CN111662163A - Application of organic membrane in hemp extraction - Google Patents
Application of organic membrane in hemp extraction Download PDFInfo
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- CN111662163A CN111662163A CN202010453768.XA CN202010453768A CN111662163A CN 111662163 A CN111662163 A CN 111662163A CN 202010453768 A CN202010453768 A CN 202010453768A CN 111662163 A CN111662163 A CN 111662163A
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- 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
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Abstract
The invention belongs to the field of membrane separation, and particularly relates to application of an organic membrane in hemp extraction. An application of organic membrane in extracting Cannabis sativa comprises extracting Cannabis sativa with organic solvent, sequentially filtering with microporous membrane and non-porous organic membrane, collecting filtrate, and recovering solvent to obtain Cannabis sativa extract. The invention adopts a special organic membrane as a non-porous membrane, the separation of the non-porous membrane is mainly dominated by molecular solubility, but not diffusibility, and the membrane filtration separation is carried out on the extracting solution, so that a series of problems caused by low-temperature freezing extraction/winterization treatment can be solved at one time.
Description
Technical Field
The invention belongs to the field of membrane separation, and particularly relates to application of an organic membrane in hemp extraction.
Background
Cannabidiol (CBD) is the main chemical component in medicinal plant marijuana, is extracted from female marijuana plant, is a non-addictive component in marijuana, and has pharmacological effects of resisting spasm, anxiety and inflammation.
At present, the cannabidiol extraction process comprises a freezing extraction step or a winterization step, the freezing extraction at (-50 ℃) has high requirements on equipment, the requirements on equipment heat preservation, sealing and related accessories are high, and the consumption of vulnerable parts is increased. The equipment needs to be insulated when winterization treatment is carried out at (-40 ℃), the winterization time is generally 48 hours, and a large amount of solvent storage tank equipment needs to be occupied. Centrifugation or filtration is needed after winterization, and the operation of the treatment process is complicated. The removal rate of the product pigment and wax after freezing extraction or winterization treatment is about 70-80%, and a large amount of impurities exist in the product, so that the subsequent further separation and purification are influenced.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides the application of the organic membrane in the extraction of the hemp, and the specific organic membrane is used as a separation medium, so that the prepared product has good and stable quality, the extraction operation is simple and convenient, the cost is low, and the production process is clean and environment-friendly.
The purpose of the invention is realized by the following technical scheme:
the application of an organic membrane in hemp extraction comprises the following steps:
extracting the hemp raw material by using an organic solvent, sequentially carrying out microfiltration membrane filtration and non-porous organic membrane filtration, collecting filtrate, and recovering the solvent to obtain the hemp extract.
Preferably, in the above technical solution, the organic solvent is any one of methanol, ethanol, acetone, n-hexane, n-heptane and ethyl acetate.
Preferably, in the above technical solution, the pore size of the microporous filter membrane is 0.1-50 μm.
Preferably, in the above technical solution, the non-porous organic film is a polyimide composite film.
Preferably, in the above technical solution, the non-porous organic film is a silicon-coated polyimide composite film.
Preferably, in the above technical solution, the membrane pressure difference of the non-porous organic membrane is 0.5-2.0 Mpa.
Preferably, in the above technical scheme, in the non-porous organic membrane filtration process, the temperature of the liquid to be filtered is 20 ℃ to 55 ℃.
Preferably, in the above technical solution, in the non-porous organic membrane filtration process, when the volume ratio of the membrane permeated solution to the membrane non-permeated solution is greater than 5, an organic solvent is added for thorough washing.
Preferably, in the above technical solution, in the non-porous organic membrane filtration process, when the volume ratio of the membrane permeated solution to the membrane non-permeated solution is greater than 10, an organic solvent is added for thorough washing.
Preferably, in the above technical solution, the amount of the organic solvent added is 1-5 times of the volume of the solution that does not permeate the membrane.
