CN112430496A - Method for extracting full-spectrum CBD oil from industrial hemp waste slag - Google Patents
Method for extracting full-spectrum CBD oil from industrial hemp waste slag Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/106—Production of fats or fatty oils from raw materials by extracting using ultra-sounds
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
- C11B1/108—Production of fats or fatty oils from raw materials by extracting after-treatment, e.g. of miscellae
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/001—Refining fats or fatty oils by a combination of two or more of the means hereafter
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/005—Refining fats or fatty oils by wave energy or electric current, e.g. electrodialysis
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/006—Refining fats or fatty oils by extraction
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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- C11B3/00—Refining fats or fatty oils
- C11B3/12—Refining fats or fatty oils by distillation
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- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
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- C11B3/00—Refining fats or fatty oils
- C11B3/16—Refining fats or fatty oils by mechanical means
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Abstract
The invention relates to a method for extracting full-spectrum CBD oil from industrial hemp waste slag, which comprises the steps of sequentially drying the industrial hemp waste slag, performing ultrasonic extraction treatment, filtering by a refrigeration plate frame filter, adding a physical settling agent for freezing and settling, then performing falling film concentration treatment, pure water cooling and settling, performing high-speed centrifugal separation, and performing alcohol precipitation treatment, dialysis filtration and ultrafiltration filtration to obtain a purified product; detecting the content of CBD and THC in the purified product to obtain a qualified product, and then placing the qualified product into a microwave density regulating device for microwave density controlAdjusting and controlling the density to obtain the density of 1.05-1.35 kg/m3The full spectrum CBD oil of (a). The CBD oil extraction method provided by the invention can be used for extracting cannabidiol from waste slag with low CBD content, so that the utilization rate of raw materials is improved.
Description
Technical Field
The invention relates to the technical field of industrial hemp extraction, in particular to a method for extracting full-spectrum CBD oil from industrial hemp waste slag.
Background
The industrial hemp refers to the hemp with the tetrahydrocannabinol content of less than 0.3 percent, the industrial hemp is called hemp (hemp) in China, is a 1-year-old herbaceous plant in the Cannabis genus (Cannabiaceae) in the Cannabiaceae family, and is divided into the industrial hemp and drug hemp, and the hemp widely applied at home and abroad is the industrial hemp at present. Tetrahydrocannabinol (THC) and Cannabidiol (CBD) are the two most prominent natural compounds in industrial cannabis, and they are isomers, because of the same spatial structure, they are highly susceptible to interconversion during the growth process, i.e. THC can be converted to CBD, which is also readily converted to THC. On the premise that THC is not out of specification (content < 0.3%), the higher the CBD yield, the better.
In the prior art, cannabidiol is usually extracted from cannabis sativa leaves, and in view of the existing extraction process, the yield of the extracted cannabidiol is about 0.4%, the purity is 95%, but the residual content of the cannabidiol in the generated waste slag is still high and reaches 0.5-0.6%, so that the waste of raw materials is caused.
Disclosure of Invention
Based on the above situation, the main object of the present invention is to provide a method for extracting full spectrum CBD oil from industrial hemp waste slag, so as to improve the utilization rate of raw materials.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the invention provides a method for extracting full-spectrum CBD oil from industrial hemp waste slag, which comprises the following steps:
s10: drying the waste slag after the extraction of the industrial hemp to obtain dry slag;
s20: mixing the dry slag with an ethanol solution, and performing ultrasonic extraction treatment to obtain an extract liquid;
s30: filtering the extract liquor by a refrigeration plate-frame filter, and adding a physical settling agent for freezing and settling to obtain primary supernatant;
s40: carrying out falling film concentration treatment on the primary supernatant to obtain a fluid extract;
s50: diluting the fluid extract by using pure water, stirring to dissolve the fluid extract, and then cooling and settling to obtain secondary supernatant;
s60: carrying out high-speed centrifugal separation on the secondary supernatant to obtain a separation filtrate;
s70: adding ethanol into the separated filtrate, and performing alcohol precipitation treatment to obtain supernatant for three times;
s80: carrying out dialysis filtration on the third supernatant to obtain a dialysis membrane separation solution;
s90: carrying out ultrafiltration filtration on the dialysis membrane separation liquid to obtain a purified product;
s100: detecting the content of CBD and THC in the purified product, and if the content of CBD is more than or equal to 80% and the content of THC is less than 0.3%, judging the purified product to be a qualified product;
s110: putting the qualified product into a microwave density regulating and controlling device for microwave density regulation and control to obtain the product with the density of 1.05-1.35 kg/m3The full spectrum CBD oil of (a).
Preferably, the drying temperature of the drying treatment in the S10 is 60-100 ℃, and the drying time is 24-48 hours; the moisture content of the obtained dry slag is 3-5%.
