CN111099970A - Method for industrially extracting cannabidiol from industrial cannabis sativa - Google Patents
Method for industrially extracting cannabidiol from industrial cannabis sativa Download PDFInfo
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Abstract
The invention provides a method for industrially extracting cannabidiol from industrial cannabis sativa, which comprises the following steps: 1) screening; 2) drying; 3) crushing; 4) drying again; 5) micronizing; 6) granulating; 7) extraction: performing supercritical carbon dioxide supercritical extraction on the particles to obtain a primary extract of industrial cannabis rich in cannabidiol; 8) and (3) purification: heating the primary extract, performing molecular distillation to obtain cannabidiol concentrate, and performing supercritical fluid chromatographic separation on the cannabidiol concentrate for purification to obtain cannabidiol which does not contain tetrahydrocannabinol and has mass purity of more than 99%. The method is suitable for large-scale industrial production, the obtained product does not need additional separation and purification steps, the cost of an enterprise is greatly reduced, and meanwhile, the purity of the obtained cannabidiol product is more than 99%.
Description
Technical Field
The invention relates to a chemical extraction method, belongs to the technical field of chemical substance extraction, and particularly relates to a method for extracting cannabidiol from industrial cannabis sativa.
Background
Industrial hemp (Stevia rebaudiana Bertoni) is an annual plant of the genus cannabis of the family cannabinaceae, widely distributed around the world. The Cannabis plants in the world are mainly 3 species of wild Cannabis sativa (Cannabis ruderalisisch), Indian Cannabis sativa (Cannabis indica Lam) and cultivated Cannabis sativa (Cannabis sativaL), and many Cannabis varieties and subspecies are generated in the long-term biological evolution process. Cannabis sativa contains Tetrahydrocannabinol (THC), a hallucinogenic secondary metabolite, and is one of the well-known drug-source plants. For convenience of supervision and reasonable use, the varieties of cannabis with THC content of less than 0.3% in cannabis are internationally defined as industrial cannabis which does not have drug utilization value. At present, 27 countries in the world grow industrial cannabis, and 26 industrial cannabis varieties with THC content of less than 0.3% are cultivated. The industrial hemp plants are tall and big, the branches are few, the fiber content is high, and the economic value of the industrial hemp plants relates to a plurality of aspects such as papermaking, spinning, building materials, food, medicine and the like.
Research has shown that Cannabidiol (CBD), a non-addictive component in industrial cannabis sativa, has the effects of resisting inflammation, killing bacteria, easing pain, resisting anxiety, resisting psychosis, resisting oxidation, improving learning and memory, protecting nerves, reducing intestinal peristalsis and the like, can be used for treating multiple arteriosclerosis and Parkinson's disease, preventing myocardial infarction, blocking breast cancer metastasis, inhibiting glioma cell metastasis, inhibiting sex hormone secretion and the like, and can also be used for treating spasticity and dyskinesia, cancer pain, neuralgia, migraine, epilepsy and the like of patients suffering from glaucoma, paraplegia and multiple sclerosis. Therefore, the vigorous development and utilization of industrial hemp is a green project benefiting the nation and the people and protecting the natural ecological environment, and the diversified products thereof have a wide international market.
At present, a plurality of new varieties of excellent industrial hemp are bred in many countries by means of variety breeding and improvement, hybridization and genetic engineering breeding. China also continuously explores the aspects of planting and breeding of industrial marihuana. For example, the agricultural academy of sciences of Yunnan province has been leading to the breeding of a plurality of varieties of industrial hemp of the Yuma series, such as Yuma No. 1, Yuma No. 2, Yuma No. 3, Yuma No. 4, Yuma No. 5, Yuma No. 6, Yuma No. 7, etc., which have been popularized and planted in China, such as inner Mongolia, Heilongjiang, Anhui, etc.
With the recent change in the product policy of industrial hemp, several methods for extracting cannabidiol from industrial hemp have been disclosed.
CN109202391A discloses a method for extracting cannabidiol from industrial cannabis sativa, comprising: taking industrial hemp leaves, drying and crushing, adding a mixed solution of cell wall decomposition enzyme cellulase and pectinase, hydrolyzing, and then adding an extraction solvent, and stirring and extracting; performing rotary evaporation on the extracted supernatant to obtain an oily substance; adding methanol into the oily matter, centrifuging at low temperature to obtain supernatant, decolorizing the supernatant with activated carbon, filtering to obtain filtrate, and rotary steaming; and then adding chloroform into the rotary evaporation product to dissolve the rotary evaporation product, and filtering the solution through an organic membrane to obtain the industrial cannabidiol solution. However, although the method increases the extraction amount of cannabidiol due to the addition of cell wall lytic enzyme, more impurities are introduced, which brings difficulty to the later separation and purification of the product and increases the cost, and is not suitable for industrial production.
