US010406453B2

(12) United States Patent (10) Patent No.: US 10 ,406 ,453 B2

Ko et al. (45) Date of Patent: Sep. 10, 2019
(54 ) CANNABINOID EXTRACTION PROCESS (2013.01); C07C 39/ 19 ( 2013 .01); C07D
USING BRINE 311/80 (2013.01); C07C 2601/ 16 (2017.05 )
(71) Applicant: NextLeaf Solutions Ltd ., Coquitlam (58 ) Field of Classification Search
(CA ) CPC ... BO1D 11 /0288 ; B01D 3/ 085 ; B01D 15 /00 ;
B01D 3 /40 ; B01D 11/0292 ; C07C 37 /50 ;
(72 ) Inventors: Ryan Delmoral Ko, Coquitlam (CA ); C07C 37 /74 ; C07C 37 /86 ; C07C 37 /004 ;
Brock Hughes , Port Coquitlam (CA ); C07C 39 /19 ; C07C 2601/ 16 ; CO7D
Krupal Pal, Burnaby (CA ); 311 /80
Alexzander Samuelsson , Vancouver See application file for complete search history .
(CA )
( 73 ) Assignee : Nextleaf Solutions Ltd ., Vancouver (56 ) References Cited
(CA ) U .S . PATENT DOCUMENTS
( * ) Notice: Subject to any disclaimer, the term of this 2014 /0271940 A1 * 9 /2014 Wurzer ................ A61K 36 / 185
patent is extended or adjusted under 35 424 /725
U . S .C . 154 (b ) by 0 days .
FOREIGN PATENT DOCUMENTS
(21) Appl. No.: 16 / 112 ,033
Wo 2013165251 11/ 2013
(22) Filed : Aug. 24, 2018
OTHER PUBLICATIONS
(65) Prior Publication Data
US 2019 /0099696 A1 Apr. 4 , 2019 Canadian Intellectual Property Office Examination Report dated
Nov . 20 , 2018 issued for the co -pending Canadian application
Related U .S . Application Data assigned Application No. 3,016 ,078 with an International Filing
(63 ) Continuation -in -part of application No. 15/ 993 ,457 , Date of Aug. 31, 2018 .
filed on May 30 , 2018 , which is a continuation of * cited by examiner
application No. 15 /721 ,344 , filed on Sep . 29 , 2017,
now Pat. No . 9 ,987 , 567 .
(60 ) Provisional application No.62/676 ,261, filed on May Primary Examiner — John M Mauro
24 , 2018, provisional application No. 62/675 ,620 , (74 ) Attorney, Agent, or Firm — Damien G . Loveland
filed on May 23, 2018 .
(51) Int. Cl. (57) ABSTRACT
B01D 11 /02 ( 2006 .01)
BOID 3 /08 (2006 .01) Raw cannabis plant material is mixed with ethanol and
B01D 3 /40 ( 2006 .01) spun -dry to extract cannabinoids. The ethanol may be
C07C 37 /50 ( 2006 .01) chilled before adding it to the raw cannabis plant material,
CO7C 37 /74 (2006 .01) and a non -polar solvent stage may be used to increase the
C07C 37 /00 ( 2006 .01 ) yield of the extraction . The resulting crude oil and ethanol
C07C 37 /86 (2006 .01) with the dissolved cannabinoids is separated from the raw
C07C 39 / 19 ( 2006 .01 ) cannabis plant material and filtered to remove particulates ,
B01D 15 /00 (2006 .01) waxes, lipids, fats and dissolved impurities . The ethanol is
CO7D 311/80 (2006 .01 ) then evaporated from the resulting mixture of oil and
(52) U .S . CI. ethanol, and the remaining oil then undergoes brine-wash
CPC .... . .. B01D 11/ 0288 ( 2013 .01); B01D 3 / 085 ing, decarboxylation and distillation to obtain the cannabi
( 2013 .01) ; BOID 3 /40 (2013 .01 ) ; BOID noids and other desirable volatile phytochemicals.
11 /0292 (2013 .01) ; B01D 15 / 00 ( 2013.01) ;
C07C 37 /004 ( 2013 .01); C07C 37 /50
(2013.01); C07C 37 /74 (2013.01 ); C07C 37/86 28 Claims, 7 Drawing Sheets
atent Sep. 10 , 2019 Sheet 1 of 7 US 10 ,406 ,453 B2

L 10
ADD ETHANOL TO PLANTMATERIAL UNDER
PRESSURE

12
DRAIN ETHANOL FROM PLANT MATERIAL
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STRIKE 16
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EVAPORATE ETHANOL WWWWWWWWWWWWWWWWWWWWWWW

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DECARBOXYLATE WWWWWWW W WWWWWWWWWWW

FILM WIPET
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FILM WIPE
WWWWWWWW W WWWWWWWWWWW

FIG . 1
 atent Sep. 10 , 2019 Sheet 2 of 7 US 10 ,406 ,453 B2

100 Wwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwwww

301AOdd MVH INVID

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CHILL ETHANOL TV KREKRYERERE

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ADD ETHANOL TO PLANT
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PRESSURIZE ETHANOL AND XXXXXXXXX YOXLR

