CN107382672A - Utilize the method and its cannabidiol product of supercritical carbon dioxide extracting cannabidiol - Google Patents
Utilize the method and its cannabidiol product of supercritical carbon dioxide extracting cannabidiol Download PDFInfo
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- CN107382672A CN107382672A CN201710631532.9A CN201710631532A CN107382672A CN 107382672 A CN107382672 A CN 107382672A CN 201710631532 A CN201710631532 A CN 201710631532A CN 107382672 A CN107382672 A CN 107382672A
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- cannabidiol
- carbon dioxide
- supercritical carbon
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- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 title claims abstract description 96
- ZTGXAWYVTLUPDT-UHFFFAOYSA-N cannabidiol Natural products OC1=CC(CCCCC)=CC(O)=C1C1C(C(C)=C)CC=C(C)C1 ZTGXAWYVTLUPDT-UHFFFAOYSA-N 0.000 title claims abstract description 77
- QHMBSVQNZZTUGM-UHFFFAOYSA-N Trans-Cannabidiol Natural products OC1=CC(CCCCC)=CC(O)=C1C1C(C(C)=C)CCC(C)=C1 QHMBSVQNZZTUGM-UHFFFAOYSA-N 0.000 title claims abstract description 76
- QHMBSVQNZZTUGM-ZWKOTPCHSA-N cannabidiol Chemical compound OC1=CC(CCCCC)=CC(O)=C1[C@H]1[C@H](C(C)=C)CCC(C)=C1 QHMBSVQNZZTUGM-ZWKOTPCHSA-N 0.000 title claims abstract description 76
- 229950011318 cannabidiol Drugs 0.000 title claims abstract description 76
- PCXRACLQFPRCBB-ZWKOTPCHSA-N dihydrocannabidiol Natural products OC1=CC(CCCCC)=CC(O)=C1[C@H]1[C@H](C(C)C)CCC(C)=C1 PCXRACLQFPRCBB-ZWKOTPCHSA-N 0.000 title claims abstract description 73
- 229910002092 carbon dioxide Inorganic materials 0.000 title claims abstract description 48
- 239000001569 carbon dioxide Substances 0.000 title claims abstract description 48
- 238000000034 method Methods 0.000 title claims abstract description 23
- 238000000605 extraction Methods 0.000 claims abstract description 42
- 239000000843 powder Substances 0.000 claims abstract description 36
- 244000025254 Cannabis sativa Species 0.000 claims abstract description 22
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 claims abstract description 20
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 claims abstract description 20
- 235000009120 camo Nutrition 0.000 claims abstract description 20
- 235000005607 chanvre indien Nutrition 0.000 claims abstract description 20
- 239000011487 hemp Substances 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 17
- 239000002994 raw material Substances 0.000 claims abstract description 14
- 239000002904 solvent Substances 0.000 claims abstract description 9
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 239000000284 extract Substances 0.000 claims description 13
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 12
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 8
- 239000002253 acid Substances 0.000 claims description 6
- 125000001931 aliphatic group Chemical group 0.000 claims description 6
- 150000003505 terpenes Chemical class 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 239000003208 petroleum Substances 0.000 claims description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims 1
- 238000011084 recovery Methods 0.000 abstract description 6
- 241000218236 Cannabis Species 0.000 abstract 1
- 239000003960 organic solvent Substances 0.000 description 5
- 238000012986 modification Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 240000004308 marijuana Species 0.000 description 2
- 206010006187 Breast cancer Diseases 0.000 description 1
- 208000026310 Breast neoplasm Diseases 0.000 description 1
- UVOLYTDXHDXWJU-UHFFFAOYSA-N Cannabichromene Chemical compound C1=CC(C)(CCC=C(C)C)OC2=CC(CCCCC)=CC(O)=C21 UVOLYTDXHDXWJU-UHFFFAOYSA-N 0.000 description 1
- UVOLYTDXHDXWJU-NRFANRHFSA-N Cannabichromene Natural products C1=C[C@](C)(CCC=C(C)C)OC2=CC(CCCCC)=CC(O)=C21 UVOLYTDXHDXWJU-NRFANRHFSA-N 0.000 description 1
- WVOLTBSCXRRQFR-SJORKVTESA-N Cannabidiolic acid Natural products OC1=C(C(O)=O)C(CCCCC)=CC(O)=C1[C@@H]1[C@@H](C(C)=C)CCC(C)=C1 WVOLTBSCXRRQFR-SJORKVTESA-N 0.000 description 1