The invention adopts a special organic membrane as a non-porous membrane, the separation of the non-porous membrane is mainly dominated by molecular solubility, but not diffusibility, and the membrane filtration separation is carried out on the extracting solution, so that a series of problems caused by low-temperature freezing extraction/winterization treatment can be solved at one time.
The method can be used for extracting the cannabidiol at room temperature, only common extraction equipment is used, the membrane occupies less equipment, the equipment investment is reduced, and meanwhile, the energy consumption is saved by more than 60%. The winterization process is eliminated, the process time is greatly shortened from the original 48 hours to 12 hours. The organic membrane separation replaces the steps of freezing, winterization and centrifugation, the obtained product has lighter color, the removal rate of pigment and wax reaches more than 95%, fewer impurities and higher purity, the product quality is improved, the subsequent further separation and purification steps are simplified, the production efficiency is improved, and the production cost of the product is reduced by 40% in total.
The method for separating the cannabidiol by using the organic membrane has the characteristics of high speed and high recovery rate. The method has the advantages of reasonable design, safe and reliable process, simple operation and good popularization and use values.
Drawings
FIG. 1 is a color schematic of the hemp extract of the present invention and winterization/freezing extraction, wherein the left flask contains membrane-treated hemp extract and the right flask contains winterization/freezing extract.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the embodiments of the present invention are not limited to the scope of the examples. These examples are intended to illustrate the invention only and are not intended to limit the scope of the invention. In addition, various modifications may occur to those skilled in the art upon reading the present disclosure, and such equivalent variations are within the scope of the present invention as defined in the appended claims.
Example 1
Pulverizing 1Kg of hemp flower leaf raw material into 80 mesh powder by a pulverizer, adding 8L of methanol, extracting at room temperature, and filtering the extractive solution with 10 μm microporous membrane filter to obtain a first filtrate. Pumping the first filtrate into an organic membrane filter, wherein the organic membrane is a polyimide composite membrane (non-porous membrane) (membrane brand: EVONIK, membrane type number: Puramem), controlling the membrane pressure difference to be 1.0Mpa, controlling the temperature of the liquid to be filtered to be 40 ℃, carrying out membrane filtration, adding a methanol solvent with 3 times volume of the solution which does not permeate the membrane for thorough washing when the volume ratio of the solution which permeates the membrane to the solution which does not permeate the membrane is 6, combining the filtrate and the washing solution, and recovering the solvent until the solvent is completely recovered to obtain 116g of the hemp extract.
Example 2
Pulverizing 1Kg of hemp flower leaf raw material into 80 mesh powder by a pulverizer, adding 8L of ethanol, extracting at room temperature, and filtering the extractive solution with 30 μm microporous membrane filter to obtain a first filtrate. Pumping the first filtrate into an organic membrane filter, wherein the organic membrane is a silicon-coated polyimide composite membrane (non-porous membrane) (membrane brand: EVONIK, membrane type number: Puramem), controlling the membrane pressure difference to be 1.2Mpa, controlling the temperature of the liquid to be filtered to be 45 ℃, carrying out membrane filtration, adding an ethanol solvent with 3 times volume of the solution which does not permeate the membrane for thorough washing when the volume ratio of the solution which permeates the membrane to the solution which does not permeate the membrane is 7, combining the filtrate and the washing liquid, and recovering the solvent until the solvent is completely recovered to obtain 119g of the hemp extract.
Example 3
Pulverizing 1Kg of hemp flower leaf raw material into 80 mesh powder by a pulverizer, adding 8L of acetone, extracting at room temperature, and filtering the extractive solution with a 15 μm microporous membrane filter to obtain a first filtrate. Pumping the first filtrate into an organic membrane filter, wherein the organic membrane is a polyimide composite membrane (non-porous membrane), controlling the membrane pressure difference to be 1.0Mpa, controlling the temperature of the liquid to be filtered to be 55 ℃, carrying out membrane filtration, adding an acetone solvent with the volume 2 times that of the solution which does not permeate the membrane for washing when the volume ratio of the solution which permeates the membrane to the solution which does not permeate the membrane is 8, combining the filtrate and the washing solution, and recovering the solvent until the solvent is completely recovered to obtain 117g of the hemp extract.