Preferably, the solid-to-liquid ratio of the dry slag to the ethanol solution in the step S20 is 1: (10-20); the concentration of the ethanol solution is 40-95%; and the ultrasonic countercurrent extraction treatment in the S20 adopts a tubular multistage ultrasonic countercurrent extraction device.
Preferably, the temperature of the frozen settlement in the S30 is lower than-15 ℃, and the standing time is 6-18 hours.
Preferably, the density of the fluid extract obtained in S40 is 1.25-1.35 kg/m3。
Preferably, the S50 is specifically:
s51: mixing the fluid extract with pure water with the mass 2-3 times of that of the fluid extract, and stirring to dissolve the fluid extract to obtain a mixed solution;
s52: and cooling the mixed solution to-15 to-30 ℃, and standing for 6 to 18 hours to obtain the secondary supernatant.
Preferably, the speed of high-speed centrifugal separation in the S60 is 3500 r/min-50000 r/min.
Preferably, the S70 is specifically:
s71: according to the solid-liquid ratio of 1: (6-10) adding 40-95% (v/v) ethanol into the separation solution according to the proportion to obtain an ethanol mixed solution;
s72: and standing the ethanol mixed solution for 6-18 hours at the temperature of-15 to-30 ℃ to obtain supernatant liquid for three times.
Preferably, the dialysis treatment in S80 adopts an 80-120kD dialysis membrane;
in the S90, the ultrafiltration membrane of V62-7640H is selected for ultrafiltration.
Preferably, the S100 further includes:
and if the content of CBD is less than 80 percent or the content of THC is more than or equal to 0.3 percent, taking the purified product as a fluid extract, and returning to S50.
The CBD oil extraction method adopts the modes of multiple sedimentation and multiple membrane filtration, greatly reduces the content of HTC, and reserves the cannabidiol with the molecular weight of 500-1500. Obviously, the method can extract the cannabidiol from the waste slag with low content of CBD, thereby improving the utilization rate of raw materials.
Other advantages of the present invention will be described in the detailed description, and those skilled in the art will understand the technical features and technical solutions presented in the description.
Drawings
Preferred embodiments of the present invention will be described below with reference to the accompanying drawings. In the figure:
FIG. 1 is a flow chart of a preferred embodiment of the present invention.
Detailed Description
The present invention will be described below based on examples, but the present invention is not limited to only these examples. In the following detailed description of the present invention, certain specific details are set forth in order to avoid obscuring the nature of the present invention, well-known methods, procedures, and components have not been described in detail.
Further, those of ordinary skill in the art will appreciate that the drawings provided herein are for illustrative purposes and are not necessarily drawn to scale.
Unless the context clearly requires otherwise, throughout the description and the claims, the words "comprise", "comprising", and the like are to be construed in an inclusive sense as opposed to an exclusive or exhaustive sense; that is, what is meant is "including, but not limited to".
In the description of the present invention, it is to be understood that the terms "first," "second," and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance. In addition, in the description of the present invention, "a plurality" means two or more unless otherwise specified.
In the industrial hemp preparation, Cannabidiol (CBD) is directly extracted from plants such as hemp flower leaves and the like, a lot of slag is left due to the limitation of preparation processes and equipment, the content of the cannabidiol in the slag is still high, but the content of the cannabidiol in the waste slag is greatly reduced relative to the content of raw materials such as hemp flower leaves and the like, so that the direct adoption of the existing cannabidiol extraction method cannot be realized.
In order to improve the utilization rate of raw materials, the application provides a method for extracting full-spectrum CBD oil from industrial hemp waste slag, as shown in figure 1, comprising the following steps:
s10: drying the waste slag after the extraction of the industrial hemp to obtain dry slag;
s20: mixing the dry slag with an ethanol solution, and performing ultrasonic extraction treatment to obtain an extract liquid;
s30: filtering the extract liquor by a refrigeration plate-frame filter, and adding a physical settling agent for freezing and settling to obtain primary supernatant;
s40: carrying out falling film concentration treatment on the primary supernatant to obtain a fluid extract;
s50: diluting the fluid extract by using pure water, stirring to dissolve the fluid extract, and then cooling and settling to obtain secondary supernatant;
s60: carrying out high-speed centrifugal separation on the secondary supernatant to obtain a separation filtrate;
s70: adding ethanol into the separated filtrate, and performing alcohol precipitation treatment to obtain supernatant for three times;
s80: carrying out dialysis filtration on the third supernatant to obtain a dialysis membrane separation solution;
s90: carrying out ultrafiltration filtration on the dialysis membrane separation liquid to obtain a purified product;
s100: detecting the content of CBD and THC in the purified product, and if the content of CBD is more than or equal to 80% and the content of THC is less than 0.3%, judging the purified product to be a qualified product;
s110: putting the qualified product into a microwave density regulating and controlling device for microwave density regulation and control to obtain the product with the density of 1.05kg/m3～1.35kg/m3Of a full spectrum of CBD oils, e.g. having a density of 1.05kg/m3、1.10kg/m3、1.15kg/m3、1.16kg/m3、1.17kg/m3、1.18kg/m3、1.19kg/m3、1.20kg/m3、1.21kg/m3、1.22kg/m3、1.23kg/m3、1.24kg/m3、1.25kg/m3、1.26kg/m3、1.27kg/m3、1.28kg/m3、1.29kg/m3、1.30kg/m3、1.31kg/m3、1.32kg/m3、1.33kg/m3、1.34kg/m3、1.35kg/m3。
The CBD oil extraction method adopts the modes of ultrasonic tube type multistage countercurrent extraction, multiple sedimentation and multiple membrane filtration, greatly reduces the HTC content, and retains the cannabidiol with the molecular weight of 500-1500. Obviously, the method can extract the cannabidiol from the waste slag with low content of CBD, thereby improving the utilization rate of raw materials.
