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CN107325881A - The extracting process and its cannabis leaf oil product of cannabis leaf oil - Google Patents

The extracting process and its cannabis leaf oil product of cannabis leaf oil Download PDF

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Publication number
CN107325881A
CN107325881A CN201710631525.9A CN201710631525A CN107325881A CN 107325881 A CN107325881 A CN 107325881A CN 201710631525 A CN201710631525 A CN 201710631525A CN 107325881 A CN107325881 A CN 107325881A
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CN
China
Prior art keywords
leaf oil
powder
cannabis leaf
extraction
degrees celsius
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710631525.9A
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Chinese (zh)
Inventor
项伟
刘绍兴
顾文云
李泳霖
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Yunnan Han Musen Biotechnology LLC
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Yunnan Han Musen Biotechnology LLC
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Yunnan Han Musen Biotechnology LLC filed Critical Yunnan Han Musen Biotechnology LLC
Priority to CN201710631525.9A priority Critical patent/CN107325881A/en
Publication of CN107325881A publication Critical patent/CN107325881A/en
Pending legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/02Pretreatment
    • C11B1/04Pretreatment of vegetable raw material
    • CCHEMISTRY; METALLURGY
    • C11ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
    • C11BPRODUCING, 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
    • C11B1/00Production of fats or fatty oils from raw materials
    • C11B1/10Production of fats or fatty oils from raw materials by extracting
    • C11B1/104Production of fats or fatty oils from raw materials by extracting using super critical gases or vapours

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Acyclic And Carbocyclic Compounds In Medicinal Compositions (AREA)
  • Medicines Containing Plant Substances (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a kind of extracting process of cannabis leaf oil, including:Pretreatment:The flower and leaf of hemp are placed under 105 120 degrees Celsius and dried 0.5 4 hours, the raw material A that moisture content is less than 7% is obtained;Crush:Raw material A is crushed to 50 100 mesh, powder B is obtained;Dry:Powder B is placed under 105 120 degrees Celsius and dried 0.5 1 hours, the powder C that moisture content is less than 5% is obtained;Extraction:Supercritical carbon dioxide extracting is carried out to powder C, liquid D and residue E are obtained after extraction;Separation:Liquid D parses cannabidiol through throttling expansion, and is recovered to solvent F.The cannabis leaf oil in hemp is extracted with supercritical carbon dioxide, the recovery rate highest of cannabidiol can reach 90%, and purity is more than 20%.

