finished products, namely the cannabidiol.
Detecting whether the obtained finished product contains tetrahydrocannabinol by adopting the following liquid chromatography: the instrument comprises the following steps: agilent 2100, column: c18 Agilent Eclipse XDB-C184.6X 150mm, mobile phase: methanol: water 78: 22, flow rate: 1.0ml/min, detection wavelength: 220nm, column temperature: 25 ℃, control source: shanghai Michelin Biochemical technology Ltd, at concentrations of 0.04mg/ml, 0.08mg/ml, 0.16mg/ml, 0.32mg/ml, 0.4 mg/ml. No tetrahydrocannabinol was detected.
Accounting for cannabidiol yield
The crude paste is obtained from branches and leaves through countercurrent extraction and resin column treatment, and the yield is 95.3%. In particular, the mass of the coarse paste is divided by the mass of the dry slag.
The crude paste is separated by chromatography and crystallized, and the purity is more than 99%. The yield thereof was found to be 81.6%. In particular, the quality of the finished product is divided by the quality of the dry slag.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like are used in the orientation or positional relationship indicated in the drawings, which are merely for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and are therefore not to be construed as limiting the invention. Furthermore, the terms "first", "second", etc. are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first," "second," etc. may explicitly or implicitly include one or more of that feature. In the description of the invention, the meaning of "a plurality" is two or more unless otherwise specified.
In the description of the invention, it is to be noted that, unless otherwise explicitly specified or limited, the terms "mounted", "connected" and "connected" are to be construed broadly, e.g. as being fixed or detachable or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meaning of the above terms in the creation of the present invention can be understood by those of ordinary skill in the art through specific situations.
It is to be noted that "comprising" in the present invention means that it may include other components in addition to the components described, and the "comprising" may be replaced with "being" or "consisting of … …" in a closed manner.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. The method for separating the cannabidiol is characterized by comprising the following steps of:
s1, drying flowers and leaves of industrial hemp, then crushing to obtain crushed slag, and adding an extraction solvent for countercurrent extraction to obtain an extracting solution;
s2, firstly concentrating the extracting solution obtained in the step S1, then adding water for dilution to obtain a diluent, adsorbing the diluent by using a resin column, and then eluting by using an elution solvent to obtain an eluent;
s3, concentrating the eluent obtained in the step S2 to obtain a crude paste;
s4, carrying out reverse chromatography gradient elution on the crude paste obtained in the step S3 to obtain a semi-finished product liquid;
s5, concentrating the semi-finished product liquid obtained in the step S4 to obtain a crude product;
s6, recrystallizing the crude product obtained in the step S5, filtering to obtain a filter cake, and drying to obtain a finished product, namely the cannabidiol.
2. The method for separating cannabidiol as claimed in claim 1, wherein in step S1, the drying temperature is 100 ℃ and 200 ℃ for 2-6 h; the mesh number of the crushed slag is 5-100 meshes; the temperature of the countercurrent extraction is 30-80 ℃; the extraction solvent is a mixture of any one of methanol, ethanol, petroleum ether and ethyl acetate and water in any proportion; the mass volume ratio of the slag to the extraction solvent is 1: (3-10).
3. The method for separating cannabidiol as claimed in claim 1, wherein in step S2, the concentration is performed by vacuum concentration in a vacuum concentration tank; the flow rate of the diluent in the adsorption is 300-1000 ml/min; the elution solvent is ethyl acetate or hexane; the stationary phase in the resin column is one or more of macroporous resin D101, macroporous resin H-103, macroporous resin DM-130, macroporous resin X-5 and macroporous resin XAD-16.
4. The method for separating cannabidiol as claimed in claim 1, wherein in step S3, the concentration is performed by vacuum concentration in a vacuum concentration tank.
5. The method of separating cannabidiol as claimed in claim 1, wherein the step of subjecting the crude paste to reverse chromatographic gradient elution at step S4 comprises the steps of:
s41, adding a solvent into the crude paste for dissolving, adding a stationary phase, uniformly stirring, concentrating to obtain a solid, adding water according to the mass volume ratio of 1 (1-2) to the solid, uniformly stirring, and filling into a column to obtain a separation column;
s42, standing the separation column obtained in the step 41 for 2-6 hours, performing gradient elution by using an eluent, and collecting liquid to obtain semi-finished liquid.
6. The method of separating cannabidiol as claimed in claim 5, wherein in step S41, the stationary phase is added in an amount of 5-20kg per separation column, and the stationary phase is one of macroporous resin PRP-4, macroporous resin PRP-5, macroporous resin PRP-6 and macroporous resin PRP-7.
7. The method of separating cannabidiol as claimed in claim 5, wherein in step S42, the conditions of the reverse chromatographic gradient elution are: the eluent is a mixture of water and one of organic solvents of methanol, ethanol, acetone and acetonitrile; the elution gradient was: the volume of the organic solvent of the first gradient accounts for 30-60% of the mixture, the volume of the organic solvent of the second gradient accounts for 60-90% of the mixture, and the volume of the organic solvent of the third gradient accounts for 90-100% of the mixture; the elution volumes were: the first gradient is the volume of 2-6 separation columns; the second gradient is the volume of 6-10 separation columns; the third gradient is the volume of 1-2 separation columns.
8. The method for separating cannabidiol as claimed in any one of claims 1 to 7, wherein in step S5, the concentration is performed by vacuum concentration in a vacuum concentration tank.
9. The method for separating cannabidiol as claimed in any one of claims 1 to 7, wherein in step S6, the solvent used for recrystallization is one of n-hexane, petroleum ether, ethyl acetate and acetonitrile, the dissolving temperature is 30 to 60 ℃, and the addition amount of the solvent is 1: (10-30); in step S6, the crystallization temperature is-20 ℃ to 5 ℃, and the crystallization time is 4 to 24 hours; in step S6, the drying pressure is-0.05-0.09 Mpa, the drying temperature is 30-60 ℃, and the drying time is 6-24 h.
10. A cannabidiol separation system is characterized by comprising a countercurrent extraction device (1), an elution tower (5), a chromatographic separation system, a recrystallization tank (14), a drying device (16) and a finished product tank (18);
be equipped with feed inlet (2) on countercurrent extraction device (1), the output of countercurrent extraction device (1) with the input of elution tower (5) is connected, the output of elution tower (5) with chromatographic separation system's input is connected, chromatographic separation system's output with the input of recrystallization jar (14) is connected, the output of recrystallization jar (14) with the input of drying device (16) is connected, the output of drying device (16) with finished product jar (18) is connected.
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