Specifically, the drying temperature of the drying treatment in the step S10 is 60-100 ℃, and the drying time is 24-48 hours; the moisture content of the obtained dry slag is 3-5%. For example, the extraction rate of CBD can be improved by drying the waste slag after extraction of industrial hemp by the conventional process in a baking oven at 60 ℃, 65 ℃, 70 ℃, 75 ℃, 80 ℃, 85 ℃, 90 ℃, 95 ℃ or 100 ℃ for 24 hours, 25 hours, 26 hours, 27 hours, 28 hours, 29 hours, 30 hours, 31 hours, 32 hours, 33 hours, 34 hours, 35 hours, 36 hours, 37 hours, 38 hours, 39 hours, 40 hours, 41 hours, 42 hours, 43 hours, 44 hours, 45 hours, 46 hours, 47 hours or 48 hours to a moisture content of 3%, 4% or 5%.
In one embodiment, the solid-to-liquid ratio of the dry slag to the ethanol solution in S20 is 1 (10-20); the concentration of the ethanol solution is 40-95%; and the ultrasonic countercurrent extraction treatment in the S20 adopts a tubular multistage ultrasonic countercurrent extraction device. Namely, drying the slag according to the solid-liquid ratio of 1:10. 1:10.5, 1:11, 1:11.5, 1:12, 1:12.5, 1:13, 1:13.5, 1:14, 1:14.5, 1:15, 1:15.5, 1:16, 1:16.5, 1:17, 1:17.5, 1:18, 1:18.5, 1:19, 1:19.5 or 1:20 to 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90% or 95% ethanol, followed by ultrasonic counter-current extraction. Wherein, the power of the ultrasonic extraction device can be 300W-3000W, such as 300W, 400W, 500W, 600W, 700W, 800W, 900W, 1000W, 1100W, 1200W, 1300W, 1400W, 1500W, 1600W, 1700W, 1800W, 1900W, 2000W, 2100W, 2200W, 2300W, 2400W, 2500W, 2600W, 2700W, 2800W, 2900W or 3000W, the frequency is 20 KHZ-40 KHZ for automatic tracking, such as 20KHZ, 30KHZ and 40KHZ for selection.
The temperature of the frozen settlement in the S30 is lower than-15 ℃, and is preferably-15 ℃ to-30 ℃; and standing for 6-18 hours. Specifically, S30 may be: the extraction liquid enters a freezing and settling tank through a refrigeration type plate frame filter, when the extraction liquid is cooled to-15 ℃, -16 ℃, -17 ℃, -18 ℃, -19 ℃, -20 ℃, -21 ℃, -22 ℃, -23 ℃, -24 ℃, -25 ℃, -26 ℃, -27 ℃, -28 ℃, -29 ℃ or-30 ℃, a physical settling agent is added, and the extraction liquid is frozen and kept standing for 6 hours, 7 hours, 8 hours, 9 hours, 10 hours, 11 hours, 12 hours, 13 hours, 14 hours, 15 hours, 16 hours, 17 hours or 18 hours and the like, so that the effect of removing impurities is achieved, and primary supernatant is obtained.
The density of the fluid extract obtained in the step S40 is 1.25-1.35 kg/m3E.g. a density of 1.25kg/m3、1.26kg/m3、1.27kg/m3、1.28kg/m3、1.29kg/m3、1.30kg/m3、1.35kg/m3、1.32kg/m3、1.33kg/m3、1.34kg/m3、1.35kg/m3And the like. S40 specifically includes: adding primary supernatant from the top of a concentrator, uniformly feeding the primary supernatant into a heating pipe under the action of a feed liquid distributor, allowing the primary supernatant to flow downwards naturally along the inner wall of the pipe in a film shape under the action of the rapid flow of secondary steam and the gravity of the material, heating the primary supernatant to evaporate and concentrate continuously, allowing the concentrated feed liquid and the secondary steam to enter a separator for separation, discharging the secondary steam from the top of the separator, discharging the concentrated material from the bottom, and recording the concentrate as fluid extract.