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128 . FILM WIPE TO OBTAIN

FILTER OFF CHARCOAL EXTRACT

FIG . 2
U.S.Patent sousu sua usmemesana
atent Sep. 10 , 2019

202
Sheet 3 of 7 US 10 ,406 ,453 B2

210 La 220
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atent Sep. 10 , 2019 Sheet 4 of 7 US 10 ,406 ,453 B2

402
WASH - DRY CRUDE OIL AND ETHANOL
w

MIXTURE WWWWWWWWWWWWWWWWW W

MEDIA TREATMENT
WWWW 406
EVAPORATE ETHANOL
408

EVAPORATE NON - POLAR SOLVENT

WWWWWWWWWWWWWWWWWWWWWWWWWWWW

DECARBOXYLATE
* * * * 414
DISTILL

FIG . 4
U . S . Patent Sep . 10, 2019 Sheet 5 of 7 US 10 ,406 ,453 B2

PROVIDE RAW PLANT

MATERIAL MM HEAT CRUDE OIL
HEAT CRUDE OIL

422 TREATWITH MgO

w
DRY PLANT MATERIAL
w YYYYYYYYYYYYYYYYYYYYYYYYYYYYYY
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COOL CRUDE OIL 99402190

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 atent Sep. 10 , 2019 Sheet 6 of 7 US 10 ,406 ,453 B2

