CN110407672A - A kind of fusion-crystallization extracts the application method of dewaxing technique in cannabidiol in medical cannabis - Google Patents
A kind of fusion-crystallization extracts the application method of dewaxing technique in cannabidiol in medical cannabis Download PDFInfo
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- CN110407672A CN110407672A CN201810396133.3A CN201810396133A CN110407672A CN 110407672 A CN110407672 A CN 110407672A CN 201810396133 A CN201810396133 A CN 201810396133A CN 110407672 A CN110407672 A CN 110407672A
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- medicinal extract
- cannabidiol
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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
- C07C37/004—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom of a six-membered aromatic ring by obtaining phenols from plant material or from animal material
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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
- C07C37/685—Processes comprising at least two steps in series
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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
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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
- C07C37/84—Purification; separation; Use of additives, e.g. for stabilisation by physical treatment by crystallisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C2601/00—Systems containing only non-condensed rings
- C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
- C07C2601/16—Systems containing only non-condensed rings with a six-membered ring the ring being unsaturated
Abstract
The invention discloses a kind of application methods of fusion-crystallization dewaxing technique in medical cannabis extraction cannabidiol, it dewaxes including solvent extraction, fusion-crystallization, the present invention realizes effective and simple dewaxing process to cannabidiol using the method for fusion-crystallization, in this process, realize circular flow continuous production, effectively reduce dewaxing cost, and process for dewaxing of the invention is high-efficient, wax content < 0.5% of product after dewaxing ensures that cannabidiol plays good effect in the application of field of medicaments.
Description
Technical field
The invention belongs to medication chemistry separation fields, and in particular to a kind of fusion-crystallization extracts cannabidiol in medical cannabis
The application method of middle dewaxing technique.
Background technique
Hemp is annual herb, is a kind of plant of Cannabaceae Cannabis, and China also produces, and ancient times are referred to as the " Chinese
Fiber crops ".Contain many components in hemp, at present with three tetrahydrocannabinol (THC), cannabidiol (CBD), cannabinol (CBN) groups
It is divided into leading representative, wherein tetrahydrocannabinol (THC) is considered as that psychoactive drug substance has habituation and hallucinogenic action.Hemp is therefore
Drugs, including federal laws are defined as by many state's laws.But there are the hemps of non-psychoactive drug substance again in hemp
Diphenol (CBD) has treatment anxiety, depression and analgesic and other effects, and can hinder influence of the THC component to nerve system of human body.
It therefore whether is drugs about hemp, academia disputes on so far not to stop, and scientific research is still continuing, and hemp is in field of medicaments at present
There is original effectiveness as medicinal therapeutic substance.
Cannabidiol (CBD) is to find do not have essence in substance that scientist extracts acquisition in the chemical constituent of cannabis plants
The active substance of mind, not will lead to physiological dependence, and the World Health Organization also adds that cannabidiol is different from tetrahydrocannabinol,
Without cause it is unreal, addicted, rely on the effects of, cannabidiol is safe, and is had in the mankind and animal body good by resistance to
Property, therefore will not have a negative impact to publilc health.
Cannabidiol is that medical cannabis is obtained by extraction by organic solvent, however currently, obtained cannabidiol purity
Lower (wherein having wax to coexist), results in it during use in this way, can cause to damage to body, influence cannabidiol
Using effect.
Summary of the invention
In view of the defects and deficiencies of the prior art, the present invention intends to provide a kind of fusion-crystallizations to mention in medical cannabis
Take the application method of dewaxing technique in cannabidiol.
To achieve the above object, the invention adopts the following technical scheme:
(1) by the flower of medical cannabis, leaf, stem, fruit solvent extraction, by extract liquor, a large amount of solvents are removed with concentration evaporator
After to obtain cannabidiol medicinal extract stand-by；
(2) fusion-crystallization technology is utilized, dewaxing treatment, detailed process are carried out to medicinal extract molten liquid under certain temperature and pressure
Are as follows:
A, medicinal extract is put into medicinal extract melting tank and medicinal extract, which is heated to 50 DEG C~95 DEG C, makes medicinal extract thawing reach flowing shape (liquid
State), while melting crystallizer is cooled to -20~20 DEG C.Flowing shape medicinal extract liquid is driven into 1# melting crystallizer again with pump
1# medicinal extract flow container is flowed into, liquid level is switched to the operation of 2# melting crystallizer group when reaching setting position.As wax contains in 1# medicinal extract flow container
It measures exceeded, the medicinal extract liquid in 1# medicinal extract flow container is returned in 1# melting crystallizer again with 3# delivery pump, circulate operation, until leaching
Wax content is up to standard in medicinal extract liquid in cream flow container；
B, the wax that solidification is precipitated in elution 1# melting crystallizer is carried out after the completion of step a, is heated molten in cleaning solvent tank
Temperature is set to 50~90 DEG C, solvent is squeezed into 1# melting crystallizer with 2# delivery pump and is washed by agent and 1# melting crystallizer, molten
Agent and the miscible inflow 1# solvent tank of wax are collected, and the liquid level of 1# solvent tank is controlled, and circulation cleans up 1# fused junction for several times
It is spare after brilliant device；
C, the operation of 2# melting crystallizer group is identical as 1# melting crystallizer, and alternate run repeats the above steps, in cyclic process
Just intermittent continuous operation process is realized.