The S50 specifically includes:
s51: mixing the fluid extract with pure water with the mass 2-3 times of that of the fluid extract, wherein the mass ratio of the fluid extract to the pure water is 1:2, 1:2.1, 1:2.2, 1:2.3, 1:2.4, 1:2.5, 1:2.6, 1:2.7, 1:2.8, 1:2.9 or 1:3.0, and the like, and stirring to fully dissolve the fluid extract to obtain a mixed solution;
s52: cooling the mixed solution to-15 to-30 ℃, such as-15 ℃, 16 ℃, 17 ℃, 18 ℃, 19 ℃, 20 ℃, 21 ℃, 22 ℃, 23 ℃, 24 ℃, 25 ℃, 26 ℃, 27 ℃, 28 ℃, 29 ℃, 30 ℃ and the like, freezing and standing for 6 to 18 hours, such as 6 hours, 7 hours, 8 hours, 9 hours, 10 hours, 11 hours, 12 hours, 13 hours, 14 hours, 15 hours, 16 hours, 17 hours, 18 hours and the like, and obtaining secondary supernatant.
With the above method, impurities can be removed as much as possible, and since tetrahydrocannabinol is slightly soluble in water, most of it can be removed.
In a preferred embodiment, the speed of high speed centrifugation in S60 is 3500 r/min-50000 r/min, such as 3500r/min, 4000r/min, 4500r/min, 5000r/min, 5500r/min, 6000r/min, 6500r/min, 7000r/min, 7500r/min, 8000r/min, 8500r/min, 9000r/min, 9500r/min, 10000r/min, 40000r/min, 40500r/min, 41000r/min, 41500r/min, 42000r/min, 42500r/min, 43000r/min, 43500r/min, 44000r/min, 44500r/min, 45000r/min, 49000r/min, 49500r/min, 50000r/min, etc.
The S70 specifically includes:
s71: according to the solid-liquid ratio of 1: (6-10) adding 40-95% (v/v) ethanol into the separation liquid to obtain an ethanol mixed liquid, wherein the ethanol mixed liquid is selected from 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, 80%, 85%, 90%, 95% ethanol, and the like, and the solid-to-liquid ratio is 1:6, 1:7, 1:7.5, 1:8, 1:9, 1:10, and the like;
s72: and standing the ethanol mixed solution for 6 to 18 hours, such as 6 hours, 7 hours, 8 hours, 9 hours, 10 hours, 11 hours, 12 hours, 13 hours, 14 hours, 15 hours, 16 hours, 17 hours, 18 hours and the like at the temperature of-15 to-30 ℃, such as-15 to-16 to-17 to-18 to-19 to-20 to-21 to-22 to-23 to-24 to-25 to-26 to-27 to-28 to-29 to-30 ℃ to obtain a supernatant for three times.
By adopting the arrangement, the HTC can be better removed by utilizing the characteristic that the HTC is dissolved in water, and the content of the HTC in the extracted cannabidiol is further reduced.
Performing membrane filtration on the supernatant of the third time in the extraction method, and performing segmentation interception, wherein in S80, a dialysis membrane of 80-120kD, such as 80kD, 100kD, 110kD, and 120kD, is selected for dialysis treatment; in S90, the ultrafiltration membrane of V62-7640H is selected for ultrafiltration. Specifically, the supernatant obtained in the third time passes through a dialysis membrane of 80-120kD, and small molecular substances in the solute are diffused from a high-concentration solution to a low-concentration solution through a semipermeable membrane until the osmotic pressure reaches an equilibrium. Due to the selectivity of the porous membrane, small molecular substances in the solute can pass through, larger substances are intercepted, the components with the molecular weight of 4000-; then the separated liquid of the dialysis membrane passes through an ultrafiltration membrane of V62-7640H, so that macromolecules are intercepted, and the full-spectrum CBD oil with the molecular weight of 500-1500 is intercepted, and a purified product is obtained.
S100, when the purified product is detected, some of the purified product becomes a qualified product, but there may be some unqualified products, and for this reason, in a preferred embodiment of the present invention, S100 further includes: and if the CBD content is less than 80 percent or the THC content is more than 3 percent, the purified product is regarded as an unqualified product, the unqualified purified product is taken as a fluid extract and returned to S50, namely the unqualified product is subjected to S50-S100 in sequence until the unqualified product becomes a qualified product.