Description

The extracting process and its cannabis leaf oil product of cannabis leaf oil
Technical field
Field is extracted the present invention relates to material, and in particular to extracting process and its cannabis the leaf oil production of cannabis leaf oil Product.
Background technology
Hemp(Cannabis sativaL.)Also known as fire fiber crops or hemp, are Moraceae, Cannabis plant, annual upright grass This, it is high 1-3 meters.The cannabidiol contained in hemp(CBD)Composition, is the phenols not yet isolated in other animals and plants at present Compound, cannabidiol(CBD)It is non-additive composition, with very high medical value.Research shows, if cannabidiol is closed The application of reason ground medically, then has anti-epileptic, an antipsychotic, anti-melancholy, analgesic, mitigate cancer because of caused by chemotherapy nausea with And treat the functions such as asthma.Scientist also found cannabidiol in recent years(CBD)It is some many with blocking for powerful antioxidants Phenol is to the adverse effect of human nerve, and with blocking Metastasis in Breast Cancer, resisting rheumatoid arthritis, anti-insomnia etc. a series of Physiological active functionses.THC according to contained by hemp(THC)Ratio, it is generally divided into industrial hemp and drugs The class of hemp two.Industrial hemp belongs to low toxicity hemp, wherein THC(THC)Content not more than 0.3%(Generally acknowledge by various countries Define method), without drugs value;And in the leaf of marijuana hemp and spray THC(THC)Content It is higher, belong to high poison hemp.
Due to the medical value of cannabidiol, built up many extraction factories in the whole world, and prior art extracts big cannabidiol It is to be extracted using organic solvent extraction mostly, this aspect consumes a large amount of organic solvents, increase extracts cost and to ring The pollution in border, the organic solvent on the other hand remained in cannabidiol extract can also reduce the product of cannabidiol extract Matter, so reducing the extracting method pole of production cost while the purity and extraction efficiency of a kind of big cannabidiol extract of raising To be important.
The content of the invention
It is an object of the invention to provide a kind of extracting process of cannabis leaf oil and its cannabis rich in cannabidiol Leaf oil product, solves prior art and utilizes solution restricted-access media cannabis leaf oil, consumes a large amount of organic solvents, increase extraction The problem of wherein cannabidiol quality being reduced while cost and the pollution to environment.
To solve above-mentioned technical problem, the present invention uses following technical scheme:
A kind of extracting process of cannabis leaf oil, including:
Pretreatment:The flower and leaf of hemp are placed under 125-135 degrees Celsius and dried 0.1-0.4 hours, moisture content is obtained and is less than 6% raw material A;
Crush:Raw material A is crushed to 30-45 mesh, powder B is obtained;
Dry:Powder B is placed under 125-135 degrees Celsius and dried 0.2-0.4 hours, the powder C that moisture content is less than 4% is obtained;
Extraction:Supercritical carbon dioxide extracting is carried out to powder C, liquid D and residue E are obtained after extraction;
Separation:Liquid D parses cannabidiol through throttling expansion, and is recovered to solvent F.
The cannabis leaf oil in hemp is extracted using supercritical carbon dioxide, is extracted compared to using organic solvent, it is super to face The purity of cannabidiol is higher in the cannabis leaf oil that boundary's carbon dioxide draw is obtained, recovery rate is higher, extraction rate is faster, and The content of active ingredient is also much higher in cannabis leaf oil;Re-used after carbon dioxide can be collected after parsing, even The partial CO 2 of loss will not also be polluted to operating environment, and carbon dioxide will not be in obtained cannabis leaf oil production Remained in product.
As preferred, powder C is carried out before supercritical carbon dioxide extracting, powder C is cooled to 18-25 degrees Celsius simultaneously Its moisture content is kept to be less than 5%.
As preferred, in the extraction step, the temperature of extraction is 30-40 degrees Celsius, pressure is 10-20MPa, extraction Time is 2-5 hours.
As preferred, in the extraction step, the flow of carbon dioxide is 300-600 kgs/hr.
As preferred, in the separating step, the temperature of parsing is 30-40 degrees Celsius, pressure is 2-10MPa.
As preferred, the cannabis leaf oil parsed in the separating step is heated to after 60 degrees Celsius, is kept for 10 points More than clock, it is put into homogenizer, the homogeneous rear next step that enters is handled.
As preferred, entrainer is additionally added in the extraction step, the entrainer includes ethyl acetate, industrial naptha With the one or more in petroleum ether.
Extracted for the cannabis leaf oil in industrial hemp, entrainer, energy between entrainer and thing to be extracted can be used Extraction efficiency can be improved by enough forming chemical bond, therefore adding entrainer.It is general to use ethyl acetate, industrial naptha and petroleum ether Deng, entrainer is remarkably improved extraction yield, but can correspondingly cause post-processing difficulty and production cost increase.
As preferred, the entrainer and powder C weight ratio are 0.3-1.0:100.
Entrainer is very few, does not have the effect for improving extraction efficiency, and entrainer consumption is excessive, may be because of solution in parsing Analysis is insufficient to make entrainer remain in cannabis leaf oil product.
As preferred, reextraction is carried out to residue E, the temperature of the reextraction is 20-50 degrees Celsius, pressure is 5-30MPa, extraction time are 1-5.5 hours, the flow of carbon dioxide is 500-850 kgs/hr.
A kind of cannabis leaf oil, by weight, including cannabidiol 10-20%, unsaturated aliphatic acid 61-68%, terpene Compound 8-10%.