Example 4
Pulverizing 1Kg of hemp flower leaf raw material into 80 mesh powder by a pulverizer, adding 8L of n-hexane, extracting at room temperature, and filtering the extract with a 20 μm microporous membrane filter to obtain a first filtrate. Pumping the first filtrate into an organic membrane filter, wherein the organic membrane is a silicon coating polyimide composite membrane (non-porous membrane), controlling the membrane pressure difference to be 1.2Mpa, controlling the temperature of the liquid to be filtered to be 42 ℃, carrying out membrane filtration, adding n-hexane solvent with the volume 4 times that of the solution which does not permeate the membrane for washing when the volume ratio of the solution which permeates the membrane to the solution which does not permeate the membrane is 9, combining the filtrate and the washing solution, and recovering the solvent until the solvent is completely recovered to obtain 120g of the hemp extract.
Example 5
Pulverizing 1Kg of hemp flower leaf raw material into 80 mesh powder by a pulverizer, adding 8L of n-heptane for room temperature extraction, and filtering the extractive solution with 0.1 μm microporous membrane filter to obtain first filtrate. Pumping the first filtrate into an organic membrane filter, wherein the organic membrane is a silicon coating polyimide composite membrane (non-porous membrane), controlling the membrane pressure difference to be 0.5Mpa, controlling the temperature of the liquid to be filtered to be 20 ℃, carrying out membrane filtration, adding an n-heptane solvent with the volume 1 time of that of the solution which does not permeate the membrane to carry out permeation when the volume ratio of the solution which permeates the membrane to the solution which does not permeate the membrane is 10, combining the filtrate and the permeation solution, and recovering the solvent until the solvent is completely recovered to obtain 122g of the hemp extract.
Example 6
Pulverizing 1Kg of hemp flower leaf raw material into 80 mesh powder by a pulverizer, adding 8L of ethyl acetate, extracting at room temperature, and filtering the extract with a 50 μm microporous membrane filter to obtain a first filtrate. Pumping the first filtrate into an organic membrane filter, wherein the organic membrane is a polyimide composite membrane (non-porous membrane), controlling the membrane pressure difference to be 2.0Mpa, controlling the temperature of the liquid to be filtered to be 55 ℃, carrying out membrane filtration, adding an ethyl acetate solvent with the volume 5 times that of the solution which does not permeate the membrane for washing when the volume ratio of the solution which permeates the membrane to the solution which does not permeate the membrane is 11, combining the filtrate and the washing solution, and recovering the solvent until the solvent is completely recovered to obtain 118g of the hemp extract.
Comparative example 1
Pulverizing 1Kg of folium Cannabis raw material to 80 mesh with a pulverizer, adding 8L of ethanol, freezing at low temperature (-50 deg.C) for extraction, and filtering the extractive solution with 30 μm microporous membrane filter to obtain extractive solution. Recovering solvent from the extractive solution to obtain Cannabis sativa extract 130 g.
Comparative example 2
Pulverizing 1Kg of folium Cannabis raw material into 80 mesh powder with a pulverizer, adding 8L of ethanol, extracting at room temperature, and filtering the extractive solution with 30 μm microporous membrane filter to obtain extractive solution. Freezing the extractive solution in a freezing jacketed tank for 48 hr, centrifuging to remove precipitate to obtain filtrate, and recovering solvent to obtain cannabis extract 128 g.
