CN111116322A - Method for extracting cannabidiol beneficial to human health from industrial cannabis sativa - Google Patents
Method for extracting cannabidiol beneficial to human health from industrial cannabis sativa Download PDFInfo
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- CN111116322A CN111116322A CN201911239519.4A CN201911239519A CN111116322A CN 111116322 A CN111116322 A CN 111116322A CN 201911239519 A CN201911239519 A CN 201911239519A CN 111116322 A CN111116322 A CN 111116322A
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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
- C07C37/685—Processes comprising at least two steps in series
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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
- 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
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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
- C07C37/70—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment
- C07C37/74—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/16—Systems containing only non-condensed rings with a six-membered ring the ring being unsaturated
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/141—Feedstock
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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Abstract
The invention provides a method for extracting cannabidiol beneficial to human health from industrial cannabis sativa, which comprises the following steps: firstly, the method comprises the following steps: introducing CO2Converting the gas into liquid to make it reach supercritical state; II, secondly: processing the raw material industrial hemp to make it reach the required quality state; thirdly, the method comprises the following steps: supercritical CO2Dissolving the liquid in an extraction kettle and collecting an industrial hemp extract; extracting with a separation kettle and a special rectifying column to separate the extractive solution; fourthly, the method comprises the following steps: introducing CO2Liquid is reversed into the low pressure separator to make CO2The liquid is separated and enters a separation tank to quickly form gas-liquid separation; fifthly: CO 22The gas returns to the main storage tank, and the CBD oil is discharged from the separator，CO2Returning the gas to the extraction kettle for recycling; the extraction rate of CBD can reach more than 90 percent, the CBD content is 20-30 percent, the method is scientific, the manufacturability is good, and the method can be directly applied to cosmetics, health care products and medicine markets; reduce the environmental pollution of the product and achieve the purpose of organic green biological extraction.
Description
(I) technical field
The invention provides a method for extracting cannabidiol beneficial to human health from industrial cannabis, which relates to the extraction of CO2A supercritical method for extracting, separating and enriching cannabidiol from industrial hemp belongs to the technical field of biological extraction of effective components.
(II) background of the invention
Research shows that more than 130 cannabinoids are contained in cannabis, and most of cannabinoids have high application value. Of these, tetrahydrocannabinol (i.e., T H C) and cannabidiol (i.e., CBD) are two common cannabinoids. THC is a hallucinogenic addictive component of Cannabis sativa, and is classified into industrial Cannabis sativa (THC) according to content of THC<0.3 percent) and intermediate hemp (0.3 percent)<THC<0.5%) and recreational hemp (0.5%<THC is also known as narcotic cannabis). Unlike thc, cannabidiol, CBD, does not induce hallucinogenic addiction and is inhibitory to this "toxicity". CBD has high market value, and is widely used in medical field, and has the efficacies of relieving pain and inflammation, resisting epilepsy, resisting cancer, resisting anxiety, treating depression and the like; the product can be used in food, and has effects in improving sleep quality and immunity; can be used in skin care products, and has oxidation, antiinflammatory and acne removing effects. Cannabidiol, or "CBD", is usually present in decreasing amounts in each part of cannabis, in the order bract, flower, leaf, fine stem and coarse stem, with the highest amount in flowers and leaves of female plants. The most used extraction process of Cannabidiol (CBD) from industrial hemp in the prior art is solvent extraction method, such as n-hexane, petroleum ether, dichloromethane, chloroform and methanol, although the extraction rate of Cannabidiol (CBD) is improved, the use of organic solvent is harmful to the environment, and the solvent residue in the final product can not be removedThe safety of the product is influenced; the other is ethanol as an extractant, which reduces the toxicity of organic solvents, but has the problem of low extraction rate caused by low solubility of cannabidiol. Using supercritical CO2The fluid extraction technology applied to the extraction process of cannabidiol in recent years has the advantages of strong extraction capacity, high extraction rate, strong selectivity, good product quality and the like, but the extracted product still contains more impurities.
Disclosure of the invention
(1) Objects of the invention
In order to improve the purity of a target product, the invention separates and extracts the product by using a specially-prepared rectifying column in the process of supercritical extraction of carbon dioxide, thereby reducing the content of organic impurities such as pigment, wax and the like, effectively and quickly extracting cannabidiol, namely CBD, obviously improving the extraction rate, separating the organic impurities (such as chlorophyll, wax and the like) and reducing the product pollution.