Much more American-European at present use 30% to 60% cannabis leaf oil for health product raw material, medicinal raw material is sometimes for approaching 99% purity.There is provided the method that cannabidiol is carried at the beginning of one for health-product market by the present invention.The product prepared through this law contains Cannabidiol composition is 10% to 30%, and remaining main component is unsaturated aliphatic acid, accounts for 50% to 60%.It is simultaneously also other Nearly 100 of terpenoid, such as CBDA, CBGA, CBDV, CBC, CBN, CBG, THC etc., it is combined and accounts for 9-11% altogether.Its It is polysaccharide, including the impurity such as albumen and pectin.
Compared with prior art, beneficial effects of the present invention are at least one of following:
1)The cannabis leaf oil in hemp is extracted using supercritical carbon dioxide, the recovery rate highest of wherein cannabidiol can reach To 90%, purity is more than 20%.
2)The cannabis leaf oil in hemp is extracted using supercritical carbon dioxide, after carbon dioxide can be collected after parsing Re-use, often extract once, the loss late of carbon dioxide is less than 15%, and the partial CO 2 even lost also will not be right Operating environment is polluted, and carbon dioxide will not be remained in obtained cannabis leaf oil product.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to embodiments, to the present invention It is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, it is not used to Limit the present invention.
Embodiment 1:
A kind of extracting process of cannabis leaf oil, including:
Pretreatment:The flower and leaf of hemp are placed under 125 degrees Celsius and dried 0.1 hour, moisture content is obtained up to 6% raw material A;
Crush:Raw material A is crushed to 30-35 mesh, powder B is obtained;
Dry:Powder B is placed under 125 degrees Celsius and dried 0.2 hour, moisture content is obtained and is less than 4% powder C, and make powder C It is cooled to 18 degrees Celsius and keeps its moisture content to be less than 5%;
Extraction:Carry out supercritical carbon dioxide extracting to powder C, the temperature of extraction is 30 degrees Celsius, pressure is 10MPa, extraction Time is 2 hours, the flow of carbon dioxide is 300 kgs/hr, and liquid D and residue E are obtained after extraction;
Separation:Liquid D temperature be 30 degrees Celsius, pressure is to parse cannabis leaf oil under conditions of 2MPa, and is recovered to molten Agent F;The cannabis leaf oil parsed is heated to after 60 degrees Celsius, is kept for 10 minutes, is put into homogenizer, homogeneous rear filling or enter Enter next step processing.
The cannabis leaf oil that the present embodiment is obtained, by weight, including cannabidiol 13.9%, unsaturated aliphatic acid 68.3%th, terpenoid 8.4%.
Embodiment 2:
A kind of extracting process of cannabis leaf oil, including:
Pretreatment:The flower and leaf of hemp are placed under 135 degrees Celsius and dried 0.4 hour, the raw material A of moisture content 4.8% is obtained;
Crush:Raw material A is crushed to 40-45 mesh, powder B is obtained;
Dry:Powder B is placed under 135 degrees Celsius and dried 0.4 hour, the powder C of moisture content 3.6% is obtained, and drops powder C Temperature is to 25 degrees Celsius and keeps its moisture content 4%;
Extraction:Carry out supercritical carbon dioxide extracting to powder C, the temperature of extraction is 40 degrees Celsius, pressure is 20MPa, extraction Time is 5 hours, the flow of carbon dioxide is 600 kgs/hr, and liquid D and residue E are obtained after extraction;
Separation:Liquid D temperature be 40 degrees Celsius, pressure is to parse cannabis leaf oil under conditions of 10MPa, and is recovered to molten Agent F;The cannabis leaf oil parsed is heated to after 60 degrees Celsius, is kept for more than 10 minutes, is put into homogenizer, homogeneous rear filling Or enter next step processing.
The cannabis leaf oil that the present embodiment is obtained, by weight, including cannabidiol 15.9%, unsaturated aliphatic acid 61.1%th, terpenoid 9.1%.
Embodiment 3:
A kind of extracting process of cannabis leaf oil, including:
Pretreatment:The flower and leaf of hemp are placed under 132 degrees Celsius and dried 0.25 hour, the raw material A of moisture content 5.7% is obtained;
Crush:Raw material A is crushed to 35-40 mesh, powder B is obtained;
Dry:Powder B is placed under 132 degrees Celsius and dried 0.3 hour, moisture content is obtained and is less than 4% powder C, and make powder C It is cooled to 22 degrees Celsius and keeps its moisture content to be less than 5%;
Extraction:Carry out supercritical carbon dioxide extracting to powder C, the temperature of extraction is 37 degrees Celsius, pressure is 15MPa, extraction Time is 3.5 hours, the flow of carbon dioxide is 450 kgs/hr, and liquid D and residue E are obtained after extraction;
Separation:Liquid D is that 36 degrees Celsius, pressure are to parse cannabis leaf oil under conditions of 7MPa in temperature, and is recovered to molten Agent F;The cannabis leaf oil parsed is heated to after 80 degrees Celsius, is kept for more than 10 minutes, is put into homogenizer, homogeneous rear filling Or enter next step processing.
The cannabis leaf oil that the present embodiment is obtained, by weight, including cannabidiol 19.7%, unsaturated aliphatic acid 65.8%th, terpenoid 9.2%.
Following table show cannabidiol content and solvent in the cannabidiol recovery rate of embodiment 1-3 methods describeds, product The measurement result of loss late:
Embodiment Cannabidiol recovery rate % Cannabidiol content wt% in product Solvent loss rate %
1 90.6 13.9 10.7
2 92.4 15.9 12.2
3 93.2 19.7 9.0
As can be seen from the above table, either cannabidiol content or solvent loss rate side in cannabidiol recovery rate, product Face considers, is all that embodiment 3 is more excellent.
Although reference be made herein to invention has been described for multiple explanatory embodiments of the invention, however, it is to be understood that Those skilled in the art can be designed that a lot of other modification and embodiment, and these modifications and embodiment will fall in this Shen Please be within disclosed spirit and spirit.More specifically, can be to master in the range of disclosure and claim The building block and/or layout for inscribing composite configuration carry out a variety of variations and modifications.Except what is carried out to building block and/or layout Outside modification and improvement, to those skilled in the art, other purposes also will be apparent.

