WO2021237841A1 - 一种有机膜在大麻提取中的应用 - Google Patents

一种有机膜在大麻提取中的应用 Download PDF

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WO2021237841A1
WO2021237841A1 PCT/CN2020/097467 CN2020097467W WO2021237841A1 WO 2021237841 A1 WO2021237841 A1 WO 2021237841A1 CN 2020097467 W CN2020097467 W CN 2020097467W WO 2021237841 A1 WO2021237841 A1 WO 2021237841A1
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membrane
organic
cannabis
extraction
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French (fr)
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宋云飞
李义军
赵军
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桂林莱茵生物科技股份有限公司
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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
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
    • A61K36/18—Magnoliophyta (angiosperms)
    • A61K36/185—Magnoliopsida (dicotyledons)
    • A61K36/60—Moraceae (Mulberry family), e.g. breadfruit or fig

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  • the invention belongs to the field of membrane separation, and specifically relates to an application of an organic membrane in cannabis extraction.
  • Cannabidiol (CBD for short) is the main chemical component in the medicinal plant cannabis. It is extracted from female cannabis plants. It is a non-addictive component in cannabis. It has anti-spasm, anti-anxiety, anti-inflammatory and other pharmacological effects.
  • the extraction process of cannabidiol includes freezing extraction or winterization steps.
  • Frozen extraction (-50°C) has high requirements for equipment, high requirements for equipment insulation, sealing and related accessories, and consumption of vulnerable parts Increase.
  • the use of winterization (-40°C) requires heat preservation of the equipment, and the winterization time is generally 48 hours, which requires a large amount of solvent storage tank equipment.
  • After winterization centrifugation or filtration is required, and the processing operation is cumbersome.
  • the removal rate of product pigment and wax is about 70% to 80%, and there will be a large number of impurities in the product, which will affect the subsequent further separation and purification.
  • the present invention provides an application of organic membranes in cannabis extraction.
  • a specific organic membrane is used as the separation medium to ensure good and stable product quality and make the extraction operation simple and cost-effective. Low, the production process is clean and environmentally friendly.
  • An application of organic film in cannabis extraction includes the following steps:
  • the microporous membrane filtration and the non-porous organic membrane filtration are carried out in sequence, the filtrate is collected, and the solvent is recovered to obtain the cannabis extract.
  • the organic solvent is any one of methanol, ethanol, acetone, n-hexane, n-heptane, and ethyl acetate.
  • the pore size of the microporous filter membrane is 0.1-50 ⁇ m.
  • the non-porous organic membrane is a polyimide composite membrane.
  • the non-porous organic film is a silicon-coated polyimide composite film.
  • the membrane pressure difference of the non-porous organic membrane filtration is 0.5-2.0Mpa.
  • the temperature of the liquid to be filtered is 20°C-55°C.
  • an organic solvent is added to wash through.
  • the amount of the organic solvent added is 1-5 times the volume of the membrane impermeable solution.
  • the invention adopts a special organic membrane as a non-porous membrane, and its separation is mainly dominated by molecular solubility rather than diffusivity.
  • the extraction liquid is separated by membrane filtration, which can solve a series of problems caused by low-temperature freezing extraction/wintering treatment at one time. .
  • the invention can extract cannabidiol at room temperature by using ordinary extraction equipment, the membrane occupies less equipment, reduces equipment investment, and saves energy consumption by more than 60%.
  • the winterization process is eliminated, and the process time is greatly shortened from the original 48 hours to 12 hours.
  • Organic membrane separation replaces freezing, winterization and centrifugation steps, the color of the resulting product is lighter, the removal rate of pigment and wax is more than 95%, the impurity is less, the purity is higher, the quality of the product is improved, and the subsequent process is simplified. Further separation and purification steps to improve production efficiency, so that the overall production cost of the product is reduced by 40%.