CN110041171A discloses a method for extracting cannabidiol from industrial cannabis sativa leaves, which adopts the following technical scheme:
(1) drying industrial hemp leaves, carrying out superfine grinding and sieving to obtain industrial hemp powder; (2) adjusting the water content of industrial hemp leaf powder to 8% -10%, and then performing microwave-assisted solvent extraction to obtain a crude extraction solution; (3) separating the crude extract with three phases to obtain solvent phase; (4) carrying out reduced pressure distillation on the solvent phase to obtain grease containing cannabidiol; (5) obtaining the cannabidiol through molecular distillation. However, the method adopts microwave assistance, and the control of microwave energy is a difficulty of the method, which causes the reaction of a large amount of chemical substances, so that the actual yield of cannabidiol is low, and the method is also not beneficial to industrial production.
CN110066216A discloses a method for extracting and separating cannabidiol, which comprises the following steps:
1) crushing: crushing dried industrial hemp flowers and leaves into particles by using a grinding dispersion machine; 2) extraction: ethanol, petroleum ether or solvent gasoline are used as a single solvent or a mixed solvent to carry out reflux extraction on the materials; 3) enrichment: carrying out macroporous resin laminate on the industrial hemp fluid extract obtained by extraction and concentration, collecting eluent in sections and concentrating to obtain cannabidiol concentrate; 4) separation: and (3) carrying out silica gel column chromatography on the cannabidiol enriched product, collecting eluent in sections, and concentrating, drying and crystallizing the eluent to obtain the cannabidiol.
Therefore, it is an urgent technical problem to provide a practical extraction method of cannabidiol which is applicable to large-scale industrial production.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for industrially extracting cannabidiol from industrial cannabis sativa, which comprises the following steps:
1) screening: selecting industrial hemp, removing mildewed and deteriorated parts, and reserving clean and healthy plant parts as raw materials;
2) drying: placing the selected raw materials in drying equipment for drying;
3) crushing: crushing the dried raw materials;
4) and (5) drying again: drying the crushed raw materials again;
5) superfine grinding: carrying out superfine grinding on the raw material which is dried again to ensure that cell walls of cells in the raw material are broken;
6) and (3) granulation: adding a proper amount of solvent into the superfine crushed material for granulation to obtain particles taking industrial hemp as a raw material;
7) extraction: performing supercritical carbon dioxide supercritical extraction on the particles to obtain a primary extract of industrial cannabis rich in cannabidiol;
8) and (3) purification: heating the primary extract, performing molecular distillation to obtain cannabidiol concentrate, and performing supercritical fluid chromatographic separation on the cannabidiol concentrate for purification to obtain cannabidiol which does not contain tetrahydrocannabinol and has mass purity of more than 99%.
Further, the industrial cannabis in step 1) comprises flowers, leaves, stems, roots and/or fruits of industrial cannabis.
Further, the drying device in the step 2) comprises an oven, a baking tray, a steam heat exchanger and/or an air supply device.
Further, the drying temperature in the step 2) is 120-.
Further, in the step 2), the water content of the dried raw material is lower than 8 percent (by mass). Preferably, the drying temperature is 160 ℃ and the drying time is 30 minutes.
Further, the crushing in the step 3) comprises crushing the dried raw materials by a crusher until the passing rate of the dried raw materials passing through a 80-mesh sieve is more than or equal to 95 percent (by mass), and the passing rate of the dried raw materials passing through the 60-mesh sieve reaches 100 percent.
Further, the drying in the step 4) is carried out again at the temperature of 110 ℃ and 140 ℃ for 10-20 minutes.
Further, in the step 4), drying is carried out again, and the water content of the dried raw material is lower than 5 percent (mass). Preferably, the drying temperature is 120 ℃ and the drying time is 15 minutes.
Further, the micronization in the step 5) comprises pulverizing the raw material having a water content of less than 5% by mass to a size of 200 mesh or more to ensure sufficient cell wall breakage of the raw material.