(2) Technical scheme
The invention provides a method for extracting cannabidiol beneficial to human health from industrial cannabis sativa, which comprises the following specific implementation steps:
the method comprises the following steps: introducing CO2Converting the gas into liquid to make it reach supercritical state; the method comprises the following steps:
① production of CO in a compression chamber2Reducing the temperature to below-56 deg.C, increasing the pressure to over 75MPa, and introducing CO2Converting the gas into liquid;
② increasing the temperature and pressure to over 31 deg.C and 7.38MPa until CO is obtained2The liquid becomes "supercritical" state; the supercritical CO2Liquid is able to fill the container while maintaining density (liquid state); when CO is present2When the liquid is in a supercritical state, it is the most ideal choice for chemical extraction because it does not cause denaturation or damage;
step two: the raw material "industrial hemp" is treated to achieve the desired quality state by the following:
① drying or baking industrial hemp flowers and leaves in full-bloom stage to make water content within a specified range and ash content below the required specification, vacuum drying at a temperature and for a time within the required range to make water content within the required range;
② pulverizing dried industrial hemp flower and leaf with pulverizer to obtain desired fineness (mesh);
step three: supercritical CO2Dissolving the liquid in an extraction kettle and collecting plant (namely industrial hemp) extract;
extracting with a separation kettle and a rectifying column to separate the extractive solution; the specific situation is as follows:
① filling the pretreated industrial hemp flowers and leaves with CO2The liquid is in an extraction kettle in a supercritical state;
② due to CO2The liquid is in a supercritical state, fully contacts with the industrial hemp material, and is extracted in an extraction kettle at specified temperature and pressure to form extraction liquid;
③ pumping appropriate amount of ethanol into the extraction kettle via solvent pump to increase solubility of the extractive solution and increase extraction rate;
④ controlling the extraction liquid to enter the separation kettle through a valve, adjusting the pressure and temperature of the separation kettle to separate the extraction liquid in the separation kettle;
⑤ the extraction liquid in the separation kettle is controlled by a valve to enter a special rectification column, the proper pressure and temperature in the rectification column are adjusted, the CBD in the industrial hemp extraction liquid is enriched at a step under the temperature and the pressure, and the extraction rate of the CBD is effectively improved;
step four: CO to be liquid2The plant extract will automatically be extracted from the CO by the valve control back into the low pressure separator2Separating out the liquid; supercritical fluid for extracting solute at certain temperature and pressure enters the separating tank through the expansion valve, and the pressure is reduced to make CO2The liquid turns into gas and forms gas-liquid separation with the extract (industrial hemp plant liquid, namely CBD oil) rapidly;
step five: CO 22The gas is returned to the main tank and the extract (CBD oil) is discharged from the separator under reduced pressure, CO2The gas is returned to the extraction kettle for recycling through a compressor.
Wherein, the industrial hemp flower and leaf described in the second step ① has moisture content of 15-20% and soil content of less than 5% after sun drying or baking drying, and is dried under vacuum at 150-180 ℃ for 20-40 minutes to ensure that the moisture content of the industrial hemp flower and leaf is 5-8%.
Wherein, in the step two ②, the dried industrial hemp flowers and leaves are crushed by a crusher, and the crushing degree reaches 10 to 15 meshes.
Wherein in step three ② the term "due to CO" is used2The liquid is in supercritical state, and is fully contacted with industrial hemp material, and is extracted in an extraction kettle at a specified temperature and pressure to form an extract liquid, wherein the specified temperature is 50 ℃, and the pressure is 30 Mpa.
Wherein, in the step three ④, the extraction liquid is fed into the separation kettle under the control of a valve, and the pressure and the temperature of the separation kettle are adjusted to separate the extraction liquid in the separation kettle, wherein the pressure is 12MPa, and the temperature is 50 ℃.
Wherein, in the step three ⑤, the extraction liquid in the separation kettle, namely the extraction liquid, is controlled by a valve to enter a special rectification column, the proper pressure and temperature in the rectification column are adjusted, the CBD in the industrial hemp extraction liquid is further enriched under the temperature and the pressure, the extraction content extraction rate of the CBD is effectively improved, and the proper pressure and temperature in the rectification column are 15Mpa and 50 ℃.
Wherein, the rectification column in the step three ⑤ is a special device specially made for the invention (another patent application), and the main function of the rectification column is to ensure the purity and extraction rate of the product CBD.