  • the method for separating cannabidiol by using organic membrane in the present invention has the characteristics of rapidness and high recovery rate.
  • the method has reasonable design, safe and reliable process, simple operation and good promotion and use value.
  • Figure 1 is a schematic diagram of the color of the cannabis extract obtained from the present invention and winterization/frozen extraction.
  • the liquid contained in the triangular flask on the left in the figure is the extracted liquid after membrane treatment, and the liquid contained in the triangular flask on the right is winterized/frozen. Extraction solution.
  • the organic membrane is a polyimide composite membrane (non-porous membrane) (membrane brand: EVONIK, membrane model: PuraMem), and the membrane pressure difference is controlled to be 1.0Mpa.
  • the temperature of the liquid is controlled to 40°C, and membrane filtration is performed.
  • the organic membrane is a silicon-coated polyimide composite membrane (non-porous membrane) (membrane brand: EVONIK, membrane model: PuraMem), and the membrane pressure difference is controlled to be 1.2Mpa, The temperature of the liquid to be filtered is controlled to 45°C and membrane filtration is performed.
  • the organic membrane is a polyimide composite membrane (non-porous membrane).
  • the membrane pressure difference is controlled to 1.0Mpa, and the temperature of the liquid to be filtered is controlled to 55°C for membrane filtration.
  • the organic membrane is a silicon-coated polyimide composite membrane (non-porous membrane).
  • the membrane pressure difference is controlled to 1.2Mpa, and the temperature of the liquid to be filtered is controlled to 42°C.
  • Membrane filtration when the ratio of the volume of the membrane permeated solution to the volume of the membrane impermeable solution is 9, add 4 times the volume of the membrane impermeable solution n-hexane solvent to wash through, combine the filtrate and the wash solution, and recover the solvent to complete 120g of hemp extract.
  • the organic membrane is a silicon-coated polyimide composite membrane (non-porous membrane).
  • the membrane pressure difference is controlled to 0.5Mpa, and the temperature of the liquid to be filtered is controlled to 20°C.
  • Membrane filtration when the ratio of the volume of the membrane permeated solution to the volume of the membrane impermeable solution is 10, add 1 times the volume of the membrane impermeable solution n-heptane solvent to wash through, combine the filtrate and wash liquid, and recover the solvent to completion 122 g of hemp extract was obtained.
  • the organic membrane is a polyimide composite membrane (non-porous membrane).
  • the membrane pressure difference is controlled to 2.0Mpa, and the temperature of the liquid to be filtered is controlled to 55°C for membrane filtration.
  • hemp flower and leaf raw material Take 1Kg of hemp flower and leaf raw material, first use a pulverizer to pulverize to 80 mesh, then add 8L ethanol for low-temperature freezing (-50°C) extraction, and pass the extract through a 30 ⁇ m microporous membrane filter to obtain the extract. After the extraction liquid recovers the solvent to completion, 130 g of hemp extract is obtained.
  • Example 1 Light yellow 64% 92% Room temperature extraction membrane treatment (Example 2) light yellow 66% 95% Room temperature extraction membrane treatment (Example 3) light yellow 65% 93% Room temperature extraction membrane treatment (Example 4) light yellow 63% 92% Room temperature extraction membrane treatment (Example 5) light yellow 66% 96% Room temperature extraction membrane treatment (Example 6) light yellow 68% 95% Frozen extraction (comparative example 1) Brown green 55% 90% Extract winterization treatment at room temperature (Comparative Example 2) Brown green 56% 82% Reflux extraction winterization treatment (comparative example 3) Brown green 54% 84%
  • Table 1 shows that, compared with freezing extraction or winterization treatment, the method of the present invention has a lighter color and higher cannabidiol content and recovery rate in the cannabis extract.

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Abstract

一种有机膜在大麻提取中的应用，是将大麻原料经过有机溶剂提取之后依次进行微孔滤膜过滤、非孔有机膜过滤，收集滤液、回收溶剂即得大麻提取物。采用特种有机膜为非孔膜，其分离主要由分子溶解性主导，而非扩散性，对提取液进行膜过滤分离，一次性可以解决低温冷冻提取/冬化处理带来的一系列问题。

