CN115028614A - Method for extracting cannabinol from industrial cannabis sativa - Google Patents

Method for extracting cannabinol from industrial cannabis sativa Download PDF

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Publication number
CN115028614A
CN115028614A CN202210600835.5A CN202210600835A CN115028614A CN 115028614 A CN115028614 A CN 115028614A CN 202210600835 A CN202210600835 A CN 202210600835A CN 115028614 A CN115028614 A CN 115028614A
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liquid
extraction
pressure
extracting
industrial hemp
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周禹州
莫建红
李勇
胡宗辰
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Shenzhen Tiancheng Mingdao Medical Technology Co ltd
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Shenzhen Tiancheng Mingdao Medical Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07DHETEROCYCLIC COMPOUNDS
    • C07D311/00Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings
    • C07D311/02Heterocyclic compounds containing six-membered rings having one oxygen atom as the only hetero atom, condensed with other rings ortho- or peri-condensed with carbocyclic rings or ring systems
    • C07D311/78Ring systems having three or more relevant rings
    • C07D311/80Dibenzopyrans; Hydrogenated dibenzopyrans
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals
    • Y02P20/54Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

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  • Organic Chemistry (AREA)
  • Extraction Or Liquid Replacement (AREA)

Abstract

The invention provides a method for extracting cannabinol from industrial cannabis sativa, which comprises the following steps: firstly, the method comprises the following steps: converting CO2 gas into liquid to reach supercritical state; II, secondly: processing the raw material industrial hemp to make it reach the required quality state; thirdly, the steps of: dissolving the supercritical CO2 liquid in an extraction kettle and collecting the industrial hemp extract; extracting with a separation kettle and a special rectifying column to separate extractive solution; fourthly, the method comprises the following steps: the CO2 liquid is reversely fed into a low-pressure separator, so that the CO2 liquid is separated and enters a separation tank to quickly form gas-liquid separation; fifthly: returning CO2 gas to the main storage tank, discharging CBN oil in the separator, and returning CO2 gas to the extraction kettle for recycling; the extraction rate of CBN by the method can reach more than 90 percent, the CBN content is 10-20 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