Claims (7)

1. a kind of extracting process of cannabis leaf oil, it is characterised in that including:
Pretreatment:The flower and leaf of hemp are placed under 125-135 degrees Celsius and dried 0.1-0.4 hours, moisture content is obtained and is less than 6% raw material A;
Crush:Raw material A is crushed to 30-45 mesh, powder B is obtained;
Dry:Powder B is placed under 125-135 degrees Celsius and dried 0.2-0.4 hours, the powder C that moisture content is less than 4% is obtained;
Extraction:Supercritical carbon dioxide extracting is carried out to powder C, liquid D and residue E are obtained after extraction;
Separation:Liquid D parses cannabis leaf oil through throttling expansion, and is recovered to solvent F.
2. the extracting process of cannabis leaf oil according to claim 1, it is characterised in that overcritical two are carried out to powder C Before carbonoxide extraction, powder C is cooled to 18-25 degrees Celsius and keep its moisture content to be less than 5%.
3. the extracting process of cannabis leaf oil according to claim 1, it is characterised in that in the extraction step, extraction Temperature be 30-40 degrees Celsius, pressure be that 10-20MPa, extraction time are 2-5 hours.
4. the extracting process of cannabis leaf oil according to claim 1, it is characterised in that in the extraction step, dioxy The flow for changing carbon is 300-600 kgs/hr.
5. the extracting process of cannabis leaf oil according to claim 1, it is characterised in that in the separating step, parsing Temperature be 30-40 degrees Celsius, pressure be 2-10MPa.
6. the extracting process of cannabis leaf oil according to claim 1, it is characterised in that parsed in the separating step Cannabis leaf oil be heated to after 60 degrees Celsius, keep more than 10 minutes, be put into homogenizer, it is homogeneous after enter next step at Reason.
7. cannabis leaf oil made from a kind of extracting process of the cannabis leaf oil described in claim 1-6, it is characterised in that press Weight meter, including cannabidiol 10-20%, unsaturated aliphatic acid 61-68%, terpenoid 8-10%.
CN201710631525.9A 2017-07-28 2017-07-28 The extracting process and its cannabis leaf oil product of cannabis leaf oil Pending CN107325881A (en)