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 atent Sep. 10 , 2019 Sheet 7 of 7 US 10 ,406 ,453 B2
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FIG . 6B
 US 10 ,406 ,453 B2
CANNABINOID EXTRACTION PROCESS Disclosed herein is a process for extracting cannabinoids
USING BRINE from raw cannabis plant material comprising the steps of :
adding ethanol to dried and ground cannabis plant material
CROSS -REFERENCE TO RELATED to form an initial mixture ; spinning the initial mixture to
APPLICATIONS 5 separate a crude oil and ethanol mixture from the initial
mixture ; treating the crude oil and ethanol mixture with
This application is a continuation - in - part of and claims media to remove unwanted components therefrom ; evapo
the benefit of U . S . patent application Ser. No . 15 / 993 ,457 , rating ethanol from the treated crude oil and ethanolmixture
filed May 30 , 2018 , which is a continuation of U .S . patent to leave oil; washing the oil with brine ; decarboxylating the
application Ser. No . 15 / 721 , 344 , filed Sep . 29 , 2017 , now 10 brine -washed oil to form decarboxylated oil; and distilling
U .S . Pat. No. 9 , 987,567, both incorporated herein in their the decarboxylated oil to obtain cannabinoids.
entirety. It also claims benefit of U . S . provisional patent
application No . 62/675 ,620 , filed May 23 , 2018 and U . S .
provisional patent application No. 62 /676 , 261, filed May 24, BRIEF DESCRIPTION OF DRAWINGS
2018 , both incorporated herein in their entirety . 15
The following drawings illustrate embodiments of the
TECHNICAL FIELD invention , which should not be construed as restricting the
scope of the invention in any way.
This application relates to the extraction of cannabinoids
from raw cannabis plant material. More specifically, it 20 a FIG . 1 is a high - level flowchart showing the key steps of
process for extracting cannabinoids according to an
relates to the extraction of cannabinoids by means of an
ethanol- based method that includes washing the extracted embodiment FIG . 2 is a
of the present invention .
flowchart showing more detailed steps of a
oil with brine. process for extracting cannabinoids according to an embodi
BACKGROUND 25 ment of the present invention .
FIG . 3 is a schematic diagram of the apparatus used for
In legal, adult - use markets , sales of extracts are growing the extraction of cannabinoids according to an embodiment
ten times faster compared to the sales of dried cannabis , and of the present invention.
extracts account for over 60 % of revenue. With legalization , FIG . 4 is a high -level flowchart showing the key steps of
consumer preferences are shifting from dried cannabis to 30 a process for extracting cannabinoids according to a further
extracted cannabis products . embodiment of the present invention .
However, the scent and flavors of cannabis can be unde FIG . 5 is a flowchart showing more detailed steps of a
sirable in many infused products because of excess lipids ,
plant matter and impurities present in currently available process for extracting cannabinoids according to a further
extracts . 35 embodiment of the present invention .
U .S . Pat. No. 9 ,155,767 to Hospodor et al. relates to the FIGS. 6A - B show a schematic diagram of the apparatus
extraction ofmedicinal cannabis compounds into an eluate , used for the extraction of cannabinoids according to a
by separating a portion of medicinal cannabis compounds further embodiment of the present invention .
contained within a portion of eluate at a first extraction target
level , to provide enough clean solvent to continue extraction 40 DESCRIPTION
operations . A high efficiency concentrator processes eluate
from one or more tanks, creating clean solvent when extrac
tion targets are met or when clean solvent is exhausted . This A . Glossary
manages eluate concentration levels and limits the quantity
of concentrated medicinal cannabis compounds on site at 45 Conchi
Cannabidiol (CBD ) is one of the active cannabinoids
any moment in time. found in cannabis and is used formedicinal purposes.
U .S . Pat. No. 7 , 700 ,368 to Flockhart et al. relates to the
purification of cannabinoid oil from plant material. The high Cannabimemetics are phytochemicals that act on the
degree of purity for the final cannabinoid oil extract is cannabinoid receptors within the body but are not derived
obtained using a combination of chromatography techniques 50 from the cannabis plant nor are they strictly classified as
and different types of solvent for preparing the cannabinoid cannabinoids.
oil extract and removing any insoluble impurity therefrom . Cannabinoids are a group of chemicals that act on can
This background information is provided to reveal infor - nabinoid receptors in thebody, numerous ofwhich are found
mation believed by the applicant to be of possible relevance in the cannabis plant.
to the present invention . No admission is necessarily 55 Crude oil is a term for the description of condensed ,
intended , nor should be construed, that any of the preceding non - filtered oil, i.e . oil that is non -winterized and not treated
information constitutes prior art against the present inven via charcoal , clay and silica . The crude oil contains the
tion . cannabinoids.
SUMMARY OF INVENTION 60 noidTetrahydrocannabinol ( THC ) is a psychotropic cannabi
and is the main psychoactive ingredient of cannabis .
The present invention is directed to the extraction of form THC also hasmedicinal uses. THCa is the non -psychoactive
cannabinoids from plant material. In particular it relates to of THC .
mixing dried and ground cannabis plants with ethanol in a WSD (wash and spin -dry ) separator — a solvent based
wash and spin -dry (WSD ) apparatus, followed by filtration , 65 extraction system /centrifuge drum used to extract botanical
evaporation of ethanol, brine-washing, decarboxylation and compounds from diverse plant species . The device provides
distillation . a process in which the plant material is first washed or
 US 10 ,406 ,453 B2
agitated in solvent, and then spun -dry to separate the extract - the ethanol than if the moisture level were higher. If the
laden solvent from the waste biomass. Agitation includes ethanol that is reclaimed is diluted with water, it will be less
rotating the drum back and forth , for example . effective for repeat processes. Nevertheless, in other
Rotovapa rotary evaporator. embodiments , the moisture content can be as high as 15 %
Winterization refers to the cooling of oil to precipitate and 5 while still allowing for an acceptable process . In other
remove unwanted plant fats , waxes, and lipids through embodiments , other drying techniques may be used .
cooling and filtering . In step 110 , the dried plantmaterial is ground , for example