- REOZWEGFPHTFEI-JKSUJKDBSA-N Cannabidivarin Chemical compound OC1=CC(CCC)=CC(O)=C1[C@H]1[C@H](C(C)=C)CCC(C)=C1 REOZWEGFPHTFEI-JKSUJKDBSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 241001471082 Colocasia bobone disease-associated cytorhabdovirus Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 206010027476 Metastases Diseases 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 241000218231 Moraceae Species 0.000 description 1
- 206010028813 Nausea Diseases 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 208000013738 Sleep Initiation and Maintenance disease Diseases 0.000 description 1
- CYQFCXCEBYINGO-UHFFFAOYSA-N THC Natural products C1=C(C)CCC2C(C)(C)OC3=CC(CCCCC)=CC(O)=C3C21 CYQFCXCEBYINGO-UHFFFAOYSA-N 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 230000002411 adverse Effects 0.000 description 1
- 230000000202 analgesic effect Effects 0.000 description 1
- 230000003556 anti-epileptic effect Effects 0.000 description 1
- 230000000561 anti-psychotic effect Effects 0.000 description 1
- 239000001961 anticonvulsive agent Substances 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 208000006673 asthma Diseases 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 201000011510 cancer Diseases 0.000 description 1
- WVOLTBSCXRRQFR-DLBZAZTESA-M cannabidiolate Chemical compound OC1=C(C([O-])=O)C(CCCCC)=CC(O)=C1[C@H]1[C@H](C(C)=C)CCC(C)=C1 WVOLTBSCXRRQFR-DLBZAZTESA-M 0.000 description 1
- REOZWEGFPHTFEI-UHFFFAOYSA-N cannabidivarine Natural products OC1=CC(CCC)=CC(O)=C1C1C(C(C)=C)CCC(C)=C1 REOZWEGFPHTFEI-UHFFFAOYSA-N 0.000 description 1
- QXACEHWTBCFNSA-UHFFFAOYSA-N cannabigerol Natural products CCCCCC1=CC(O)=C(CC=C(C)CCC=C(C)C)C(O)=C1 QXACEHWTBCFNSA-UHFFFAOYSA-N 0.000 description 1
- SEEZIOZEUUMJME-FOWTUZBSSA-N cannabigerolic acid Chemical compound CCCCCC1=CC(O)=C(C\C=C(/C)CCC=C(C)C)C(O)=C1C(O)=O SEEZIOZEUUMJME-FOWTUZBSSA-N 0.000 description 1
- SEEZIOZEUUMJME-UHFFFAOYSA-N cannabinerolic acid Natural products CCCCCC1=CC(O)=C(CC=C(C)CCC=C(C)C)C(O)=C1C(O)=O SEEZIOZEUUMJME-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000002512 chemotherapy Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 231100001231 less toxic Toxicity 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000009401 metastasis Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000008693 nausea Effects 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 239000002574 poison Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 238000012805 post-processing Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 206010039073 rheumatoid arthritis Diseases 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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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
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/105—Plant extracts, their artificial duplicates or their derivatives
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L33/00—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof
- A23L33/10—Modifying nutritive qualities of foods; Dietetic products; Preparation or treatment thereof using additives
- A23L33/115—Fatty acids or derivatives thereof; Fats or oils
- A23L33/12—Fatty acids or derivatives thereof
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mycology (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Organic Chemistry (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Botany (AREA)
- Medicines Containing Plant Substances (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
The invention discloses a kind of method using supercritical carbon dioxide extracting cannabidiol, including：Pretreatment：The flower of hemp and leaf are placed under 105 120 degrees Celsius and dried 0.5 4 hours, obtains the raw material A that moisture content is less than 7%；Crush：Raw material A is crushed to 50 100 mesh, obtains powder B；Dry：Powder B is placed under 105 120 degrees Celsius and dried 0.5 1 hours, obtains the powder C that moisture content is less than 5%；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 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
Technical field
The present invention relates to material extract field, and in particular to using supercritical carbon dioxide extracting cannabidiol method and
Its cannabidiol product.