(3) Compared with the prior art, the invention has the advantages that:
the method has the advantages that data display is carried out in the implementation, the CBD extraction rate can reach more than 90%, the method is scientific, and the manufacturability is good; the content of CBD is 20-30%. Chlorophyll, wax and the like in the plant can be effectively removed, 50-60% of unsaturated fatty acid and 9-11% of terpenoid are contained in the extract, and the extract product can be directly applied to cosmetics, health care products and medicine markets after being treated. The method has the advantages of improving the extraction rate of CBD, avoiding using a large amount of organic solvents (such as ethanol, petroleum ether and the like) in the production process, reducing the environmental pollution of products, achieving the purpose of organic green biological extraction, and saving a plurality of steps and cost for the post-treatment of industrial hemp extraction.
(IV) description of the drawings
FIG. 1 is a flow chart of the method of the present invention.
(V) detailed description of the preferred embodiments
The invention discloses a method for extracting cannabidiol beneficial to human health from industrial cannabis sativa, which is shown in figure 1 and comprises the following specific implementation steps:
the method comprises the following steps: introducing CO2Converting the gas into liquid to make it reach supercritical state; the method comprises the following steps:
① production of CO in a compression chamber2Reducing the temperature to below-56 ℃ and increasing the pressure to above 75psi to convert the CO to CO2Converting the gas into liquid;
② increasing temperature and pressure until CO2The liquid becomes "supercritical" state; the supercritical CO2Liquid is able to fill the container while maintaining density (liquid state); when CO is present2When the liquid is in a supercritical state, it is the most ideal choice for chemical extraction because it does not cause denaturation or damage;
step two: the raw material "industrial hemp" is treated to achieve the desired quality state by the following:
① drying or baking industrial hemp flower and leaf in full-bloom stage to water content of 15-20% and soil content below 5%, vacuum drying at 150-180 deg.C for 20-40 min to water content of 5-8%;
② pulverizing dried industrial hemp flower and leaf with pulverizer to 10-15 mesh;
step three: supercritical CO2Dissolving the liquid in an extraction kettle and collecting plant (namely industrial hemp) extract; extracting with a separation kettle and a rectifying column, and separatingSeparating the extract; the specific situation is as follows:
① filling the pretreated industrial hemp flowers and leaves with CO2The liquid is in an extraction kettle in a supercritical state;
② due to CO2The liquid reaches a supercritical state, fully contacts with industrial hemp material introduced into an extraction kettle, and is extracted at the temperature of 50 ℃ and the pressure of 30Mpa to form extraction liquid;
③ pumping appropriate amount of ethanol into the extraction kettle via solvent pump to increase solubility of the extractive solution and increase extraction rate;
④ controlling the extraction liquid to enter the separation kettle via valve, adjusting the pressure (12 Mpa) and temperature (50 deg.C) of the separation kettle, and separating the extraction liquid in the separation kettle;
⑤ the extraction liquid in the separation kettle is controlled by a valve to enter a special equipment rectification column, the proper pressure (15 Mpa) and temperature (50 ℃) in the rectification column are adjusted, the target substance is further extracted, the equipment rectification column is special equipment specially made for the invention (another patent application), and the main function of the equipment rectification column is to ensure the purity and extraction rate of the product cannabidiol CBD.
Step four: CO to be liquid2The plant extract will automatically be extracted from the CO by the valve control back into the low pressure separator2Separating out the liquid; supercritical fluid for extracting solute at certain temperature and pressure enters the separating tank through the expansion valve, the pressure is reduced, and CO is made to flow2The liquid turns into gas and forms gas and liquid separation rapidly with the extract (industrial hemp plant liquid, namely CBD oil);
step five: CO 22Returning the gas to the main storage tank, discharging CBD oil from the separator under reduced pressure, discharging extract (CBD oil) from the separator under reduced pressure, and discharging CO2The gas is returned to the extraction kettle for recycling through a compressor.