to an average size between 250 - 300 um . However, it is
B . Overview possible in other embodiments to grind the dried plant
10 material to a size of thousands of microns, and the process
Referring to FIG . 1, a flowchart of the basic steps of the has been found to work with average particle sizes of up to
process is shown . In step 10 , a solvent such as ethanol is 3000 -5000 um . If the plant material is ground to less than
added to dried and ground cannabis plant material under 250 um , say , then problems occur with unwanted packing of
pressure . The ethanolmay be at room temperature or chilled the material in the material columns ( 240 , FIG . 3 ). Notably ,
As a result , the cannabinoids found in the plant material 15 the unwanted packing is due to the raw material packing into
dissolve into the ethanol. In step 12, the ethanol solution is a plug under applied pressure . If the particulate is too fine,
drained from the plant material to form a crude oil and the raw material will form a seemingly solid mass making it
ethanol mixture . The first two steps are considered to be the difficult for ethanol to pass through it.
primary extraction phase . Note that, in other embodiments , the grinding step may
In step 14 , impurities are then removed by media treat - 20 take place before the drying step .
ment of the crude oil and ethanol mixture , which contains In step 112 , the ethanol is chilled to a temperature
the cannabinoids . In step 16 , ethanol is removed or between - 35° C . and - 50° C ., in a tank surrounded by a
reclaimed from the mixture , by evaporation , for example . pressurized liquid CO2 jacket, for example . In other embodi
Steps 14 and 16 are considered to be the solvent reclamation ments , the ethanol is chilled using a heat exchanger or a
stage . 25 jacket of solid CO2 or liquid nitrogen .
In step 18 , the oil remaining after the evaporation is in step 115 , the chilled ethanol is added to the material
decarboxylated to activate the THC . Decarboxylation con - column into which the ground and dried plant material has
verts THCa into THC ; the process activates the THC by been placed . Typically, approximately 50 liters of ethanol is
separating the acid component of THCa , the acidic form of used for every 5 kg of plant material, although it is possible
the cannabinoid , converting it into THC , the neutral form , by 30 that other ratios can be used .
heating to remove the carboxylic acid group and liberate In some embodiments where the ethanol is chilled , the
carbon dioxide . The residue after decarboxylation is then , in optimum temperature has been found to be - 45° C . How
step 20 , distilled using a film wipe apparatus in order to ever , the optimum temperature may be different in other
extract the cannabinoids . embodiments . The optimum choice is a compromise
35 between keeping the timeneeded for chilling to a minimum ,
C . Exemplary Process keeping the consumption of the liquid nitrogen and /or liquid
CO2 coolant down, and maximizing the miscibility of the
Referring to FIG . 2 , a detailed process for the extraction ethanol with the cannabinoids that are to be extracted .
of cannabinoids is shown . This exemplary process relates to Nevertheless, using the treatment and filtration process
the extraction of cannabinoids from cannabis plant material. 40 described herein , the fats and lipids can be removed eco
Steps 100 - 123 relate to the primary extraction phase . nomically from the extracted crude oil and ethanol mixture .
Steps 124 - 138 relate to the adsorbent media treatment stage . The use of chilled ethanol is more efficient for the process
The rotovap stage 160 forms the solvent reclamation phase . in general with respect to post- filtration steps, however, it
Step 165 relates to the decarboxylation stage, and steps has slightly less efficiency with respect to yield . Non -chilled
170 - 180 relate to the distillation of the cannabinoids. 45 ethanol is more efficient in terms of extraction yield but very
In step 100 , raw cannabis plant material is provided . The inefficient for post- filtration steps. Non -chilled ethanol
raw cannabis plant material includes, for example, the extracts unwanted fats, waxes and lipids. In some embodi
flower, the leaves and the stems close to the leaves . Any part m ents , step 112 is optional and the extraction process takes
of the plant that contains cannabinoid resin glands can be place with the ethanol chilled or at room temperature , i.e .
included . Not all stems and leaves have these glands present. 50 within a range of - 60° C . to + 18° C .
In other cases , the raw cannabis plant material includes only In step 118 , the mixture of ethanol and plant material is
the flowers , or the raw cannabis plant material includes only pressurized to a pressure in the range of 70 - 280 kPa ( 10 - 40
the leaves and stems, i.e . the parts of the plant that would psi ). The aim is to select a pressure that is just low enough
normally be considered waste , in which valuable phyto to prevent a plug of plant material forming within the
chemicals are found only in lower concentrations. 55 material column . The actual value of the pressure is deter
In step 105 , the raw cannabis plant material is dried , if it mined by the material column packing . The tighter the raw
is not already provided in dried form . The raw cannabis plant cannabis plant material is packed into the column, the lower
material is dried in a dry room with a dehumidifier air is the upper pressure limit with which the ethanol can be
controller, or it may be flash dried in a vacuum oven at a driven through the column . While under pressure , the tem
pressure of < 2 kPa. Ideally , the moisture content of the raw 60 perature of the mixture may vary by up to 25° C ., but it
cannabis plant material after drying is 10 % or below , by should not be allowed to rise above - 35° C . Note that in
weight. The temperature of the oven and the drying time some embodiments , pressure is applied to the mixture of
depend on how much moisture the raw material has , and ethanol and plant material by centrifugal action .
how much raw material there is . Moisture content is mea - In step 120 , the plant material is allowed to soak in the
sured using a moisture analyzer. In some embodiments a 65 ethanol for a while in order to allow the cannabinoids to
hygrometer may be used . The lower the moisture content is , dissolve into it. Typically , the plant material soaks for up to
the better,because lower moisture will cause less dilution of 15 minutes provided that the temperature is below - 35° C .
 US 10 ,406 ,453 B2
In other embodiments , the soaking time may be different. of between 10 -50° C . Other filter media or material, or a
The pressure is maintained in the range of 70 - 280 kPa filter screen may be used instead . For example , the solution