Description

一种有机膜在大麻提取中的应用 技术领域
本发明属于膜分离领域，具体涉及一种有机膜在大麻提取中的应用。
背景技术
大麻二酚(简称CBD)是药用植物大麻中的主要化学成分，提取自雌性大麻植株，是大麻中的非成瘾性成分，具有抗痉挛、抗焦虑、抗炎等药理作用。
目前，大麻二酚提取过程包括冷冻提取或冬化步骤，冷冻提取(-50℃)对设备的要求很高，对设备保温、密封及相关配件的要求很高，且易损件的耗用量增大。采用冬化处理(-40℃)需要对设备进行保温处理，冬化时间一般为48小时，需要占用大量的溶剂储罐设备。冬化处理后需要进行离心或过滤处理，处理过程操作繁琐。冷冻提取或冬化处理后对产品色素及蜡质的去除率为70％～80％左右，产品中还会有大量的杂质存在，影响后续的进一步分离纯化。
公开于该背景技术部分的信息仅仅旨在增加对本发明的总体背景的理解，而不应当被视为承认或以任何形式暗示该信息构成已为本领域一般技术人员所公知的现有技术。
发明内容
为了解决上述现有技术的不足之处，本发明提供了一种有机膜在大麻提取中的应用，采用特定的有机膜作为为分离介质，确保制备所得产品质量良好稳定，使提取操作简便，成本低，生产过程清洁环保。
本发明的目的通过如下技术方案实现：
一种有机膜在大麻提取中的应用，包括以下步骤：
大麻原料经过有机溶剂提取之后依次进行微孔滤膜过滤、非孔有机膜过滤，收集滤液、回收溶剂即得大麻提取物。
优选地，上述技术方案中，所述有机溶剂为甲醇、乙醇、丙酮、正己烷、正庚烷、乙酸乙酯中的任意一种。
优选地，上述技术方案中，所述微孔滤膜孔径为0.1-50μm。
优选地，上述技术方案中，所述非孔有机膜为聚酰亚胺复合膜。
优选地，上述技术方案中，所述非孔有机膜为硅涂层聚酰亚胺复合膜。
优选地，上述技术方案中，所述非孔有机膜过滤的膜压差为0.5-2.0Mpa。
优选地，上述技术方案中，在非孔有机膜过滤过程中，待过滤液体温度为20℃-55℃。
优选地，上述技术方案中，在非孔有机膜过滤过程中，当膜透过溶液体积和膜未透过溶液体积比大于5时，加入有机溶剂透洗。
优选地，上述技术方案中，在非孔有机膜过滤过程中，当膜透过溶液体积和膜未透过溶液体积比大于10时，加入有机溶剂透洗。
优选地，上述技术方案中，所述有机溶剂加入量为膜未透过溶液1-5倍体积。
本发明采用特种有机膜为非孔膜，其分离主要由分子溶解性主导，而非扩散性，对提取液进行膜过滤分离，一次性可以解决低温冷冻提取/冬化处理带来的一系列问题。
本发明可室温条件下对大麻二酚进行提取，利用普通提取设备即可，膜占用设备少，降低了设备投入，同时能耗节省60％以上。去掉了冬化工艺，大大缩短了工艺时间，由原来的48小时缩短至12小时。有机膜分离替代了冷冻、冬化和离心步骤，所得产品的色泽更浅，色素和蜡质的去除率达到95％以上，杂质更少，纯度更高，提高了产品的品质，简化了后续的进一步分离纯化步骤，提高生产效率，使产品的生产成本总体下降了40％。
本发明利用有机膜分离大麻二酚的方法具有快速，高回收率的特性。该方法设计合理、工艺安全可靠，操作简单具有良好的推广使用价值。
附图说明
图1是本发明以及冬化/冷冻提取所得大麻提取液的颜色示意图，其中，图中左边三角瓶所盛放液体为膜处理后的提取液，右边三角瓶所盛放液体为冬化/冷冻提取液。
具体实施方式
下面结合具体实施例，对本发明作进一步详细的阐述，但本发明的实施方式并不局限于实施例表示的范围。这些实施例仅用于说明本发明，而非用于限制本发明的范围。此外，在阅读本发明的内容后，本领域的技术人员可以对本发明作各种修改，这些等价变化同样落于本发明所附权利要求书所限定的范围。
实施例1
取大麻花叶原料1Kg先用粉碎机打粉到80目，再加入8L甲醇进行室温提取，提取液过10μm微孔滤膜过滤器，得到第一滤液。将第一滤液泵入有机膜过滤器，所述的有机膜为聚酰亚胺复合膜(非孔膜)(膜品牌：EVONIK，膜型号：PuraMem)，控制膜压差1.0Mpa，将待过滤液体温度控制为40℃，进行膜过滤，当膜透过溶液体积和膜未透过溶液体积比为6，加入膜未透过溶液3倍体积的甲醇溶剂透洗，合并过滤液及透洗液，回收溶剂至完全后得到大麻提取物116g。
实施例2