Advantages of the present invention:
Separation to wax in plant extracts, traditional method often use porous powder (carclazyte, diatomite, perlite,
Active carbon etc.) removal is adsorbed and is filtered, the processing method process is complicated, and needs to consume more thermal energy and electric energy.This
Invention is realized using the method for fusion-crystallization and is realized in this process to the simple and efficient dewaxing process of cannabidiol
Circular flow continuous production effectively reduces dewaxing cost, realizes low energy consumption isolation technics, and method dewaxing of the invention
High-efficient, the every circulation primary of dewaxing rate is up to 60% ~ 70%, and rear wax content can control within 2% circulation twice, ensures hemp two
Phenol plays good effect in the application of field of medicaments.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Embodiment one
A kind of fusion-crystallization extracts the application method of dewaxing technique in cannabidiol in medical cannabis, the method comprises the following steps:
(1) cannabis, leaf, stem, fruit are extracted with ethyl acetate solvent, by extract liquor with 20 times of rotary evaporator concentration volume
After to obtain cannabidiol medicinal extract stand-by (wax content 2%)；
(2) fusion-crystallization technology is utilized, dewaxing treatment, detailed process are carried out to medicinal extract at a certain temperature are as follows:
A, medicinal extract is put into medicinal extract melting tank and medicinal extract, which is heated to 75 DEG C, makes medicinal extract thawing reach flowing shape (liquid), together
When melting crystallizer is cooled to 15 DEG C.Flowing shape medicinal extract liquid is driven into 1# melting crystallizer with 1# pump and flows into 1# medicinal extract again
Flow container, liquid level are switched to the operation of 2# melting crystallizer group when reaching setting position.Medicinal extract liquid in 1# medicinal extract flow container return again into
In 1# melting crystallizer, circulate operation 2 times, samples medicinal extract liquid in 1# medicinal extract flow container and detect wax content up to 0.45%；
B, the related valve for closing the circuit step a, carries out the wax that solidification is precipitated in elution 1# melting crystallizer, and heating washing is molten
Cleaning solvent is squeezed into 1# melting crystallizer with pump and washed by agent heating tank to 50 DEG C and 1# melting crystallizer to 70 DEG C, solvent and
The miscible inflow 1# solvent tank of wax is collected, and circulation 2 times are to clean up 1# melting crystallizer；
It is 85% that medicinal extract is concentrated into solid content in rotary evaporator or scrapper thin film evaporator.
After tested, product impurity wax content is 4.7%.
Embodiment two
A kind of fusion-crystallization extracts the application method of dewaxing technique in cannabidiol in medical cannabis, the method comprises the following steps:
(1) by cannabis, leaf, stem, fruit 8 chloroform of methanol, 2 mixed extractant solvent, by extract liquor rotary evaporator condensation product
It is stand-by (wax content 2.2%) that cannabidiol medicinal extract is obtained after 25 times of product；
(2) fusion-crystallization technology is utilized, dewaxing treatment, detailed process are carried out to medicinal extract at a certain temperature are as follows:
A, medicinal extract is put into medicinal extract melting tank and medicinal extract, which is heated to 80 DEG C, makes medicinal extract thawing reach flowing shape (liquid), together
When melting crystallizer is cooled to 5 DEG C.Flowing shape medicinal extract liquid is driven into 1# melting crystallizer with 1# pump and flows into 1# medicinal extract again
Flow container, liquid level are switched to the operation of 2# melting crystallizer group when reaching setting position.Medicinal extract liquid in 1# medicinal extract flow container return again into
In 1# melting crystallizer, circulate operation 3 times, samples medicinal extract liquid in 1# medicinal extract flow container and detect wax content up to 0.2%；
B, the related valve for closing the circuit step a, carries out the wax that solidification is precipitated in elution 1# melting crystallizer, and heating washing is molten
Cleaning solvent is squeezed into 1# melting crystallizer with 2# pump and washed by agent heating tank to temperature 50 C and 1# melting crystallizer to 60 DEG C,
Solvent and the miscible inflow 1# solvent tank of wax are collected, and circulation 2 times are to clean up 1# melting crystallizer；
It is 80% that medicinal extract is concentrated into solid content in rotary evaporator or scrapper thin film evaporator.