Method for extracting cannabinol from industrial cannabis sativa
Technical Field
The invention provides a method for extracting cannabinol from industrial hemp, relates to a method for extracting, separating and enriching cannabinol by applying CO2 supercritical extraction to industrial hemp, and belongs to the technical field of biological extraction of effective components.
Background
Research shows that more than 130 cannabinoids are contained in cannabis, and most of cannabinoids have high application value. Of these, tetrahydrocannabinol (i.e., thc) and cannabinol (i.e., CBN) are two common cannabinoids. THC is a hallucinogenic addictive component of marijuana, and is classified into industrial marijuana (THC < 0.3%), intermediate marijuana (0.3% < THC < 0.5%) and recreational marijuana (0.5% < THC, also known as narcotic marijuana) according to the content of THC. Unlike T H C, cannabinol, the "CBN", is not hallucinogenic to addiction, and is inhibitory to this "toxicity". CBN has high market value, and can be widely used in medical field, and has effects in relieving pain and inflammation, resisting epilepsy, resisting cancer, resisting anxiety, and treating depression; 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. Cannabinol, or "CBN", is typically 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 extracting cannabinol (namely CBN) from industrial hemp is a solvent extraction method, such as n-hexane, petroleum ether, dichloromethane, chloroform, methanol and the like, although the extraction rate of the cannabinol (namely CBN) is improved, the use of an organic solvent can harm the environment, and the solvent residue in a final product cannot be removed completely, so that the 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 cannabinol. By applying the supercritical CO2 fluid extraction technology, the method has the advantages of strong extraction capability, high extraction rate, strong selectivity, good product quality and the like in the extraction process of cannabinol in recent years, but the extracted product still contains more impurities.
Disclosure of Invention
The invention aims to improve the purity of a target product, and the invention utilizes a specially-prepared rectifying column to separate and extract the product in the supercritical carbon dioxide extraction process, thereby reducing the content of organic impurities such as pigment, wax and the like, effectively and quickly extracting cannabinol, namely CBN, remarkably improving the extraction rate, separating the organic impurities (such as chlorophyll, wax and the like) and reducing the product pollution.
The invention provides a method for extracting cannabinol from industrial cannabis sativa, which comprises the following specific implementation steps:
the method comprises the following steps: converting CO2 gas into liquid to reach supercritical state; the method comprises the following steps: preparing CO2 in a compression chamber, reducing the temperature to below 56 ℃ below zero, increasing the pressure to over 75Mpa, and converting CO2 gas into liquid; secondly, increasing the temperature and the pressure to ensure that the temperature exceeds 31 ℃ and the pressure exceeds 7.38Mpa until the CO2 liquid becomes a supercritical state; the supercritical CO2 liquid is capable of filling the container while maintaining the density (liquid state); when the CO2 liquid is in a supercritical state, it is the most desirable 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: firstly, industrial hemp flowers and leaves in a full-bloom stage are dried in the sun or baked to ensure that the water content is in a specified range and the ash soil content is below a required specification; vacuum drying at required temperature and time to make the water content in the required range; secondly, crushing the dried industrial hemp flowers and leaves by a crusher to reach the required degree of crushing (mesh);
step three: dissolving supercritical CO2 liquid in extraction kettle, and collecting plant (industrial hemp) extractive solution; extracting with a separation kettle and a rectifying column to separate the extractive solution; the concrete conditions are as follows: firstly, putting the pretreated industrial hemp flowers and leaves into an extraction kettle in which CO2 liquid is in a supercritical state; secondly, because the CO2 liquid is in a supercritical state and is fully contacted with the industrial hemp material, extracting in an extraction kettle at a specified temperature and pressure to form an extraction liquid; pumping proper amount of ethanol into the extraction kettle via a solvent pump to increase the solubility of the extract liquid and increase the extraction rate; fourthly, the extract liquid enters a separation kettle under the control of a valve, and the pressure and the temperature of the separation kettle are adjusted to separate the extract liquid in the separation kettle; fifthly, the extracting solution in the separation kettle, namely the extracting solution enters a special rectifying column through valve control, the proper pressure and temperature in the rectifying column are adjusted, the CBN in the ingredients in the industrial hemp extracting solution is enriched at a step under the temperature and the pressure, and the extraction rate of the CBN is effectively improved;
step four: the CO2 which becomes liquid is inverted into a low-pressure separator through a valve control, and the plant extracting solution is automatically separated from the CO2 liquid; supercritical fluid for extracting solute at certain temperature and pressure enters a separation tank through an expansion valve, and the pressure is reduced to change CO2 liquid into gas, and the gas and the liquid are rapidly separated from an extract (industrial hemp plant liquid, namely CBN oil);