Further, in the granulation in the step 6), the particle size of the granules is phi 2mm x (5-8) mm.
Further, in the extraction in the step 7), the particles obtained in the step 6) are subjected to carbon dioxide supercritical extraction through an extraction kettle, then the supercritical carbon dioxide fluid rich in cannabidiol from the extraction kettle is subjected to two-stage throttling expansion, and a primary extract of industrial cannabis rich in cannabidiol is resolved from the bottom of the second separation kettle, wherein the effective content is 10-30%;
the method comprises the following specific steps: comprises that the particles which take industrial hemp as raw material are extracted by supercritical carbon dioxide in an extraction kettle, the extraction temperature range is 30-50 ℃, the pressure range is 25-30MPa, and the extraction time range is 3-8 hours, so as to obtain the supercritical carbon dioxide fluid which is rich in cannabidiol; decompressing a supercritical carbon dioxide fluid enriched with cannabidiol from the top of the extraction kettle to 15MPa through a first throttling valve, entering the first separation kettle from the top of the first separation kettle, circulating the carbon dioxide part separated from the side surface of the first separation kettle to the bottom of the extraction kettle through a pipeline, and continuously using the supercritical carbon dioxide fluid for the supercritical extraction process, decompressing the fluid from the bottom of the first separation kettle to 6MPa through a second throttling valve, entering the second separation kettle from the top of the second separation kettle, circulating the carbon dioxide further separated from the side surface of the second separation kettle to the bottom of the extraction kettle through a pipeline, and continuously using the supercritical carbon dioxide fluid for the supercritical extraction process;
further, the purification in the step 8) comprises heating the primary extract to 50-80 ℃, performing a scraper evaporator, setting the pressure to 0.01-0.1Mpa, performing molecular distillation to obtain cannabidiol concentrate, performing supercritical fluid chromatography on the cannabidiol concentrate, and purifying cannabidiol to obtain a cannabidiol product which is free of tetrahydrocannabinol and has a purity of more than 99%.
Further, the supercritical fluid chromatographic separation in step 8) is carried out under the operating conditions comprising: taking any one of 100-200-mesh macroporous resin, MCI resin or C18 silica gel as a stationary phase, and mixing the materials in a volume ratio of 50:1, the volume ratio of the supercritical carbon dioxide and ethanol (as entrainer) as a mobile phase fixed phase to the mobile phase is 1: and 20, performing isocratic elution, wherein the flow rate of the mobile phase is kept unchanged at 15-45L/min during the isocratic elution.
The invention has the beneficial effects that:
1. the invention really realizes the industrial production of extracting cannabidiol from industrial hemp;
2. the cannabidiol obtained in the operation process of the method has high purity, does not contain tetrahydrocannabinol, and has the mass purity of more than 99 percent;
3. the method is beneficial to reducing the cost of enterprises and suitable for large-scale industrial production.
Detailed Description
Example 1
A method for industrially extracting cannabidiol from industrial cannabis sativa comprises the following steps:
1) screening: selecting flowers, leaves, stems, roots and/or fruits of industrial hemp, removing moldy and deteriorated parts, and reserving clean and healthy plant parts as raw materials;
2) drying: placing the selected raw materials in an oven for drying, wherein the drying temperature is 120 ℃, and the drying time is 10 minutes;
3) crushing: crushing the dried raw materials, wherein the crushing of the dried raw materials by a crusher until the passing rate of a 80-mesh sieve is 98% (by mass) and the passing rate of a 60-mesh sieve is 100% (by mass);
4) and (5) drying again: drying the crushed raw materials again at the temperature of 110 ℃ for 10 minutes, wherein the water content of the dried raw materials is lower than 3 percent (by mass);
5) superfine grinding: carrying out superfine grinding on the raw material which is dried again, and grinding the raw material with the water content of less than 3 percent (by mass) to a material which is sieved by a 200-mesh sieve to ensure that cell walls of cells in the raw material are broken;
6) and (3) granulation: adding appropriate amount of solvent into the superfine pulverized material, and granulating to obtain granules with granularity of industrial hemp as raw material
7) Extraction: the method comprises the steps of performing supercritical carbon dioxide extraction on particles which take industrial hemp as a raw material in an extraction kettle at the extraction temperature range of 40 ℃, the pressure range of 25MPa and the extraction time range of 5 hours to obtain a supercritical carbon dioxide fluid enriched in cannabidiol; decompressing supercritical carbon dioxide fluid enriched with cannabidiol from the top of the extraction kettle to 15MPa through a first throttling valve, entering the first separation kettle from the top of the first separation kettle, circulating the carbon dioxide part from the side surface of the first separation kettle to the bottom of the extraction kettle through a pipeline after separation, continuously using the supercritical extraction process, decompressing the fluid from the bottom of the first separation kettle to 6MPa through a second throttling valve, entering the second separation kettle from the top of the second separation kettle, circulating the carbon dioxide part from the side surface of the second separation kettle to the bottom of the extraction kettle through a pipeline after further separation, and continuously using the supercritical extraction process to extract the obtained industrial cannabis extract rich in cannabis diol, wherein the effective content of cannabis diol is 17.5%;