Background technology
Hemp（Cannabis sativaL.）Also known as fire fiber crops or hemp, are Moraceae, Cannabis plant, annual upright grass
This, high 1-3 rice.The cannabidiol contained in hemp（CBD）Composition, it is the phenols not yet isolated in other animals and plants at present
Compound, cannabidiol（CBD）It is non-additive composition, there is 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 the function such as treatment asthma.Scientist also found cannabidiol in recent years（CBD）For powerful antioxidants, have and block some poison
The adverse effect of product human nerve, and with a series of lifes such as blocking Metastasis in Breast Cancer, resisting rheumatoid arthritis, anti-insomnias
Manage active function.THC according to contained by hemp（THC）Ratio, it is generally divided into industrial hemp and drugs are big
Numb two classes.Industrial hemp belongs to less toxic hemp, wherein THC（THC）Content not more than 0.3%（Generally acknowledge by various countries
Define method）, without drugs value；And in the leaf and flower THC of marijuana hemp（THC）Content it is higher, category is high
Malicious 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, and 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
A kind of side it is an object of the invention to provide cannabidiol and using supercritical carbon dioxide extracting cannabidiol
Method, solve prior art and utilize solution restricted-access media cannabidiol, consume a large amount of organic solvents, increase extracts cost and right
The problem of cannabidiol quality is reduced while the pollution of environment.
To solve above-mentioned technical problem, the present invention uses following technical scheme：
A kind of method using supercritical carbon dioxide extracting cannabidiol, including：
Pretreatment：The flower of hemp and leaf are placed under 105-120 degrees Celsius and dry 0.5-4 hours, obtains moisture content less than 7%
Raw material A；
Crush：Raw material A is crushed to 50-100 mesh, obtains powder B；
Dry：Powder B is placed under 105-120 degrees Celsius and dries 0.5-1 hours, obtains the powder C that moisture content is less than 5%；
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 cannabidiol in hemp is extracted using supercritical carbon dioxide, is extracted compared to using organic solvent, it is overcritical
The purity of the cannabidiol that carbon dioxide draw obtains is higher, recovery rate is higher, extraction rate is faster, and in cannabidiol effectively
The content of composition is also much higher；Carbon dioxide re-uses after can collecting after parsing, the part titanium dioxide even lost
Carbon will not also pollute to operating environment, and carbon dioxide will not remain in obtained cannabidiol product.
As preferable, before carrying out supercritical carbon dioxide extracting to powder C, powder C is set to be cooled to 18-25 degrees Celsius simultaneously
Its moisture content is kept to be less than 5%.Cooling environment should keep drying, prevent powder C from being absorbed water again in temperature-fall period.
As preferable, in the extraction step, the temperature of extraction is 20-50 degrees Celsius, pressure 5-30MPa, extraction
Time is 1-5 hours.
As preferable, in the extraction step, the flow of carbon dioxide is 500-850 kgs/hr, carbon dioxide
Flow and powder C dosage are substantially unrelated
As preferable, in the separating step, the temperature of parsing is 20-50 degrees Celsius, pressure 1-15MPa.
As preferable, after the cannabidiol parsed in the separating step is heated to 70 degrees Celsius, kept for 10 minutes
More than, it is put into homogenizer, homogeneous filling afterwards or entrance is handled in next step.
As preferable, 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 cannabidiol in industrial hemp, entrainer can be used, can between entrainer and thing to be extracted
Chemical bond is formed, therefore add entrainer to improve extraction efficiency.Typically 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 preferable, the weight ratio of the entrainer and powder C is 0.3-1.0：100.
Entrainer is very few, does not have the effect for improving extraction efficiency, and entrainer dosage is excessive, may be because of solution in parsing
Analysing insufficient makes entrainer remain in cannabidiol product.
As preferable, 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, by obtained extract and
Separating step is carried out after liquid D mixing.
A kind of cannabidiol, by weight, including cannabidiol 10-30%, unsaturated aliphatic acid 50-60%, terpenoid
Thing 9-11%.
More cannabidiols using 30% to 60% American-European at present are oily to be used as health product raw material, and medicinal raw material is sometimes for close
99% purity.The present invention is directed to health-product market, there is provided the method that cannabidiol is carried at the beginning of one.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., 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 cannabidiol in hemp is extracted using supercritical carbon dioxide, the recovery rate highest of cannabidiol can reach 90%,
Purity is more than 20%.