( 10 - 40 psi) while the mixture of ethanol and plant material is filtered through a 10 - 30 um paper filter or screen and then
is soaking. through an 0 .25 - 1 um paper filter or screen . In other embodi
In step 122, the ethanol, now with the crude oil and 5 ments , a different number of paper or screen filters can be
dissolved cannabinoids, is drained off from the bulk of the used , and they can have different sizes . In another example ,
plant material, to form a mixture of crude oil and ethanol. a filter cartridge is used , with a pore size of 0 . 2 -1 um .
This mixture is the total fluid that comes directly out of the In step 129 , the crude oil and ethanol mixture is reheated
extractor (material column ) post-extraction . The crude oil to a temperature between 60° C . and 78° C . for further
contains cannabinoids and other phyto - compounds, and is 10 treatment
dissolved in the ethanol. The mixture also contains some step and .perform In other embodiments it is possible to omit this
the subsequent treatment and filtration
unwanted residual plant matter and other undesirable com steps at room temperature or even using the crude oil and
ponents . The crude oil and ethanol mixture is drained off
under a pressure in the range of 70 -280 kPa ( 10 - 40 psi ), i.e . ethanol mixture in its previously chilled state, or at another
it is the same pressure as the pressure used to soak the
the plant
plant 1515 chilled
chi temperature , e .g . as low as - 40° C .
material. In other embodiments, a vacuum is used to drain In step 130 , the crude oil and ethanol mixture is treated
the crude oil and ethanol mixture instead of the application with an agulite clay, also known as fuller 's earth clay,
of pressure . palygorskite, attapulgite, or bentonite . The clay primarily
In other embodiments , the ethanol is pumped continu removes pigments. The clay, when in particulate form , is
ously through the raw cannabis plantmaterial under pressure 20 first added to the heated crude oil and ethanol mixture and
in the range of 70 -280 kPa (10 -40 psi), without the specific then the mixture is agitated . The average size of the clay
soaking step . particles is in the range 0 .25 - 150 um , although other sizes
Optionally , in step 123 , a centrifuge is used to separate the are possible in other embodiments .
further plantmaterial from the crude oil and ethanol mixture . The crude oil and ethanol mixture is then cooled , or
The centrifuge may be used instead of the step 122 of 25 allowed to cool to a temperature of between 10 -50° C . in
draining of the material column , or instead of the pumping step 132 . Any clay that is in the crude oil and ethanol
of ethanol through the raw material under pressure . In this mixture is removed by filtering it out in step 133, using
case the contents of thematerial column are transferred into borosilicate glass filter paper, particularly if it has been
the centrifuge directly , or into a mesh bag and then placed added to the crude oil and ethanol mixture during the
into the centrifuge. 30 treatment process. Other filter media or material, or a filter
In step 124 , the crude oil and ethanolmixture is heated to screen may be used instead . For example , the solution is
a temperature between 60° C . and 78° C . for treatment with filtered through a 10 - 30 um paper filter or screen and then
charcoal. It is important not to exceed the upper temperature through an 0 .25 - 1 um paper filter or screen . In other embodi
of this range , because targeted elements in the crude oil will ments, a different number of paper or screen filters can be
melt into the liquid state and will be unable to be filtered out. 35 used , and they can have different sizes . In another example ,
Also , the ethanol will boil and there may be cannabinoid a filter cartridge is used , with a pore size of 0 .2 - 1 um .
degradation . In other embodiments it is possible to omit this In step 134, the crude oil and ethanol mixture is reheated
step and perform the subsequent filtration steps at room to a temperature between 60° C . and 78° C . for still further
temperature or even using the crude oil and ethanol mixture filtering. In other embodiments it is possible to omit this step
in its previously chilled state , or at another chilled tempera - 40 and perform the subsequent treatment and filtration steps at
ture, e . g . as low as - 40° C . room temperature or even using the crude oil and ethanol
In the following steps , the crude oil and ethanol mixture mixture in its previously chilled state , or at another chilled
is treated and filtered to remove further plant material that is temperature , e . g . as low as -40° C .
unavoidably retained in the mixture during the draining step . In step 135 , the crude oil and ethanol mixture is then
Treatment and filtration remove fats , lipids, chlorophyll, 45 treated with silica . The silica removes very fine plantmatter
waxes, heavy metals and other undesirable chemicals . Typi - and other particulates. The silica , when in particulate form ,
cally , there are 1 - 5 differentmedia treatments . While filtra - is first added to the heated crude oil and ethanolmixture and
tion is almost always required , the filtration steps required then the mixture is agitated . The average size of the silica
are not necessarily as robust if the ethanol used in the particles is in the range 0 . 25 - 150 um , although other sizes
primary extraction phase is chilled , compared to if the 50 are possible in other embodiments . The removal very fine
ethanol is non - chilled . solid particulates helps the winterization of the oil to occur
In step 125 , the crude oil and ethanolmixture is treated faster. Additionally, it allows for visibility of the product,
with charcoal. The charcoal removes pigments , chlorophyll , which in turn allows one to review the integrity of the
heavy metals and particulates . Charcoal is used as the first filtration process .
treatment medium in order to remove as much pigment as 55 The crude oil and ethanol mixture is then cooled or
possible . The charcoal, when in particulate form , is first allowed to cool to a temperature of between 10 - 50° C . in
added to the heated , room temperature or chilled crude oil step 137 . Any silica that is in the crude oil and ethanol
and ethanol mixture and then the mixture is agitated . The mixture is removed by filtering it out in step 138 , using
average size of the charcoal particles is in the range 0 .25 - 150 borosilicate glass filter paper, particularly if it has been
um , although other sizes are possible in other embodiments . 60 added to the crude oil and ethanol mixture during the
The crude oil and ethanol mixture is then cooled , or treatment process . Other filter media or material, or a filter