step five: the CO2 gas is returned to the main storage tank, the extract (CBN oil) is discharged from the separator under the condition of pressure reduction, and the CO2 gas is returned to the extraction kettle for recycling through a compressor.
Wherein, after the industrial hemp flowers and leaves in the second step are dried in the sun or baked, the moisture content is between 15 and 20 percent, and the content of the soil is below 5 percent; vacuum drying at 150-180 deg.c for 20-40 min; the water content of the industrial hemp flowers and leaves is between 5 and 8 percent.
Wherein, in the second step, the dried industrial hemp flowers and leaves are crushed by a crusher, and the crushing degree reaches 10 to 15 meshes.
Wherein, in the third step, the CO2 liquid is in a supercritical state, fully contacts with the industrial hemp material, and is extracted in the extraction kettle under the specified temperature and pressure to form the extraction liquid, the specified temperature is 50 ℃, and the pressure is 30 Mpa.
Wherein, in the step III, the extraction liquid is controlled by a valve to enter the separation kettle, 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 third-fifth step, the extracting solution in the separating kettle, namely the extracting solution, is controlled by a valve to enter a special rectifying column, the proper pressure and temperature in the rectifying column are adjusted, the CBN in the industrial hemp extracting solution is further enriched under the temperature and the pressure, the extraction rate of the CBN is effectively improved, and the proper pressure and temperature in the rectifying column are 15Mpa and 50 ℃.
Wherein, the equipment in the third-fifth step is special equipment specially made for the invention (another patent application), and the main function of the equipment is to ensure the purity and extraction rate of the product 'cannabinol, namely CBN'.
The invention has the advantages that: the data of the method in implementation shows that the extraction rate of CBN can reach more than 90%, the method is scientific, and the manufacturability is good; the content of CBN 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 high extraction rate of CBN, no use of large amount of organic solvent (such as ethanol, petroleum ether, etc.) during production, reduced environmental pollution, and reduced steps and cost for post-treatment of industrial hemp.
Drawings
FIG. 1 is a flow chart of the method of the present invention.
Detailed Description
The invention discloses a method for extracting cannabinol from industrial cannabis sativa, which is shown in figure 1 and comprises the following specific implementation steps:
the method comprises the following steps: converting CO2 gas into liquid to reach supercritical state; the method comprises the following steps: preparing CO2 in a compression chamber, reducing the temperature to below-56 ℃, increasing the pressure to over 75psi, and converting CO2 gas into liquid; secondly, the step of: increasing the temperature and pressure until the CO2 liquid becomes "supercritical" state; the supercritical CO2 liquid is capable of filling the container while maintaining the density (liquid state); when the CO2 liquid is in a supercritical state, it is the most desirable 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: firstly, industrial hemp flowers and leaves in a full-bloom stage are dried in the sun or baked to ensure that the moisture is between 15 and 20 percent and the content of soil is below 5 percent, and then are dried in vacuum at the temperature of between 150 and 180 ℃ for 20 to 40 minutes to ensure that the moisture of the industrial hemp flowers and leaves is between 5 and 8 percent; secondly, crushing the dried industrial hemp flowers and leaves by a crusher to reach 10-15 meshes;
step three: dissolving supercritical CO2 liquid in extraction kettle, and collecting plant (industrial hemp) extractive solution; extracting with a separation kettle and a rectifying column to separate the extractive solution; the concrete conditions are as follows: firstly, filling the pretreated industrial hemp flowers and leaves into an extraction kettle in which CO2 liquid is in a supercritical state; secondly, because the CO2 liquid reaches a supercritical state, the CO2 liquid is fully contacted with the industrial hemp material introduced into the extraction kettle, and extraction is carried out at the temperature of 50 ℃ and the pressure of 30Mpa to form extraction liquid; pumping proper amount of ethanol into the extraction kettle via a solvent pump to increase the solubility of the extract liquid and increase the extraction rate; controlling the extraction liquid to enter a separation kettle through a valve, adjusting the pressure (12 Mpa) and the temperature (50 ℃) of separation kettle equipment, and separating the extraction liquid from the separation kettle; fifthly, the extracting solution in the separation kettle, namely the extracting solution enters a special device, namely a rectifying column through valve control, the proper pressure (15 Mpa) and temperature (50 ℃) in the rectifying column are adjusted
Step four: the CO2 which becomes liquid is inverted into a low-pressure separator through a valve control, and the plant extracting solution is automatically separated from the CO2 liquid; supercritical fluid for extracting solute at certain temperature and pressure enters a separation tank through an expansion valve, the pressure is reduced, CO2 liquid is changed into gas, and the gas and the liquid are rapidly separated from an extract (industrial hemp plant liquid, namely CBN oil);
step five: and returning CO2 gas to the main storage tank, discharging the CBN oil from the separator under the condition of pressure drop, discharging an extract (CBN oil) from the separator under the condition of pressure drop, and returning CO2 gas to the extraction kettle for recycling through a compressor.