8) and (3) purification: heating the primary extract in a water bath at 80 ℃ for 1.5 hours, enabling the temperature of the primary extract to reach 60 ℃, entering a scraper evaporator, setting the pressure to be 0.05MPa, heating, and then performing molecular distillation, wherein the distillation conditions are as follows: 160 ℃ and the condensation temperature of 10 ℃ to obtain the cannabidiol concentrate, and then carrying out supercritical fluid chromatography separation on the cannabidiol concentrate, wherein the operation conditions are as follows: taking 100-mesh macroporous resin as a stationary phase, taking supercritical carbon dioxide and ethanol (as an entrainer) with a volume ratio of 50:1 as a mobile phase, taking the stationary phase and the mobile phase with a volume ratio of 1:20, carrying out isocratic elution, keeping the flow rate of the mobile phase at 20L/min in the isocratic elution process, and purifying a cannabidiol product through supercritical fluid chromatography to obtain cannabidiol which does not contain tetrahydrocannabinol and has the mass purity of 99.37%.
Example 2
A method for industrially extracting cannabidiol from industrial cannabis sativa comprises the following steps:
1) screening: selecting flowers, leaves, stems, roots and/or fruits of industrial hemp, removing moldy and deteriorated parts, and reserving clean and healthy plant parts as raw materials;
2) drying: placing the selected raw materials in an oven for drying, wherein the drying temperature is 180 ℃, and the drying time is 15 minutes;
3) crushing: crushing the dried raw materials, wherein the crushing step comprises crushing the dried raw materials by a crusher to obtain a 80-mesh sieve with a passing rate of 95% (by mass) and a 60-mesh sieve with a passing rate of 100% (by mass);
4) and (5) drying again: drying the crushed raw materials again at 140 ℃ for 13 minutes, wherein the water content of the dried raw materials is lower than 1.5 percent (by mass);
5) superfine grinding: carrying out superfine grinding on the raw material which is dried again, and grinding the raw material with the water content of less than 1.5 percent (by mass) to a material which is sieved by a 300-mesh sieve to ensure that cell walls of cells in the raw material are broken;
6) and (3) granulation: adding appropriate amount of solvent into the superfine pulverized material, and granulating to obtain granules with granularity of industrial hemp as raw material
7) Extraction: the method comprises the steps of performing supercritical carbon dioxide extraction on particles which take industrial hemp as a raw material in an extraction kettle at the extraction temperature range of 50 ℃, the pressure range of 29MPa and the extraction time range of 8 hours to obtain a supercritical carbon dioxide fluid enriched with cannabidiol; decompressing supercritical carbon dioxide fluid enriched with cannabidiol from the top of the extraction kettle to 15MPa through a first throttling valve, entering the first separation kettle from the top of the first separation kettle, circulating the carbon dioxide part from the side surface of the first separation kettle to the bottom of the extraction kettle through a pipeline after separation, continuously using the supercritical extraction process, decompressing the fluid from the bottom of the first separation kettle to 6MPa through a second throttling valve, entering the second separation kettle from the top of the second separation kettle, circulating the carbon dioxide part from the side surface of the second separation kettle to the bottom of the extraction kettle through a pipeline after further separation, and continuously using the supercritical extraction process to extract the obtained industrial cannabis extract rich in cannabis diol, wherein the effective content of cannabis diol is 20.3%;
8) and (3) purification: heating the primary extract in water bath at 80 ℃ for 1 hour, enabling the temperature of the primary extract to reach 70 ℃, entering a scraper evaporator, setting the pressure to be 0.03MPa, heating, and performing molecular distillation, wherein the distillation conditions are as follows: obtaining cannabidiol concentrate at 190 ℃ and a condensation temperature of 17 ℃, and then performing supercritical fluid chromatography separation on the cannabidiol concentrate, wherein the operation conditions are as follows: using 200-mesh C18 silica gel as a stationary phase, using 50:1 volume ratio of supercritical carbon dioxide and ethanol (as an entrainer) as a mobile phase, using 1:20 volume ratio of the stationary phase to the mobile phase, performing isocratic elution, keeping the flow rate of the mobile phase at 30L/min during the isocratic elution, and purifying a cannabidiol product by supercritical fluid chromatography to obtain cannabidiol which does not contain tetrahydrocannabinol and has the mass purity of 99.5%.