取大麻花叶原料1Kg先用粉碎机打粉到80目，再加入8L乙醇进行室温提取，提取液过30μm微孔滤膜过滤器，得到第一滤液。将第一滤液泵入有机膜过滤器，所述的有机膜为硅涂层聚酰亚胺复合膜(非孔膜)(膜品牌：EVONIK，膜型号：PuraMem)，控制膜压差1.2Mpa，将待过滤液体温度控制为45℃，进行膜过滤，当膜透过溶液体积和膜未透过溶液体积比为7，加入膜未透过溶液3倍体积的乙醇溶剂透洗，合并过滤液及透洗液，回收溶剂至完全后得到大麻提取物119g。
实施例3
取大麻花叶原料1Kg先用粉碎机打粉到80目，再加入8L丙酮进行室温提取，提取液过15μm微孔滤膜过滤器，得到第一滤液。将第一滤液泵入有机膜过滤器，所述的有机膜为聚酰亚胺复合膜(非孔膜)，控制膜压差1.0Mpa，将待过滤液体温度控制为55℃，进行膜过滤，当膜透过溶液体积和膜未透过溶液体积比为8，加入膜未透过溶液2倍体积的丙酮溶剂透洗，合并过滤液及透洗液，回收溶剂至完全后得到大麻提取物117g。
实施例4
取大麻花叶原料1Kg先用粉碎机打粉到80目，再加入8L正己烷进行室温提取，提取液过20μm微孔滤膜过滤器，得到第一滤液。将第一滤液泵入有机膜过滤器，所述的有机膜为硅涂层聚酰亚胺复合膜(非孔膜)，控制膜压差1.2Mpa，将待过滤液体温度控制为42℃，进行膜过滤，当膜透过溶液体积和膜未透过溶液体积比为9，加入膜未透过溶液4倍体积的正己烷溶剂透洗，合并过滤液及透洗液，回收溶剂至完全后得到大麻提取物120g。
实施例5
取大麻花叶原料1Kg先用粉碎机打粉到80目，再加入8L正庚烷进行室温提取，提取液过0.1μm微孔滤膜过滤器，得到第一滤液。将第一滤液泵入有机膜过滤器，所述的有机膜为硅涂层聚酰亚胺复合膜(非孔膜)，控制膜压差0.5Mpa，将待过滤液体温度控制为20℃，进行膜过滤，当膜透过溶液体积和膜未透过溶液体积比为10，加入膜未透过溶液1倍体积的正庚烷溶剂透洗，合并过滤液及透洗液，回收溶剂至完全后得到大麻提取物122g。
实施例6
取大麻花叶原料1Kg先用粉碎机打粉到80目，再加入8L乙酸乙酯进行室温提取，提取液过50μm微孔滤膜过滤器，得到第一滤液。将第一滤液泵入有机膜过滤器，所述的有机膜为聚酰亚胺复合膜(非孔膜)，控制膜压差2.0Mpa，将待过滤液体温度控制为55℃，进行膜过滤，当膜透过溶液体积和膜未透过溶液体积比为11，加入膜未透过溶液5倍体积的乙酸乙酯溶剂透洗，合并过滤液及透洗液，回收溶剂至完全后得到大麻提取物118g。
对比例1
取大麻花叶原料1Kg先用粉碎机打粉到80目，再加入8L乙醇进行低温冷冻(-50℃)提取，将提取液过30μm微孔滤膜过滤器，得到提取液。提取液回收溶剂至完全后得到大麻提取物130g。
对比例2
取大麻花叶原料1Kg先用粉碎机打粉到80目，再加入8L乙醇进行常温提取，将提取液过30μm微孔滤膜过滤器，得到提取液。提取液置于冷冻夹套罐中冷冻处理48小时，离心除沉淀后得滤液，回收溶剂至完全后得到大麻提取物128g。
对比例3
取大麻花叶原料1Kg先用粉碎机打粉到80目，再加入8L乙醇进行回流提取，将提取液过20μm微孔滤膜过滤器，得到提取液。提取液置于冷冻夹套罐中冷冻处理48小时，离心除沉淀后得滤液，回收溶剂至完全后得到大麻提取物135g
经观察，实施例1-6所得的大麻提取液颜色较浅、对应的所含的杂质含量较少，对比例1-3所得大麻提取液颜色较深，对应的所含的杂质含量较多，提取液回收溶剂之后，进行大麻二酚重量含量检测，具体结果如表1所示。
表1 不同提取方法所得产品性状及所得大麻二酚含量
项目 产品颜色 CBD含量 CBD回收率
室温提取膜处理(实施例1) 浅黄色 64％ 92％
室温提取膜处理(实施例2) 浅黄色 66％ 95％
室温提取膜处理(实施例3) 浅黄色 65％ 93％
室温提取膜处理(实施例4) 浅黄色 63％ 92％
室温提取膜处理(实施例5) 浅黄色 66％ 96％
室温提取膜处理(实施例6) 浅黄色 68％ 95％
冷冻提取(对比例1) 棕绿色 55％ 90％
室温提取冬化处理(对比例2) 棕绿色 56％ 82％
回流提取冬化处理(对比例3) 棕绿色 54％ 84％
表1显示，本发明方法与冷冻提取或冬化处理相比，其所得产品的色泽更浅，大麻提取物中大麻二酚含量以及回收率更高。