allowed to cool to a temperature of between 10 - 50° C . in screen may be used instead . For example , the solution is
step 127 . Any charcoal that is in the crude oil and ethanol filtered through a 10 - 30 um paper filter or screen and then
mixture is removed by filtering it outusing borosilicate glass through an 0 .25 - 1 um paper filter or screen . In other embodi
filter paper, in step 128 , particularly if it has been added to 65 ments, a different number of paper or screen filters can be
the crude oil and ethanol mixture during the treatment used , and they can have different sizes . In another example ,
process. Filtering out the charcoal is done at a temperature a filter cartridge is used , with a pore size of 0 . 2 -1 um .
 US 10 ,406 ,453 B2
In step 160 , the resulting oil and ethanol mixture is then also set in the range 100 - 115º C ., and is also more usually
processed with a rotovap to remove and reclaim any ethanol set in the range 107 - 110° C . The temperature of the target
that remains in it. The temperature of the rotovap is 43- 490 heater, which controls the temperature of the inner wall 372 ,
C ., and it is operated at a pressure of 83 - 101 kPa ( 25 - 30 is set within a range of 168 .5 - 170° C . The condensing coil
inHg, 635 -760 mmHg). Other evaporators may be used in 5 376 is set at a temperature of 74° C ., as is the target or
other embodiments. The ethanol that is reclaimed can be distillate discharge arm 380 and its associated pump (not
used to extract cannabinoids from a further batch of dried shown ). The temperature of the cold trap between the
and ground raw cannabis plant material. vacuum port 396 and the vacuum pump is - 22 to - 30° C .,
After the remaining ethanol has been removed using the although even cooler temperatures are possible . The film
rotovap , decarboxylation is performed on the resulting oil in 10 wipe process is performed at a pressure of 0 .03 -0 .08 mbar,
step 165 . The oil is heated to 120 - 140° C . in order to or lower.
evaporate residual solvents and to convert THCa into THC , The result from the distillate discharge arm is a tasteless ,
releasing CO2 in the process. If the temperature is below this odourless oil that contains up to 99 % pure cannabinoids.
range , then potentially there will be some residual ethanol. Often , however, the further residual oil will require another
The majority of the CO2 that is produced from decarboxy - 15 pass through the wiped -film apparatus in order to achieve
lation is removed in order to ensure consistent vacuum purities of 90 % and over.
levels later on in the process. If the temperature is above this Using this process, a given weight of dried cannabis can
range , then product degradation occurs. The oil is warmed be turned into very approximately 10 - 15 % crude oil, which
up gradually while stirring so as not to overheat portions of yields anywhere from 4 - 10 % pure cannabinoids, again very
it. In the decarboxylation step the residual ethanol is not 20 approximately .
reclaimed . The decarboxylation process typically takes sev
eralhours. Note that in an embodiment described below , the D . Apparatus
decarboxylation step is not performed in a rotovap , but in a
wiped film under vacuum , to lower the required contact Referring to FIG . 3, an example of the apparatus is shown
temperatures and prevent oxidation . 25 schematically . Raw cannabis plant material is provided in a
In step 170 and referring to FIG . 3 , the decarboxylated oil hopper 202, for example, and is released in batches into
is run through a short- path distillation film wipe apparatus container 204 . The raw cannabis plant material is dried in
370 . Since we are using a wiped film distillation process vacuum oven 210 . Next, the dried plant material is placed
versus a conventional short path still apparatus it is impor - into a grinder 220. After the grinding step , the ground plant
tant to have separated the waxes , fats and lipids pre - 30 material is placed into one or more material columns 240 .
distillation . If this is not done, the waxes, fats and lipids will Each column has a lid 241 that is removable so that the
be wiped onto the wipe film causing the distillation of some ground plant material can be placed into it . Each column
of these elements into the final product. holds 1. 5 - 4 .5 kg ( 3 - 10 lb ) of plant material depending on its
The decarboxylated oil is first run through the short-path size. Other capacities are also possible . In one example
distillation film wipe apparatus to remove some volatile 35 apparatus , there are four material columns 240. The material
terpenes . The temperature of the feed tank 365 to the film column may be surrounded by an insulating wall or vacuum
wipe is set in the range 100 - 115º C ., and is more usually set jacket 242, which can be evacuated via port 244 . Alternately,
in the range 107 - 110° C . The temperatures of the pump 366 an insulating jacket may be wrapped around the material
and feed line 367 to the film wipe are set at the same value column. The insulating wall 242 or jacket helps to maintain
as the feed tank . The temperature of the residue discharge 40 the contents 246 cool in the process that uses chilled ethanol
arm 390 and its associated pump, not shown, is also set in as the solvent. When using chilled ethanol, the material
the range 100 - 115° C ., and is also more usually set in the column is maintained chilled by the use of pressurized ,
range 107 - 110° C . The temperature of the target heater, liquid CO2 in the jacket. The ethanol 250 is cooled in a
which controls the temperature of the inner wall 372 , is set cryogenic tank 260 , the inner temperature of which is
within a range of 155 - 162° C ., usually 159.5° C . The 45 maintained low by a jacket 262 filled with pressurized liquid
condensing coil 376 is set at a temperature of 58° C ., as is CO , via port 264 . In other embodiments , other refrigerants
the target or distillate discharge arm 380 and its associated can be used , or a chiller or heat exchanger can be used .
pump (not shown ). A further temperature control unit main - Pressurized nitrogen gas is fed into the port 272 , forcing
tains the temperature of a cold trap between the vacuum port the chilled ethanol 250 through insulated tube 274 into the
396 and the vacuum pump at - 22 to - 30° C ., although even 50 material column 240. The pressure of the nitrogen is used to
cooler temperatures are possible . The film -wipe process is maintain the pressure of the mixture 246 of ethanol and raw
performed at a pressure of 0 . 3 - 0 . 8 mbar, or lower . cannabis plantmaterial, and / or to pump the ethanol through
In step 175 , the residual oil , after volatile terpene removal, the raw cannabis plant material. After the raw cannabis plant