After tested, product impurity content is 3.4%.
Claims (5)
1. the application method that a kind of fusion-crystallization extracts dewaxing technique in cannabidiol in medical cannabis, it is characterised in that the side
Method and steps are as follows:
(1) by the flower of medical cannabis, leaf, stem, fruit solvent extraction, cannabidiol medicinal extract is obtained after extract liquor is concentrated and is waited for
With；
The extractant is methanol, ethyl alcohol, chloroform or ethyl acetate, and the inspissator uses rotary evaporator, scraper plate
Thin film evaporator, outer or internal circulation evaporator, liter or falling film evaporator；
(2) fusion-crystallization technology is used, dewaxing treatment, detailed process are carried out to medicinal extract melting liquid under certain temperature control
Are as follows:
A, medicinal extract is put into medicinal extract melting tank and medicinal extract, which is heated to 50 DEG C~95 DEG C, makes medicinal extract thawing reach flowing shape (liquid
State), while 1# melting crystallizer is cooled to -20~20 DEG C；
Flowing shape medicinal extract liquid is driven into 1# melting crystallizer with pump and flows into 1# medicinal extract flow container again, when liquid level reaches setting position
It is switched to the operation of 2# melting crystallizer group；
If wax content in 1# medicinal extract flow container is exceeded, the medicinal extract liquid in 1# medicinal extract flow container is returned again in 1# melting crystallizer, is followed
Ring operation, until wax content is up to standard in medicinal extract liquid in 1# medicinal extract flow container；
B, the wax that solidification is precipitated in elution 1# melting crystallizer is carried out after the completion of step a, heats cleaning solvent tank and 1# is molten
Melt crystallizer, temperature is set to 50~90 DEG C, solvent is squeezed into 1# melting crystallizer with pump and is washed, solvent and the miscible stream of wax
Enter the collection of 1# solvent tank, control the liquid level of 1# solvent tank, cleans up spare after 1# melting crystallizer；
C, the operation of 2# melting crystallizer group is identical as 1# melting crystallizer, and alternate run repeats the above steps, in cyclic process
Just intermittent continuous operation process is realized.
2. a kind of fusion-crystallization extracts the application side of dewaxing technique in cannabidiol in medical cannabis according to claim 1
Method, which is characterized in that it is 85%- that the medicinal extract needs obtained with solvent extraction are concentrated into solid content in evaporation concentrator
95%。
3. the application side that a kind of fusion-crystallization according to claim 1 extracts dewaxing technique in cannabidiol in medical cannabis
Method, which is characterized in that the cooling temperature of the melting crystallizer is controlled at -20~20 DEG C, if cooling temperature is excessively high, wax
Solidification cannot be precipitated, dewaxing effect is unobvious, and the wax in medicinal extract cannot slough very well；If temperature is too low, cause power unrestrained
Take, and cannabidiol also has a little and then precipitation solidification attachment in medicinal extract, and product is caused to lose.
4. a kind of fusion-crystallization extracts the application side of dewaxing technique in cannabidiol in medical cannabis according to claim 1
Method, which is characterized in that the clearance-type continuous operation process is embodied in the switching of each valve group and the blocked operation of pump.
5. a kind of fusion-crystallization extracts the application side of dewaxing technique in cannabidiol in medical cannabis according to claim 1
Method, which is characterized in that described its basic procedure of fusion-crystallization process for dewaxing are as follows:
(1) medicinal extract in medicinal extract melting tank heating melting be liquid can flow freely shape → 1# delivery pump → enter 1# melt
Crystallizer → wax is precipitated the solidification → medicinal extract liquid stream containing cannabidiol and other components and goes out → 1# medicinal extract flow container (liquid level
Valve a is closed when reaching setting position, opens valve b, is switched to the operation of 2# melting crystallizer) → start 3# circulating pump again medicinal extract
Liquid squeezes into 1# melting crystallizer, and circulation stops 3# delivery pump afterwards for several times；
(2) heat in cleaning solvent tank that wax is molten in solvent and 1# melting crystallizer → 2# delivery pump → 1# melting crystallizer
Solution → 1# solvent tank → 4# delivery pump → 1# melting crystallizer, circulation elute wax sufficiently for several times；
(3) operating procedure of 2# melting crystallizer group is similar.
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Cited By (1)
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|---|---|---|---|---|
| GB2621558A (en) * | 2022-08-09 | 2024-02-21 | Univ Stellenbosch | A method of extracting cannabinoids from plant waxes |
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Application publication date: 20191105 |