Specifically, S100 can be detected by an online monitoring device such as an Agilent 1260 II high performance liquid chromatograph, and if the CBD content is more than or equal to 80% and the THC content is less than 0.3%, the product is qualified; and if the CBD content is less than 80 percent or the THC content is more than or equal to 0.3 percent, detecting that the product is unqualified, and returning the unqualified product to the step S50 of pure water sedimentation for retreatment.
S110 specifically comprises placing qualified product in a microwave density control device (such as ZS1-AV6518) for microwave density control to obtain a product with density of 1.05-1.35 kg/m3The broad spectrum CBD oil of (a).
The obtained full spectrum CBD oil contains CBD, other cannabinoids, lipid, flavonoid, terpene and aromatic compounds, and has hemp plant taste. For example, the obtained broad-spectrum CBD oil can be dissolved in an organic solvent such as PG/VG and sufficiently mixed with a coating solution, and used for the preparation of a tobacco sheet in the coating step. Improve the sensory smoking quality of the tobacco sheet, and increase the quality and the fragrance quantity of the fragrance.
It should be noted that the ranges of various temperatures, contents, etc. given above are only one preferred embodiment of each step, and are not limited to the ranges in practice.
The following description will be made with reference to specific examples.
Example 1
Drying materials: and (3) placing the waste slag after the industrial hemp is extracted in a baking oven at 70 ℃ for drying for 32 hours to obtain dry slag, wherein the moisture content of the dry slag is 3% according to the determination of a moisture determination method.
Organic extraction: and putting the dried qualified dry slag into an ultrasonic downstream extraction device, and adding 75% (v/v) ethanol according to the solid-liquid ratio of 1:12 to perform ultrasonic downstream extraction.
Freezing and settling: filtering the extract liquid by a refrigeration type plate-and-frame filter to obtain an extraction filtrate, adding a physical settling agent when the extraction filtrate entering a freezing settling tank is cooled to the temperature of-15 ℃, freezing and standing for 12 hours to obtain primary supernatant.
Falling film concentration: adding primary supernatant from the top of the concentrator, uniformly feeding into a heating pipe under the action of a feed liquid distributor, allowing the materials to naturally flow downwards along the inner wall of the pipe under the action of rapid flow and gravity of secondary steam, heating, continuously evaporating and concentrating, separating the concentrated feed liquid and the secondary steam in a separator, discharging the secondary steam from the top of the separator, discharging the concentrated material from the bottom, and preparing into the product with the density of 1.28kg/m3The fluid extract of (1).
Pure water sedimentation: adding pure water with the mass 3 times of that of the obtained fluid extract, fully stirring uniformly and fully dissolving, cooling the dissolved solution to-18 ℃, standing for 15 hours, and performing re-precipitation to obtain secondary supernatant.
High-speed centrifugal separation and alcohol precipitation: and (3) taking the secondary supernatant, carrying out high-speed centrifugal separation under the condition that the rotating speed is 12000r/min to obtain separated filtrate, adding 75% (v/v) ethanol into the high-speed centrifugal separation filtrate according to the solid-liquid ratio of 1:8, and carrying out alcohol precipitation for 12 hours at the temperature of-15 ℃ to obtain tertiary supernatant.
Membrane filtration (dialysis membrane filtration and ultrafiltration membrane filtration): and (4) performing membrane filtration on the supernatant obtained after the three times of alcohol precipitation, and adopting sectional interception. Firstly, the supernatant fluid of the third time is dialyzed and filtered by a dialysis membrane (80-120kD), and small molecular substances in the solute are diffused from a high-concentration solution to a low-concentration solution through a semipermeable membrane until the osmotic pressure reaches the balance. At this time, the components with the molecular weight cut-off of about 5000 are obtained, and the dialysis membrane separation liquid is obtained. Then, the separated liquid of the dialysis membrane is filtered by an ultrafiltration membrane of V62-7640H, the ultrafiltration membrane is used as a filtering medium, substances with the volume larger than the surface micro-pore diameter of the membrane in the stock solution are intercepted on the liquid inlet side of the membrane under certain pressure to form concentrated liquid, and therefore, the purified product with the molecular weight cutoff below 1000 is realized, and the industrial hemp essential oil online product is obtained.
Online monitoring: the industrial hemp essential oil online product is detected by an online monitoring device, and the detection result shows that the product is qualified when the CBD content is 81% and the THC content is 0.120%, namely the purified product in the embodiment is a qualified product.
And (3) microwave density regulation: placing the qualified product in a density regulating device (ZS1-AV6518) for density regulation to 1.15kg/m3Then the full-spectrum CBD oil is obtained.
Example 2
Drying materials: and (3) placing the waste slag after the industrial hemp is extracted in a baking oven at 70 ℃ for drying for 32 hours to obtain dry slag, wherein the moisture content of the dry slag is 3% according to the determination of a moisture determination method.