Example 3
A method for industrially extracting cannabidiol from industrial cannabis sativa comprises the following steps:
1) screening: selecting flowers, leaves, stems, roots and/or fruits of industrial hemp, removing moldy and deteriorated parts, and reserving clean and healthy plant parts as raw materials;
2) drying: placing the selected raw materials in an oven for drying, wherein the drying temperature is 170 ℃, and the drying time is 20 minutes;
3) crushing: crushing the dried raw materials, wherein the crushing of the dried raw materials by a crusher until the passing rate of a 80-mesh sieve is 97% (by mass) and the passing rate of a 60-mesh sieve is 100% (by mass);
4) and (5) drying again: drying the crushed raw materials again at 135 ℃ for 13 minutes, wherein the water content of the dried raw materials is lower than 4.5 percent (by mass);
5) superfine grinding: carrying out superfine grinding on the raw material which is dried again, and grinding the raw material with the water content of less than 4.5 percent (by mass) to a material which is sieved by a 200-mesh sieve to ensure that cell walls of cells in the raw material are broken;
6) and (3) granulation: adding appropriate amount of solvent into the superfine pulverized material, and granulating to obtain granules with granularity of industrial hemp as raw material
7) Extraction: the method comprises the steps of performing supercritical carbon dioxide extraction on particles which take industrial hemp as a raw material in an extraction kettle at the extraction temperature range of 48 ℃, the pressure range of 30MPa and the extraction time range of 4 hours to obtain a supercritical carbon dioxide fluid enriched in cannabidiol; decompressing supercritical carbon dioxide fluid enriched with cannabidiol from the top of the extraction kettle to 15MPa through a first throttling valve, entering the first separation kettle from the top of the first separation kettle, circulating the carbon dioxide part from the side surface of the first separation kettle to the bottom of the extraction kettle through a pipeline after separation, continuously using the supercritical extraction process, decompressing the fluid from the bottom of the first separation kettle to 6MPa through a second throttling valve, entering the second separation kettle from the top of the second separation kettle, circulating the carbon dioxide part from the side surface of the second separation kettle to the bottom of the extraction kettle through a pipeline after further separation, and continuously using the supercritical extraction process to extract the obtained industrial cannabis extract rich in cannabis diol, wherein the effective content of cannabis diol is 20.9%;
8) and (3) purification: heating the primary extract in water bath at 80 ℃ for 2 hours, enabling the temperature of the primary extract to reach 78 ℃, entering a scraper evaporator, setting the pressure to be 0.1MPa, heating, and performing molecular distillation, wherein the distillation conditions are as follows: obtaining cannabidiol concentrate at 200 ℃ and a condensation temperature of 18 ℃, and then performing supercritical fluid chromatography separation on the cannabidiol concentrate, wherein the operation conditions are as follows: using 100-mesh MCI resin as a stationary phase, using supercritical carbon dioxide and ethanol (as an entrainer) with a volume ratio of 50:1 as a mobile phase, using the stationary phase and the mobile phase with a volume ratio of 1:20, performing isocratic elution, keeping the flow rate of the mobile phase at 30L/min during the isocratic elution, and purifying a cannabidiol product through supercritical fluid chromatography to obtain the cannabidiol which does not contain tetrahydrocannabinol and has a mass purity of 99.2%.