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Cited By (11)

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Publication number Priority date Publication date Assignee Title
CN108949363A (en) * 2018-09-26 2018-12-07 常德华馥生物技术有限公司 A kind of Solventless Extraction Process of industrial hemp floral leaf essential oil
CN110101804A (en) * 2019-05-30 2019-08-09 厦门梓素生物科技有限公司 A kind of epilepsy drugs combination of the extract containing cannabidiol and preparation method thereof
CN110684589A (en) * 2019-09-27 2020-01-14 黑龙江龙麻工业大麻二酚提取有限公司 Extraction and purification method of hemp oil
CN110724589A (en) * 2019-08-27 2020-01-24 桂林莱茵生物科技股份有限公司 Method for preparing cannabidiol and coproducing cannabis full spectrum oil
CN110872210A (en) * 2019-12-23 2020-03-10 大姚麻王科华生物科技有限公司 Preparation equipment of cannabidiol
CN111000897A (en) * 2019-11-28 2020-04-14 云南汉木森生物科技有限责任公司 aerosol
WO2020211562A1 (en) * 2019-04-15 2020-10-22 云南汉盟制药有限公司 Method for extracting volatile oil from cannabis and application of volatile oil
US11040932B2 (en) 2018-10-10 2021-06-22 Treehouse Biotech, Inc. Synthesis of cannabigerol
US11084770B2 (en) 2016-12-07 2021-08-10 Treehouse Biotech, Inc. Cannabis extracts
CN113801727A (en) * 2020-06-16 2021-12-17 晨光生物科技集团股份有限公司 Industrial method for preparing high-quality industrial hemp oil
US11202771B2 (en) 2018-01-31 2021-12-21 Treehouse Biotech, Inc. Hemp powder

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WO2020211562A1 (en) * 2019-04-15 2020-10-22 云南汉盟制药有限公司 Method for extracting volatile oil from cannabis and application of volatile oil
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CN110101804A (en) * 2019-05-30 2019-08-09 厦门梓素生物科技有限公司 A kind of epilepsy drugs combination of the extract containing cannabidiol and preparation method thereof
CN110724589A (en) * 2019-08-27 2020-01-24 桂林莱茵生物科技股份有限公司 Method for preparing cannabidiol and coproducing cannabis full spectrum oil
CN110724589B (en) * 2019-08-27 2023-01-10 桂林莱茵生物科技股份有限公司 Method for preparing cannabidiol and coproducing cannabis full spectrum oil
CN110684589A (en) * 2019-09-27 2020-01-14 黑龙江龙麻工业大麻二酚提取有限公司 Extraction and purification method of hemp oil
CN111000897A (en) * 2019-11-28 2020-04-14 云南汉木森生物科技有限责任公司 aerosol
CN110872210A (en) * 2019-12-23 2020-03-10 大姚麻王科华生物科技有限公司 Preparation equipment of cannabidiol
CN113801727A (en) * 2020-06-16 2021-12-17 晨光生物科技集团股份有限公司 Industrial method for preparing high-quality industrial hemp oil

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Application publication date: 20171107