2）The cannabidiol in hemp is extracted using supercritical carbon dioxide, weight after carbon dioxide can be collected after parsing
It is new to utilize, often extract once, the loss late of carbon dioxide is less than 15%, and the partial CO 2 even lost also will not be to making
Industry environment pollutes, and carbon dioxide will not remain in obtained cannabidiol 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 method using supercritical carbon dioxide extracting cannabidiol, including：
Pretreatment：The flower of hemp and leaf are placed under 105 degrees Celsius and dried 0.5 hour, obtains moisture content up to 7% raw material A；
Crush：Raw material A is crushed to 50 mesh, obtains powder B；
Dry：Powder B is placed under 105 degrees Celsius and dried 0.5 hour, moisture content is obtained and is less than 5% powder C, and make powder C
It is cooled to 18 degrees Celsius and keeps its moisture content to be less than 5%；
Extraction：Supercritical carbon dioxide extracting is carried out to powder C, the temperature of extraction is 20 degrees Celsius, pressure 5MPa, extraction when
Between for 1 hour, the flow of carbon dioxide be 500 kgs/hr, be also added into entrainer ethyl acetate during extraction, entrainer with
Powder C weight ratio is 0.3：100；Obtain liquid D and residue E after extraction, residue E temperature be 20 degrees Celsius, pressure be
Reextraction is carried out under the conditions of 5MPa, extraction time is 1 hour, the flow of carbon dioxide is 500 kgs/hr, is extracted
Liquid；
Separation：Obtained extract and liquid D are mixed and parsed under conditions of temperature is 20 degrees Celsius, pressure is 1MPa
Cannabidiol, and it is recovered to solvent F；After the cannabidiol parsed is heated to 70 degrees Celsius, is kept for more than 10 minutes, be put into even
In matter machine, homogeneous filling afterwards or entrance is handled in next step.
The cannabidiol that the present embodiment obtains, by weight, including cannabidiol 23.4%, unsaturated aliphatic acid 58.3%,
Terpenoid 10.5%.
Embodiment 2：
A kind of method using supercritical carbon dioxide extracting cannabidiol, including：
Pretreatment：The flower of hemp and leaf are placed under 120 degrees Celsius and dried 4 hours, obtains the raw material A that moisture content is less than 7%；
Crush：Raw material A is crushed to 100 mesh, obtains powder B；
Dry：Powder B is placed under 120 degrees Celsius and dried 1 hour, moisture content is obtained and is less than 5% powder C, and drop powder C
Temperature is to 25 degrees Celsius and keeps its moisture content to be less than 5%；
Extraction：Supercritical carbon dioxide extracting is carried out to powder C, the temperature of extraction is 50 degrees Celsius, pressure 30MPa, extraction
Time is 5 hours, the flow of carbon dioxide is 850 kgs/hr, is also added into entrainer industrial naptha, entrainer during extraction
Weight ratio with powder C is 1.0：100；Obtain liquid D and residue E after extraction, residue E temperature be 50 degrees Celsius, pressure be
Reextraction is carried out under the conditions of 30MPa, extraction time is 5.5 hours, the flow of carbon dioxide is 850 kgs/hr, is extracted
Take liquid；
Separation：Obtained extract and liquid D are mixed and parsed under conditions of temperature is 50 degrees Celsius, pressure is 15MPa
Go out cannabidiol, and be recovered to solvent F；After the cannabidiol parsed is heated to 80 degrees Celsius, is kept for more than 10 minutes, be put into
In homogenizer, homogeneous filling afterwards or entrance is handled in next step.
The cannabidiol that the present embodiment obtains, by weight, including cannabidiol 25.3%, unsaturated aliphatic acid 52.6%,
Terpenoid 10.1%.