Example 4
A method for industrially extracting cannabidiol from industrial cannabis sativa comprises the following steps:
1) screening: selecting flowers, leaves, stems, roots and/or fruits of industrial hemp, removing moldy and deteriorated parts, and reserving clean and healthy plant parts as raw materials;
2) drying: placing the selected raw materials in an oven for drying, wherein the drying temperature is 140 ℃, and the drying time is 20 minutes;
3) crushing: crushing the dried raw materials, wherein the crushing of the dried raw materials by a crusher until the passing rate of a 80-mesh sieve is 99% (by mass), and the passing rate of a 60-mesh sieve is 100% (by mass);
4) and (5) drying again: drying the crushed raw materials again at 140 ℃ for 20 minutes, wherein the water content of the dried raw materials is lower than 0.5 percent (by mass);
5) superfine grinding: carrying out superfine grinding on the raw material which is dried again, and grinding the raw material with the water content of less than 0.5 percent (by mass) to a material which is sieved by a 200-mesh sieve to ensure that cell walls of cells in the raw material are broken;
6) and (3) granulation: adding appropriate amount of solvent into the superfine pulverized material, and granulating to obtain granules with granularity of industrial hemp as raw material
7) Extraction: the method comprises the steps of performing supercritical carbon dioxide extraction on particles which take industrial hemp as a raw material in an extraction kettle at the extraction temperature range of 45 ℃, the pressure range of 30MPa and the extraction time range of 7 hours to obtain a supercritical carbon dioxide fluid enriched in cannabidiol; decompressing supercritical carbon dioxide fluid enriched with cannabidiol from the top of the extraction kettle to 15MPa through a first throttling valve, entering the first separation kettle from the top of the first separation kettle, circulating the carbon dioxide part from the side surface of the first separation kettle to the bottom of the extraction kettle through a pipeline after separation, continuously using the supercritical extraction process, decompressing the fluid from the bottom of the first separation kettle to 6MPa through a second throttling valve, entering the second separation kettle from the top of the second separation kettle, circulating the carbon dioxide part from the side surface of the second separation kettle to the bottom of the extraction kettle through a pipeline after further separation, and continuously using the supercritical extraction process to extract the obtained industrial cannabis extract rich in cannabis diol, wherein the effective content of cannabis diol is 18.4%;
8) and (3) purification: heating the primary extract in 80 ℃ water bath for 2 hours, enabling the temperature of the primary extract to reach 78 ℃, entering a scraper evaporator, setting the pressure to be 0.08MPa, heating, and performing molecular distillation, wherein the distillation conditions are as follows: obtaining cannabidiol concentrate at 190 ℃ and a condensation temperature of 20 ℃, and then performing supercritical fluid chromatography separation on the cannabidiol concentrate, wherein the operation conditions are as follows: taking 100-mesh macroporous resin as a stationary phase, taking supercritical carbon dioxide and ethanol (as an entrainer) with a volume ratio of 50:1 as a mobile phase, taking the stationary phase and the mobile phase with a volume ratio of 1:20, carrying out isocratic elution, keeping the flow rate of the mobile phase at 45L/min in the isocratic elution process, and purifying a cannabidiol product through supercritical fluid chromatography to obtain cannabidiol which does not contain tetrahydrocannabinol and has the mass purity of 99.8%.
Example 5
A method for industrially extracting cannabidiol from industrial cannabis sativa comprises the following steps:
1) screening: selecting flowers, leaves, stems, roots and/or fruits of industrial hemp, removing moldy and deteriorated parts, and reserving clean and healthy plant parts as raw materials;
2) drying: placing the selected raw materials in an oven for drying, wherein the drying temperature is 130 ℃, and the drying time is 20 minutes;
3) crushing: crushing the dried raw materials, wherein the crushing of the dried raw materials by a crusher until the passing rate of a 80-mesh sieve is 96 percent (by mass) and the passing rate of a 60-mesh sieve is 100 percent (by mass);
4) and (5) drying again: drying the crushed raw materials again at 140 ℃ for 15 minutes, wherein the water content of the dried raw materials is 0.3 percent (by mass);
5) superfine grinding: carrying out superfine grinding on the raw material which is dried again, grinding the raw material with the water content of 0.3 percent (mass) to a material which is sieved by a 200-mesh sieve, and ensuring that cell walls of cells in the raw material are broken;
6) and (3) granulation: adding appropriate amount of solvent into the superfine pulverized material, and granulating to obtain granules with granularity of industrial hemp as raw material