Claims (3)

1. A method for extracting cannabinol from industrial cannabis sativa is characterized in that: the specific implementation steps are as follows:
the method comprises the following steps: converting CO2 gas into liquid to reach supercritical state; the method comprises the following steps: preparing CO2 in a compression chamber, reducing the temperature to below 56 ℃ below zero, increasing the pressure to over 75Mpa, and converting CO2 gas into liquid; secondly, increasing the temperature and the pressure to ensure that the temperature exceeds 31 ℃ and the pressure exceeds 7.38Mpa until the CO2 liquid becomes a supercritical state; the supercritical CO2 liquid is capable of filling a container while maintaining a density, i.e., liquid state; when the CO2 liquid is in a supercritical state, the CO2 liquid is the most ideal choice for chemical extraction, because it does not cause denaturation and damage;
step two: the raw material "industrial hemp" is treated to achieve the desired quality state by the following: firstly, adopting industrial hemp flowers and leaves in the full-bloom stage, and drying in the sun and baking to ensure that the water content is within a specified range and the ash soil content is below a required specification; vacuum drying at required temperature and time to make the water content in the required range; secondly, crushing the dried industrial hemp flowers and leaves by a crusher to reach the required crushing degree;
step three: dissolving the supercritical CO2 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: firstly, filling the pretreated industrial hemp flowers and leaves into an extraction kettle in which CO2 liquid is in a supercritical state; secondly, because the CO2 liquid is in a supercritical state and is fully contacted with the industrial hemp material, extracting in an extraction kettle at a specified temperature and pressure to form an extraction liquid; pumping required amount of ethanol into the extraction kettle through a solvent pump, so that the solubility of the extraction liquid is increased, and the extraction rate is improved; fourthly, the extract liquid enters a separation kettle under the control of a valve, and the pressure and the temperature of the separation kettle are adjusted to separate the extract liquid in the separation kettle; fifthly, the extracting solution in the separation kettle, namely the extracting solution enters a special rectifying column through valve control, the pressure and the temperature required in the rectifying column are adjusted, the CBN in the ingredients in the industrial hemp extracting solution is enriched at a step under the temperature and the pressure, and the extraction rate of the CBN is improved;
step four: the liquid CO2 is inverted into a low-pressure separator through a valve control system, and the plant extract is automatically separated from the CO2 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: and the CO2 gas returns to the main storage tank, the extract, namely CBN oil is discharged from the separator under the condition of pressure reduction, and the CO2 gas returns to the extraction kettle through the compressor for recycling.
2. A method of extracting cannabinol from industrial cannabis sativa as claimed in claim 1, wherein: after the industrial hemp flowers and leaves are dried in the sun and baked in the second step, the moisture content is 15-20%, and the content of the soil is below 5%; vacuum drying at 150-180 deg.c for 20-40 min; the water content of the industrial hemp flowers and leaves is between 5 and 8 percent.
3. A method of cannabinol from industrial cannabis, as claimed in claim 1, wherein: in the second step, the dried industrial hemp flowers and leaves are crushed by a crusher, and the crushing degree is 10 to 15 meshes.
CN202210600835.5A 2022-05-30 2022-05-30 Method for extracting cannabinol from industrial cannabis sativa Pending CN115028614A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105505565A (en) * 2015-12-28 2016-04-20 贵州航天乌江机电设备有限责任公司 Method for extracting industrial hemp oil rich in cannabidiol
CN110314408A (en) * 2019-08-01 2019-10-11 昆明萃醍生物科技有限公司 A kind of extraction process of high-purity cannabidiol
CN111116322A (en) * 2019-12-06 2020-05-08 云南金碧地生物科技有限公司 Method for extracting cannabidiol beneficial to human health from industrial cannabis sativa
CN211311343U (en) * 2019-03-21 2020-08-21 大连博迈科技发展有限公司 Device for preparing high-purity cannabidiol from industrial cannabis sativa
CN111718243A (en) * 2019-03-21 2020-09-29 大连博迈科技发展有限公司 Device and method for preparing high-purity cannabidiol from industrial cannabis sativa
CN113754518A (en) * 2021-09-24 2021-12-07 云南绿新生物药业有限公司 Method for efficiently purifying cannabidiol from industrial cannabis sativa leaves

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105505565A (en) * 2015-12-28 2016-04-20 贵州航天乌江机电设备有限责任公司 Method for extracting industrial hemp oil rich in cannabidiol
CN211311343U (en) * 2019-03-21 2020-08-21 大连博迈科技发展有限公司 Device for preparing high-purity cannabidiol from industrial cannabis sativa
CN111718243A (en) * 2019-03-21 2020-09-29 大连博迈科技发展有限公司 Device and method for preparing high-purity cannabidiol from industrial cannabis sativa
CN110314408A (en) * 2019-08-01 2019-10-11 昆明萃醍生物科技有限公司 A kind of extraction process of high-purity cannabidiol
CN111116322A (en) * 2019-12-06 2020-05-08 云南金碧地生物科技有限公司 Method for extracting cannabidiol beneficial to human health from industrial cannabis sativa
CN113754518A (en) * 2021-09-24 2021-12-07 云南绿新生物药业有限公司 Method for efficiently purifying cannabidiol from industrial cannabis sativa leaves

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