Organic extraction: and putting the dried qualified slag into an ultrasonic (tubular and multistage) countercurrent extraction device, and adding 75% (v/v) ethanol according to the solid-liquid ratio of 1:12 to perform ultrasonic (tubular and multistage) countercurrent extraction.
Freezing and settling: filtering the extract liquid by a refrigeration type plate-and-frame filter to obtain an extraction filtrate, adding a physical settling agent when the extraction filtrate entering a freezing settling tank is cooled to the temperature of-15 ℃, freezing and standing for 12 hours to obtain primary supernatant.
Falling film concentration: adding primary supernatant from the top of the concentrator, uniformly feeding into a heating pipe under the action of a feed liquid distributor, allowing the materials to naturally flow downwards along the inner wall of the pipe under the action of rapid flow and gravity of secondary steam, heating, continuously evaporating and concentrating, separating the concentrated feed liquid and the secondary steam in a separator, discharging the secondary steam from the top of the separator, discharging the concentrated material from the bottom, and preparing into the product with the density of 1.28kg/m3The fluid extract of (1).
Pure water sedimentation: adding pure water with the mass 3 times of that of the obtained fluid extract, fully stirring uniformly and fully dissolving, cooling the dissolved solution to-18 ℃, standing for 15 hours, and performing re-precipitation to obtain secondary supernatant.
High-speed centrifugal separation and alcohol precipitation: and (3) taking the secondary supernatant, carrying out high-speed centrifugal separation under the condition that the rotating speed is 12000r/min to obtain separated filtrate, adding 75% (v/v) ethanol into the high-speed centrifugal separation filtrate according to the solid-liquid ratio of 1:8, and carrying out alcohol precipitation for 12 hours at the temperature of-15 ℃ to obtain tertiary supernatant.
Membrane filtration (dialysis membrane filtration and ultrafiltration membrane filtration): and (4) performing membrane filtration on the supernatant obtained after the three times of alcohol precipitation, and adopting sectional interception. Firstly, the supernatant fluid of the third time is dialyzed and filtered by a dialysis membrane (80-120kD), and small molecular substances in the solute are diffused from a high-concentration solution to a low-concentration solution through a semipermeable membrane until the osmotic pressure reaches the balance. At this time, the components with the molecular weight cut-off of about 5000 are obtained, and the dialysis membrane separation liquid is obtained. Then, the separated liquid of the dialysis membrane is filtered by an ultrafiltration membrane of V62-7640H, the ultrafiltration membrane is used as a filtering medium, substances with the volume larger than the surface micro-pore diameter of the membrane in the stock solution are intercepted on the liquid inlet side of the membrane under certain pressure to form concentrated liquid, and therefore, the purified product with the molecular weight cutoff below 1000 is realized, and the industrial hemp essential oil online product is obtained.
Online monitoring: detecting the industrial hemp essential oil online product by an online monitoring device (Agilent 1260 II high performance liquid chromatograph), and detecting the product as qualified when the detection result is that the CBD content is 90% and the THC content is 0.130%.
And (3) microwave density regulation: the qualified online product of the industrial hemp essential oil enters a density control device (ZS1-AV6518) for density control, and the density is controlled to be 1.15kg/m3Then the full-spectrum CBD oil is obtained.
Example 3 differs from example 1 in that:
the material is dried to ensure that the temperature in the baking oven is 65 ℃ and the drying time is 40 hours, and the moisture content of the obtained dried slag is 3.2 percent.
The solid-liquid ratio in the organic extraction is 1:14, and 72% (v/v) ethanol is adopted for ultrasonic cocurrent extraction.
The temperature of the frozen sedimentation is-20 ℃, and the frozen standing time is 15 hours.
Falling film concentration to obtain a density of 1.26kg/m3The fluid extract of (1).
Adding pure water 2.8 times of the fluid extract in the pure water sedimentation, cooling to-18 deg.C, and standing for 16 hr.
High-speed centrifugal separation and alcohol precipitation, wherein the high-speed centrifugal separation filtrate is added with 72% (v/v) of ethanol according to the solid-liquid ratio of 1:10, and alcohol precipitation is carried out for 15 hours at the temperature of minus 20 ℃.
Online monitoring: and (3) detecting the prepared purified product, wherein the detection result shows that the purified product is qualified when the CBD content is 83% and the THC content is 0.122%.
The microwave density is regulated to 1.18kg/m3Then the full-spectrum CBD oil is obtained.
Example 4 differs from example 3 in that:
the organic extraction adopts an ultrasonic (tubular, multistage) countercurrent extraction device to carry out countercurrent extraction.
And when the detection result of online monitoring is that the content of CBD is 91% and the content of THC is 0.133%, the product is detected to be qualified.