7) Extraction: the method comprises the steps of performing supercritical carbon dioxide extraction on particles which take industrial hemp as a raw material in an extraction kettle at the extraction temperature range of 60 ℃, the pressure range of 30MPa and the extraction time range of 8 hours to obtain a supercritical carbon dioxide fluid enriched in cannabidiol; decompressing supercritical carbon dioxide fluid enriched with cannabidiol from the top of the extraction kettle to 15MPa through a first throttling valve, entering the first separation kettle from the top of the first separation kettle, circulating the carbon dioxide part from the side surface of the first separation kettle to the bottom of the extraction kettle through a pipeline after separation, continuously using the supercritical extraction process, decompressing the fluid from the bottom of the first separation kettle to 6MPa through a second throttling valve, entering the second separation kettle from the top of the second separation kettle, circulating the carbon dioxide part from the side surface of the second separation kettle to the bottom of the extraction kettle through a pipeline after further separation, continuously using the supercritical extraction process, and extracting the obtained industrial cannabis extract enriched with cannabidiol, wherein the effective content of cannabidiol is 19.1%;
8) and (3) purification: heating the primary extract in a water bath at 80 ℃ for 2 hours, enabling the temperature of the primary extract to reach 80 ℃, entering a scraper evaporator, setting the pressure to be 0.1MPa, heating, and performing molecular distillation, wherein the distillation conditions are as follows: obtaining cannabidiol concentrate at 200 ℃ and a condensation temperature of 13 ℃, and then performing supercritical fluid chromatography separation on the cannabidiol concentrate, wherein the operation conditions are as follows: using 100-mesh C18 silica gel as a stationary phase, using supercritical carbon dioxide and ethanol (as an entrainer) with a volume ratio of 50:1 as a mobile phase, using the stationary phase and the mobile phase with a volume ratio of 1:20, performing isocratic elution, keeping the flow rate of the mobile phase at 45L/min during the isocratic elution, and purifying a cannabidiol product through supercritical fluid chromatography to obtain the cannabidiol which does not contain tetrahydrocannabinol and has a mass purity of 99.76%.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, but any modifications or equivalent variations made according to the technical spirit of the present invention are within the scope of the present invention as claimed.
Claims (10)
1. A method for industrially extracting cannabidiol from industrial cannabis sativa, comprising:
1) screening: selecting industrial hemp, removing mildewed and deteriorated parts, and reserving clean and healthy plant parts as raw materials;
2) drying: placing the selected raw materials in drying equipment for drying;
3) crushing: crushing the dried raw materials;
4) and (5) drying again: drying the crushed raw materials again;
5) superfine grinding: carrying out superfine grinding on the raw material which is dried again to ensure that cell walls of cells in the raw material are broken;
6) and (3) granulation: adding a proper amount of solvent into the superfine crushed material for granulation to obtain particles taking industrial hemp as a raw material;
7) extraction: performing supercritical carbon dioxide supercritical extraction on the particles to obtain a primary extract of industrial cannabis rich in cannabidiol;
8) and (3) purification: heating the primary extract, performing molecular distillation to obtain cannabidiol concentrate, and performing supercritical fluid chromatographic separation on the cannabidiol concentrate for purification to obtain cannabidiol which does not contain tetrahydrocannabinol and has mass purity of more than 99%.
2. The method according to claim 1, wherein the industrial cannabis in step 1) comprises flowers, leaves, stems, roots and/or fruits of industrial cannabis.
3. The method of claim 1, wherein the drying device in step 2) comprises an oven, a baking tray, a steam heat exchanger, and/or an air supply device.
4. The method as claimed in claim 1, wherein the drying temperature in step 2) is 120-180 ℃ and the drying time is 10-50 minutes.
5. The method according to claim 1, wherein in step 2), the water content of the dried raw material is less than 8 mass%.
6. The method as claimed in claim 1, wherein the pulverizing in step 3) comprises pulverizing the dried raw material by a pulverizer to a 80-mesh-sieve-passing rate of not less than 95% (by mass), and a 60-mesh-sieve-passing rate of 100%.
7. The method as claimed in claim 1, wherein the re-drying in step 4) is performed at a temperature of 110 ℃ and 140 ℃ for a time of 10-20 minutes.
8. The method according to claim 1, wherein the re-drying in step 4 is carried out so that the water content of the dried raw material is less than 5% by mass.
9. The method according to claim 1, wherein the micronization in step 5) comprises pulverizing the raw material having a water content of less than 5% by mass to a size of 200 mesh or more to ensure sufficient cell wall breakage of the raw material.
10. The method according to claim 1, wherein in step 6) the granulation is carried out with a particle size of Φ 2mm x (5-8) mm.
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