is re -run through the short- path distillation film wipe to material has soaked in the ethanol, the ethanol, now with
remove some non -volatile terpenes. All of the temperatures 55 dissolved cannabinoids, is drained out of the material col
are the same except for the temperature of the inner wall, umn 240 as a mixture of crude oil and ethanol, via outlet
which is typically set to a higher temperature and is in the pipe 276 into container 280 . The bulk of the raw cannabis
range 159 - 162° C . The pressure is the same, at 0 . 3 - 0 . 8 mbar, plant material remains in the material column 240 . The
or lower . crude oil and ethanolmixture may alternately be pumped out
In step 180 , the further residual oil is again run through 60 of the material column under the pressure of the nitrogen .
the short - path distillation film wipe to remove the cannabi- Optionally , a centrifuge 290 is used to separate the bulk
noids as a whole . The temperature of the feed tank 365 to the of the plantmaterial from the mixture. If the centrifuge 290
film wipe is set in the range 100 - 115° C ., and is more usually is used , the contents of the material column are emptied into
set in the range 107 - 110° C . The temperatures of the pump the centrifuge , which then separates the bulk of the plant
366 and feed line 367 to the film wipe are set at the same 65 material from the crude oil and ethanol mixture . The cen
value as the feed tank . The temperature of the residue trifuge 290 may be used instead of the draining of the
discharge arm 390 and its associated pump, not shown , is material column, or instead of the pumping of ethanol
 US 10 ,406 ,453 B2
10
through the raw material under pressure , or it may be used Referring to FIG . 5 , details of the alternate process for the
as well as the draining and /or pumping steps. extraction of cannabinoids are shown. Steps 420 -432 relate
The crude oil and ethanol mixture is then treated with to the primary extraction phase. Steps 434 -452 relate to the
various media and fed into multiple different filters sequen media treatment and filtration stage . The remove and reclaim
tially. In this embodiment, the first treatment unit is charcoal 5 ethanol stage 454 and the non-polar solvent removal stage
310. Below the charcoal there is a 10 - 30 um filter 311 and 464 form the solvent reclamation phases . Steps 456 - 463 are
an 0 . 25 - 1 um filter 312 for filtering out charcoal. Next there the brine washing stage . Step 466 relates to the decarboxy
is a clay treatment unit 314 , below which is a 10 - 30 um filter lation stage, and step 468 relates to the distillation of the
315 and an 0 .25 - 1 um filter 316 for filtering out the clay. cannabinoids.
Following this is a silica treatment 318 , below which is a 10 In step 420 , raw cannabis plant material is provided . In
10 - 30 um filter 319 and an 0 . 25 - 1 um filter 320 for filtering step 422 , the raw cannabis plant material is dried , if it is not
out the silica . Each of the filters can be independently already provided in dried form . Ideally , themoisture content
replaced . After filtration , the resulting oil and ethanol mix of the raw cannabis plant material after drying is 10 % or
ture leaves the final filter via exit pipe 324 and is collected to below , by weight . In other embodiments , the moisture
in container 328. content can be as high as 15 % while still allowing for an
The filtered oil and ethanolmixture is then passed into a acceptable process . In other embodiments , other drying
rotovap 340 . The oil and ethanol mixture 342 is maintained techniques may be used .
at an elevated temperature in flask 346 , which is heated in In step 424 , the dried plant material is ground , for
a temperature bath 348 . Flask 350 collects the ethanol 352, 20 example to an average size between 250 - 300 um . However,
which is evaporated from the oil and ethanolmixture 342 . it is possible in other embodiments to grind the dried plant
After the ethanol 352 has been reclaimed from the oil 342 , material to a size of thousands of microns, and the process
the oil is decarboxylated in container 360, which is heated has been found to work with average particle sizes of up to
by heater 362. During the decarboxylation process , the oil 3000 - 9000 um . Note that, in other embodiments , the grind
363 is stirred by a magnetic stirrer 364. After decarboxy - 25 ing step may take place before the drying step . The ground
lation , the oil 363 is transferred to a feed chamber 365 . At and dried plant material is then placed in a closed , porous
the bottom of the feed chamber 365, a pump 366 pumps the bag .
oil via a feed line 367 and a check valve 368 into a short-path In step 426 , the ethanol is chilled ( if necessary ) to a
film wipe apparatus 370 . Pump rates are typically 1000 - temperature between -60° C . and + 18° C ., in a tank sur
1500 ml/hr, and depend on the Co , being given off , if any, 30 rounded by a pressurized liquid CO2 jacket, for example . In
the percentage of THCa converted to THC , and the vacuum some embodiments , the ethanol is used at room temperature ,
pressure of the short -path film wipe apparatus. In the short- i.e . 18° C . However, chilled ethanol, when used for extrac
path film wipe apparatus 370 , the oil is wiped in a thin film tion , reduces impurities like fats , lipids and pigments in the
around the heated , inside wall 372 of the film wipe apparatus
370 by a blade 374. The inside wall 372 is heated via a 35 In step 428 , the chilled ethanol is added to the WSD
temperature -maintained jacket. A cooler, condensing coil separator into which the bag of ground and dried plant
376 condenses the target fraction , which leaves the film wipe material has been placed . Typically, approximately 40 - 50
apparatus 370 as a distillate via target discharge tube 380 liters of chilled ethanol are used for every 5 -6 kg of plant
and is collected in container 382. The residual liquids fall material (i.e . 6 .6 - 10 liters per kg) , although it is possible that
down the inside wall 372 of the film wipe 370 and exit 40 other ratios can be used . In step 430, the plantmaterial and
through residual arm 390 to be collected in container 392 . ethanol mixture is run through the wash and spin modes of
The film wiping occurs under reduced pressure provided by the WSD separator. The ethanol is continuously fed into the
a vacuum pump connected to port 396 via a cold trap . drum as it is spun . Depending on the embodiment, the drum
is spun for 8 - 15 minutes. The ethanol, in some embodi
E . Further Exemplary Process 45 ments, is pressurized to between 1- 15 psi (7 - 100 kPa) as is
it fed into the drum . Due to the centrifugal force , the crude
Referring to FIG . 4 , a flowchart summarizing the basic oil is extracted (i.e . dissolved into the ethanol). The extent of