Claims (10)

  1. 一种有机膜在大麻提取中的应用，其特征在于，所述应用包括以下步骤：
    大麻原料经过有机溶剂提取之后依次进行微孔滤膜过滤、非孔有机膜过滤，收集滤液、回收溶剂即得大麻提取物。
  2. 根据权利要求1所述的有机膜在大麻提取中的应用，其特征在于，所述有机溶剂为甲醇、乙醇、丙酮、正己烷、正庚烷、乙酸乙酯中的任意一种。
  3. 根据权利要求1所述的有机膜在大麻提取中的应用，其特征在于，所述微孔滤膜孔径为0.1-50μm。
  4. 根据权利要求1所述的有机膜在大麻提取中的应用，其特征在于，所述非孔有机膜为聚酰亚胺复合膜。
  5. 根据权利要求1所述的有机膜在大麻提取中的应用，其特征在于，所述非孔有机膜为硅涂层聚酰亚胺复合膜。
  6. 根据权利要求1-5任一所述的有机膜在大麻提取中的应用，其特征在于，所述非孔有机膜过滤的膜压差为0.5-2.0Mpa。
  7. 根据权利要求1-5任一所述的有机膜在大麻提取中的应用，其特征在于，在非孔有机膜过滤过程中，待过滤液体温度为20℃-55℃。
  8. 根据权利要求1-5任一所述的有机膜在大麻提取中的应用，其特征在于，在非孔有机膜过滤过程中，当膜透过溶液体积和膜未透过溶液体积比大于5时，加入有机溶剂透洗。
  9. 根据权利要求8任一所述有机膜在大麻提取中的应用，其特征在于，在非孔有机膜过滤过程中，当膜透过溶液体积和膜未透过溶液体积比大于10时，加入有机溶剂透洗。
  10. 根据权利要求8所述的有机膜在大麻提取中的应用，其特征在于，所述有机溶剂加入量为膜未透过溶液1-5倍体积。
PCT/CN2020/097467 2020-05-26 2020-06-22 一种有机膜在大麻提取中的应用 WO2021237841A1 (zh)

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