Comparative example 3
Pulverizing 1Kg of folium Cannabis raw material into 80 mesh powder with a pulverizer, adding 8L of ethanol, reflux extracting, and filtering the extractive solution with 20 μm microporous membrane filter to obtain extractive solution. Freezing the extractive solution in a freezing jacketed tank for 48 hr, centrifuging to remove precipitate to obtain filtrate, recovering solvent to obtain hemp extract 135g
It was observed that the hemp extract solutions obtained in examples 1 to 6 were light in color and contained relatively little amount of impurities, the hemp extract solutions obtained in comparative examples 1 to 3 were dark in color and contained relatively much amount of impurities, and the cannabidiol content by weight was measured after the solvent was recovered from the extract solutions, and the specific results are shown in table 1.
TABLE 1 Properties of the products obtained by the different extraction methods and the resulting cannabidiol contents
Item | Product color | Content of CBD | Recovery of CBD |
Room temperature extraction film treatment (example 1) | Light yellow | 64% | 92% |
Room temperature extraction film treatment (example 2) | Light yellow | 66% | 95% |
Room temperature extraction film treatment (example 3) | Light yellow | 65% | 93% |
Room temperature extraction film treatment (example 4) | Light yellow | 63% | 92% |
Room temperature extraction film treatment (example 5) | Light yellow | 66% | 96% |
Room temperature extraction film treatment (example 6) | Light yellow | 68% | 95% |
Freeze extraction (comparative example 1) | Brownish green color | 55% | 90% |
Extraction of winterization at Room temperature (comparative example 2) | Brownish green color | 56% | 82% |
Refluxing extraction winterization treatment (comparative example 3) | Brownish green color | 54% | 84% |
Table 1 shows that the process of the invention gives products with lighter colour and higher cannabidiol content and recovery of cannabis extracts than the freeze extraction or winterization process.
Claims (10)
1. Use of an organic film in hemp extraction, characterized in that it comprises the following steps:
extracting the hemp raw material by using an organic solvent, sequentially carrying out microfiltration membrane filtration and non-porous organic membrane filtration, collecting filtrate, and recovering the solvent to obtain the hemp extract.
2. The use of the organic film according to claim 1 for hemp extraction, wherein the organic solvent is any one of methanol, ethanol, acetone, n-hexane, n-heptane, ethyl acetate.
3. Use of an organic membrane according to claim 1 for hemp extraction, characterized in that the pore size of the microfiltration membrane is 0.1-50 μm.
4. Use of an organic membrane according to claim 1 in hemp extraction, characterized in that the non-porous organic membrane is a polyimide composite membrane.
5. Use of an organic film according to claim 1 in hemp extraction, characterized in that the non-porous organic film is a silicon coated polyimide composite film.
6. Use of an organic membrane according to any one of claims 1 to 5 for hemp extraction, wherein the non-porous organic membrane filtration has a membrane pressure difference of 0.5 to 2.0 MPa.
7. Use of an organic membrane according to any one of claims 1 to 5 for the extraction of cannabis, characterised in that during the filtration of the non-porous organic membrane the temperature of the liquid to be filtered is between 20 ℃ and 55 ℃.
8. Use of an organic membrane according to any one of claims 1 to 5 in hemp extraction, characterized in that during non-porous organic membrane filtration, when the ratio of the volume of membrane-permeated solution to the volume of membrane-non-permeated solution is greater than 5, an organic solvent is added for rinsing.
9. Use of an organic membrane according to claim 8 for hemp extraction, wherein an organic solvent is added for a diafiltration process at a membrane permeate to membrane non-permeate volume ratio of greater than 10 during non-porous organic membrane filtration.
10. Use of an organic membrane for hemp extraction according to claim 8, characterized in that the organic solvent is added in an amount of 1-5 times the volume of the membrane-impermeable solution.
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PCT/CN2020/097467 WO2021237841A1 (en) | 2020-05-26 | 2020-06-22 | Use of organic membrane in hemp extraction |
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WO2021237841A1 (en) * | 2020-05-26 | 2021-12-02 | 桂林莱茵生物科技股份有限公司 | Use of organic membrane in hemp extraction |
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