Claims (6)
1. A method for extracting cannabidiol beneficial to human health from industrial cannabis sativa is characterized by comprising the following steps: the specific implementation steps are as follows:
the method comprises the following steps: will be provided withCO2Converting the gas into liquid to make it reach supercritical state; the method comprises the following steps:
① production of CO in a compression chamber2Reducing the temperature to below-56 deg.C, increasing the pressure to over 75MPa, and introducing CO2Converting the gas into liquid;
② increasing the temperature and pressure to over 31 deg.C and 7.38MPa until CO is obtained2The liquid becomes "supercritical" state; the supercritical CO2The liquid is able to fill the container while maintaining the density, i.e. liquid state; when CO is present2When the liquid is in a supercritical state, the liquid is the most ideal choice for chemical extraction, because the liquid does not cause denaturation and damage;
step two: the raw material "industrial hemp" is treated to achieve the desired quality state by the following:
① drying and baking industrial hemp flowers and leaves in full-bloom stage to make water content in a specified range and ash content below the required specification, vacuum drying at a temperature and for a time within the required range to make water content in the required range;
② pulverizing dried industrial hemp flower and leaf with pulverizer to obtain desired degree of pulverization;
step three: supercritical CO2Dissolving the liquid in an extraction kettle and collecting the plant, namely the industrial hemp extract; extracting with a separation kettle and a rectifying column to separate the extractive solution; the specific situation is as follows:
① filling the pretreated industrial hemp flowers and leaves with CO2The liquid is in an extraction kettle in a supercritical state;
② due to CO2The liquid is in a supercritical state, fully contacts with the industrial hemp material, and is extracted in an extraction kettle at specified temperature and pressure to form extraction liquid;
③ pumping required amount of ethanol into the extraction kettle by solvent pump to increase solubility of the extractive solution and increase extraction rate;
④ controlling the extraction liquid to enter the separation kettle through a valve, adjusting the pressure and temperature of the separation kettle to separate the extraction liquid in the separation kettle;
⑤ the extraction liquid in the separation kettle is controlled by a valve to enter a special rectification column, the pressure and temperature required in the rectification column are adjusted, the CBD in the industrial hemp extraction liquid is enriched at a step under the temperature and pressure, and the extraction rate of the CBD is improved;
step four: CO to be liquid2The plant extract will automatically be extracted from the CO by the valve control back into the low pressure separator2Separating out the liquid; supercritical fluid for extracting solute at a preset temperature and pressure enters a separation tank through an expansion valve, and the pressure is reduced to change C02 liquid into gas, and the gas and the liquid are rapidly separated from the extract;
step five: CO 22The gas is returned to the main storage tank, and the extract, i.e. CBD oil, is discharged from the separator under reduced pressure, CO2The gas is returned to the extraction kettle for recycling through a compressor.
2. The method as claimed in claim 1, wherein the moisture content of the "industrial hemp flower and leaf" obtained in step two ① is 15-20% and the soil ash content is less than 5% after sun drying and oven drying, and the moisture content of the industrial hemp flower and leaf is 5-8% after vacuum drying at 150-180 ℃ for 20-40 min.
3. The method of claim 1, wherein the crushing degree of the dried industrial hemp flowers and leaves by the crusher is 10-15 mesh in step two ②.
4. The process of claim 1 wherein said cannabidiol is "due to CO" at step III ②2The liquid is in supercritical state, and is fully contacted with industrial hemp material, and is extracted in an extraction kettle at a specified temperature and pressure to obtain extractive solution, wherein the specified temperature is 50 deg.C, and the pressure is30Mpa。
5. The method of claim 1, wherein the extraction liquid is fed into the separation kettle under the control of a valve, and the pressure and temperature of the separation kettle are adjusted to separate the extraction liquid in the separation kettle at the temperature of 50 ℃ under the pressure of 12MPa in step III ④.
6. The method for extracting cannabidiol from industrial hemp for human health as claimed in claim 1, wherein the extraction liquid in the separation kettle is controlled by a valve and enters a special rectification column, the pressure and temperature required in the rectification column are adjusted, the CBD in the ingredients in the extraction liquid of industrial hemp is enriched uniformly at the temperature and pressure, the extraction rate of the CBD is improved, and the pressure required in the rectification column is 15Mpa and the temperature is 50 ℃.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112353717A (en) * | 2020-09-10 | 2021-02-12 | 广州新琪化妆品有限公司 | Plant anti-hair loss and hair-fixing shampoo containing industrial hemp extract |
| CN112811989A (en) * | 2021-02-09 | 2021-05-18 | 温州市金榜轻工机械有限公司 | Complete system and process for refining high-purity cannabidiol in industrial cannabis sativa |
| CN115028614A (en) * | 2022-05-30 | 2022-09-09 | 深圳天成铭道医学科技股份有限公司 | Method for extracting cannabinol from industrial cannabis sativa |
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| CN112353717A (en) * | 2020-09-10 | 2021-02-12 | 广州新琪化妆品有限公司 | Plant anti-hair loss and hair-fixing shampoo containing industrial hemp extract |
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