The density is still regulated to 1.18kg/m in the microwave density regulation3Then the full-spectrum CBD oil is obtained.
Example 5 differs from example 4 in that:
the drying temperature in the material drying is 60 ℃, the drying time is 48 hours, and the moisture content of the obtained dry slag charge is 5%.
Adding 40% (v/v) ethanol into the organic extraction according to the solid-liquid ratio of 1:10.
The temperature is reduced to-30 ℃ during freezing and sedimentation, and the mixture is kept stand for 6 hours.
The density of the product prepared in the falling film concentration is 1.25kg/m3The fluid extract of (1).
Adding pure water 2 times of the mass of the fluid extract during pure water sedimentation, cooling to-15 ℃, and standing for 6 hours.
The rotation speed in the high-speed centrifugal separation and alcohol precipitation is 3500r/min, 95% (v/v) ethanol is added into the filtrate in the high-speed centrifugal separation according to the solid-liquid ratio of 1:6, and alcohol precipitation is carried out for 6 hours at the temperature of minus 30 ℃, so as to obtain supernatant for three times.
Online monitoring: when the detection result shows that the content of CBD is 82% and the content of THC is 0.121%, the product is qualified, that is, the purified product in this embodiment is a qualified product.
The microwave density is regulated to 1.05kg/m3Then the full-spectrum CBD oil is obtained.
Example 6 differs from example 4 in that:
the drying temperature in the material drying is 100 ℃, the drying time is 24 hours, and the moisture content of the obtained dry slag charge is 4%.
95% (v/v) ethanol is added into the organic extraction according to the solid-liquid ratio of 1: 20.
The temperature is reduced to-25 ℃ during freezing and sedimentation, and the mixture is kept stand for 18 hours.
The density of the product prepared in the falling film concentration is 1.35kg/m3The fluid extract of (1).
Adding pure water 2 times of the mass of the fluid extract during pure water sedimentation, cooling to-30 ℃, and standing for 18 hours.
The rotation speed in the high-speed centrifugal separation and alcohol precipitation is 50000r/min, 40% (v/v) ethanol is added into the filtrate in the high-speed centrifugal separation according to the solid-liquid ratio of 1:7, and alcohol precipitation is carried out for 18 hours at the temperature of minus 25 ℃ to obtain supernatant for three times.
Online monitoring: when the detection result shows that the content of the CBD is 90% and the content of the THC is 0.131%, the detection result shows that the product is qualified, namely the purified product in the embodiment is a qualified product.
The microwave density is regulated to 1.35kg/m3Then the full-spectrum CBD oil is obtained.
Wherein, the comparative table of each example is shown in Table 1
TABLE 1
As can be seen from table 1, examples 1 and 3 are comparative examples, and examples 2, 4, 5 and 6 are specific examples of full-spectrum CBD oil extracted by the method provided by the present invention, it is obvious that both CBD content and THC content of full-spectrum CBD oil extracted by the method of the present invention are consistent with the application of industrial hemp, and especially, the CBD content is higher and the THC content is lower by the ultrasonic tubular multi-stage countercurrent extraction method in high-speed centrifugal separation.
The obtained full spectrum CBD oil contains CBD, other cannabinoids, terpenes and aromatic compounds, and has the plant taste of hemp. For example, the resulting full spectrum CBD oil may be dissolved in olive oil to make CBD oil e-cartridges.
It will be appreciated by those skilled in the art that the above-described preferred embodiments may be freely combined, superimposed, without conflict.
It will be understood that the embodiments described above are illustrative only and not restrictive, and that various obvious and equivalent modifications and substitutions for details described herein may be made by those skilled in the art without departing from the basic principles of the invention.
Claims (10)
1. A method for extracting full-spectrum CBD oil from industrial hemp waste slag is characterized by comprising the following steps:
s10: drying the waste slag after the extraction of the industrial hemp to obtain dry slag;
s20: mixing the dry slag with an ethanol solution, and performing ultrasonic extraction treatment to obtain an extract liquid;
s30: filtering the extract liquor by a refrigeration plate-frame filter, and adding a physical settling agent for freezing and settling to obtain primary supernatant;
s40: carrying out falling film concentration treatment on the primary supernatant to obtain a fluid extract;
s50: diluting the fluid extract by using pure water, stirring to dissolve the fluid extract, and then cooling and settling to obtain secondary supernatant;
s60: carrying out high-speed centrifugal separation on the secondary supernatant to obtain a separation filtrate;
s70: adding ethanol into the separated filtrate, and performing alcohol precipitation treatment to obtain supernatant for three times;
s80: carrying out dialysis filtration on the third supernatant to obtain a dialysis membrane separation solution;
s90: carrying out ultrafiltration filtration on the dialysis membrane separation liquid to obtain a purified product;
s100: detecting the content of CBD and THC in the purified product, and if the content of CBD is more than or equal to 80% and the content of THC is less than 0.3%, judging the purified product to be a qualified product;
s110: putting the qualified product into a microwave density regulating and controlling device for microwave density regulation and control to obtain the product with the density of 1.05-1.35 kg/m3The full spectrum CBD oil of (a).