Embodiment 3：
A kind of method using supercritical carbon dioxide extracting cannabidiol, including：
Pretreatment：The flower of hemp and leaf are placed under 112 degrees Celsius and dried 2 hours, obtains the raw material A of moisture content 6%；
Crush：Raw material A is crushed to 75 mesh, obtains powder B；
Dry：Powder B is placed under 112 degrees Celsius and dried 0.75 hour, moisture content is obtained and is less than 5% powder C, and make powder C
It is cooled to 22 degrees Celsius and keeps its moisture content to be less than 5%；
Extraction：Supercritical carbon dioxide extracting is carried out to powder C, the temperature of extraction is 35 degrees Celsius, pressure 20MPa, extraction
Time is 3 hours, the flow of carbon dioxide is 600 kgs/hr, is also added into entrainer petroleum ether during extraction, entrainer with
Powder C weight ratio is 0.7：100；Obtain liquid D and residue E after extraction, residue E temperature be 35 degrees Celsius, pressure be
Reextraction is carried out under the conditions of 20MPa, extraction time is 3 hours, the flow of carbon dioxide is 650 kgs/hr, is extracted
Liquid；
Separation：Obtained extract and liquid D are mixed and parsed under conditions of temperature is 35 degrees Celsius, pressure is 12MPa
Go out cannabidiol, and be recovered to solvent F；After the cannabidiol parsed is heated to more than 70 degrees Celsius, kept for more than 10 minutes,
It is put into homogenizer, homogeneous filling afterwards or entrance is handled in next step.
The cannabidiol that the present embodiment obtains, by weight, including cannabidiol 32.8%, unsaturated aliphatic acid 50.6%,
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 | 92.3 | 23.4 | 9.8 |
| 2 | 93.8 | 25.3 | 15.1 |
| 3 | 95.6 | 32.8 | 12.0 |
As can be seen from the above table, cannabidiol content or solvent loss rate side either 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 modifications 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 (10)
- A kind of 1. method using supercritical carbon dioxide extracting cannabidiol, it is characterised in that including：Pretreatment：The flower of hemp and leaf are placed under 105-120 degrees Celsius and dry 0.5-4 hours, obtains moisture content less than 7% Raw material A；Crush：Raw material A is crushed to 50-100 mesh, obtains powder B；Dry：Powder B is placed under 105-120 degrees Celsius and dries 0.5-1 hours, obtains the powder C that moisture content is less than 5%；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.
- 2. the method according to claim 1 using supercritical carbon dioxide extracting cannabidiol, it is characterised in that to powder Before last C carries out supercritical carbon dioxide extracting, powder C is cooled to 18-25 degrees Celsius and keep its moisture content to be less than 5%.
- 3. the method according to claim 1 using supercritical carbon dioxide extracting cannabidiol, it is characterised in that described In extraction step, the temperature of extraction is 20-50 degrees Celsius, pressure 5-30MPa, extraction time are 1-5 hours.
- 4. the method according to claim 1 using supercritical carbon dioxide extracting cannabidiol, it is characterised in that described In extraction step, the flow of carbon dioxide is 500-850 kgs/hr.
- 5. the method according to claim 1 using supercritical carbon dioxide extracting cannabidiol, it is characterised in that described In separating step, the temperature of parsing is 20-50 degrees Celsius, pressure 1-15MPa.
- 6. the method according to claim 1 using supercritical carbon dioxide extracting cannabidiol, it is characterised in that described After the cannabidiol parsed in separating step is heated to 70 degrees Celsius, is kept for more than 10 minutes, be put into homogenizer, after homogeneous Filling or entrance is handled in next step.
- 7. the method according to claim 1 using supercritical carbon dioxide extracting cannabidiol, it is characterised in that described Entrainer is additionally added in extraction step, the entrainer includes the one or more in ethyl acetate, industrial naptha and petroleum ether.
- 8. the method according to claim 7 using supercritical carbon dioxide extracting cannabidiol, it is characterised in that described The weight ratio of entrainer and powder C is 0.3-1.0：100.
- 9. the method according to claim 1 using supercritical carbon dioxide extracting cannabidiol, it is characterised in that to residual Slag E carries out reextraction, and the temperature of the reextraction is 20-50 degrees Celsius, pressure 5-30MPa, extraction time 1-5.5 Hour, the flow of carbon dioxide be 500-850 kgs/hr, will obtained extract and liquid D mix after carry out separation step Suddenly.
- 10. hemp two made from a kind of method using supercritical carbon dioxide extracting cannabidiol described in claim 1-9 Phenol, it is characterised in that by weight, including cannabidiol 10-30%, unsaturated aliphatic acid 50-60%, terpenoid 9-11%.
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| CN113754518A (en) * | 2021-09-24 | 2021-12-07 | 云南绿新生物药业有限公司 | Method for efficiently purifying cannabidiol from industrial cannabis sativa leaves |
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