2. The method according to claim 1, wherein the drying treatment in S10 is performed at a drying temperature of 60 ℃ to 100 ℃ for 24 to 48 hours; the moisture content of the obtained dry slag is 3-5%.
3. The method according to claim 1, wherein the solid-to-liquid ratio of the dry slag to the ethanol solution in S20 is 1: (10-20); the concentration of the ethanol solution is 40-95%; and the ultrasonic countercurrent extraction treatment in the S20 adopts a tubular multistage ultrasonic countercurrent extraction device.
4. The method according to claim 1, wherein the temperature of the frozen settlement in the S30 is lower than-15 ℃ and the standing time is 6-18 hours.
5. The method according to claim 1, wherein the fluid extract obtained in S40 has a density of 1.25-1.35 kg/m3。
6. The method according to claim 1, wherein S50 is specifically:
s51: mixing the fluid extract with pure water with the mass 2-3 times of that of the fluid extract, and stirring to dissolve the fluid extract to obtain a mixed solution;
s52: and cooling the mixed solution to-15 to-30 ℃, and standing for 6 to 18 hours to obtain the secondary supernatant.
7. The method according to claim 1, wherein the speed of the high-speed centrifugation in S60 is 3500 r/min-50000 r/min.
8. The method according to claim 1, wherein S70 is specifically:
s71: according to the solid-liquid ratio of 1: (6-10) adding 40-95% (v/v) ethanol into the separation solution according to the proportion to obtain an ethanol mixed solution;
s72: and standing the ethanol mixed solution for 6-18 hours at the temperature of-15 to-30 ℃ to obtain the third supernatant.
9. The method of claim 1, wherein in the S80 dialysis treatment, an 80-120kD dialysis membrane is selected;
in the S90, the ultrafiltration membrane of V62-7640H is selected for ultrafiltration.
10. The method of claim 1, wherein the S100 further comprises:
and if the content of CBD is less than 80 percent or the content of THC is more than or equal to 0.3 percent, taking the purified product as a fluid extract, and returning to S50.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113730952A (en) * | 2021-08-24 | 2021-12-03 | 浙江双子智能装备有限公司 | Method for extracting effective components of industrial hemp |
| RU2822573C1 (en) * | 2023-12-04 | 2024-07-09 | Ворошнин Сергей Григорьевич | Method of producing purified cannabidiol |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1691954A (en) * | 2002-08-14 | 2005-11-02 | Gw药品有限公司 | Extraction of pharmaceutically active cannabinoids from plant materials |
| WO2016153347A1 (en) * | 2015-03-23 | 2016-09-29 | Echo Pharmaceuticals B.V. | Cannabidiol isolate from industrial-hemp and use thereof in pharmaceutical and/or cosmetic preparations |
| CN109053388A (en) * | 2018-08-20 | 2018-12-21 | 上海昶健生物科技有限公司 | A method of extracting cannabidiol |
| US20190134122A1 (en) * | 2017-09-01 | 2019-05-09 | MariJ Pharmaceuticals, Inc. | Cultivation, Processing, and Synthesis of Cannabidiols |
-
2020
- 2020-01-13 CN CN202010032690.4A patent/CN112430496A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1691954A (en) * | 2002-08-14 | 2005-11-02 | Gw药品有限公司 | Extraction of pharmaceutically active cannabinoids from plant materials |
| WO2016153347A1 (en) * | 2015-03-23 | 2016-09-29 | Echo Pharmaceuticals B.V. | Cannabidiol isolate from industrial-hemp and use thereof in pharmaceutical and/or cosmetic preparations |
| US20190134122A1 (en) * | 2017-09-01 | 2019-05-09 | MariJ Pharmaceuticals, Inc. | Cultivation, Processing, and Synthesis of Cannabidiols |
| CN109053388A (en) * | 2018-08-20 | 2018-12-21 | 上海昶健生物科技有限公司 | A method of extracting cannabidiol |
Non-Patent Citations (1)
| Title |
|---|
| 孟胜男等: "《药剂学》", 30 September 2011, 上海科学技术出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113730952A (en) * | 2021-08-24 | 2021-12-03 | 浙江双子智能装备有限公司 | Method for extracting effective components of industrial hemp |
| RU2822573C1 (en) * | 2023-12-04 | 2024-07-09 | Ворошнин Сергей Григорьевич | Method of producing purified cannabidiol |
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