steps of an alternate process is shown . the drying, i.e . removal of liquid from the plant material,
In step 402 , after adding ethanol to a WSD separator depends on the speed of the spin cycle . The WSD separator
containing the raw cannabis plant material, the plant mate - 50 has a centrifuge drum for the wash and extraction , and a spin
rial is washed with the ethanol in the WSD . The raw cycle mode to separate off the solvent. In step 432, the
cannabis plant material is then “ dried ” using the spinning ethanol, now with dissolved extracts (i.e . a crude oil and
cycle function of the WSD separator. Then , in step 404 , the ethanol mixture ), is drained out of the centrifuge drum
resulting crude oil and ethanol mixture is treated with during the spin cycle mode . The crude oil and ethanol
different media and filtered . During step 404 , impurities 55 mixture is drained off as a result of the centrifugal force due
contained in the crude oil and ethanolmixture are removed to the spinning action of the drum . The solid plant material
In step 406 , the ethanol from the resulting oil and ethanol remains inside the mesh bag .
mixture is evaporated and reclaimed . After that, in step 408 , In some embodiments where the ethanol is chilled , the
the oil is washed with a brine solution and then the non -polar optimum temperature has been found to be - 45° C . How
solvent added prior to the brine wash is removed in step 410 . 60 ever, the optimum temperature may be different in other
Steps 406 and 410 are considered to be the solvent recla - embodiments .
mation stages . In the following steps, the crude oil and ethanol mixture
In step 412 , the oil remaining after the evaporation of the is treated with different media and filtered to remove chlo
non -polar solvent is decarboxylated to activate the THC and rophyll , pigments , plant material and any other impurities
evaporate any remaining solvent. The residue after decar- 65 that are unavoidably retained in the mixture after the drain
boxylation is then , in step 414 , distilled using a film wipe ing step 432 . Typically , there are 1 - 5 different treatment
apparatus 592 in order to extract the cannabinoids . media .
 US 10 ,406 ,453 B2
12
In step 434 , the crude oil and ethanol mixture is treated C ., and it is operated at a pressure of 83 - 101 kPa (25 - 30
with charcoal ( charcoal scrub ). The crude oil and ethanol inHg, 635 - 760 mmHg). Other evaporators or evaporation
mixture is at a temperature between - 10° C . and + 85° C . for techniques may be used in other embodiments , for example
the charcoal scrub . The charcoal, when in particulate form , falling film evaporators , rising film evaporators or flash and
is first added to the crude oil and ethanol mixture and then 5 spray dryers can be used . The ethanol that is reclaimed may
the mixture is agitated . The average size of the charcoal be used to extract cannabinoids from a further batch of dried
particles is in the range 0 . 25 - 150 um , although other sizes and ground raw cannabis plant material. Typically , 75 % of
are possible in other embodiments . the ethanol used is reclaimed .
Any charcoal that is in the crude oil and ethanol mixture The oil, now without ethanol, is then mixed with hexane ,
is removed by filtering it out using lenticular depth filtration 10 heptane or pentane (non -polar solvents ) with the mixing
apparatuses and/ or column housing filters with insert car ratio of hexane, heptane or pentane to oil of 1 : 1 in step 456
tridges , in step 436 . Lenticular depth filtration systems to result in an oil and solvent mixture . Note that other ratios
usually use lenticular shaped filters that are able to retain and are also possible . The role of non -polar solvents here is to
collect the charcoal particles . A filter cartridge with a pore further extract the oil for following processing steps, due to
size of 0 . 2 - 1 um is used . Filtering out the charcoal is done 15 their ability to solubilize cannabinoids . Non - polar solvents
at a temperature between - 10° C . and 50° C . such as hexane , heptane or pentane dissolve fats and oils and
In another embodiment, lenticular filtration alone for the leave behind proteins, carbohydrates and other impurities
charcoal treatment is used to take care of both the charcoal insoluble in these solvents and other non -polar solvents .
treatment and the filtration process simultaneously . This type of solvent is also used in the oil extraction field for
In step 438 , the crude oil and ethanol mixture is reheated 20 its ability to be removed due to its low boiling point. In
to a temperature between 60° C . and 78° C . for further addition to that, non -polar solvents exhibit the property of
treatment. In other embodiments it is possible to omit this being insoluble in water, which helps to a certain extent to
step and perform the subsequent treatment and filtration separate water and other water - solubles from the non -polar
steps at room temperature or even using the crude oil and solvent.
ethanol mixture in its previously chilled state , or at another 25 Next, the brine solution is added to the oil and solvent
chilled temperature , e. g . as low as - 40° C . mixture in step 458. The oil and solvent mixture is then
In step 440 , the crude oil and ethanolmixture is treated washed with brine (60 % to 100 % saturated in salt ) to remove
with a bentonite clay. The clay , when in particulate form , is water- soluble compounds in step 460 , and to remove impu
first added to the heated crude oil and ethanol mixture and rities and any traces of the treatment media that may have
then the mixture is agitated . The average size of the clay 30 remained in the oil. Brine helps to disrupt emulsions and dry
particles is in the range 0 .25 - 150 um , although other sizes the oil by extracting water that may have dissolved in the
are possible in other embodiments . mixture , and also extracts ethanol from the non -polar phase
The crude oil and ethanol mixture is then allowed to cool and crude oil into the brine solution . Afterwards the brine
to a temperature of between 10 -50° C . in step 442. Any clay solution is separated from the oil in step 462.
that is in the crude oil and ethanol mixture is removed by 35 The brine solution is prepared with distilled water and
filtering it out in step 444 using lenticular depth filtration kosher salt , i.e . iodine- free sodium chloride . After brine
apparatuses and /or column housing filters with insert car washing, the brine, with water -soluble compounds, is sepa
tridges . A filter cartridge with a pore size of 0 . 2 - 1 um is used . rated from the oil and non -polar solvent by means of a
In step 446 , the crude oil and ethanol mixture is reheated centrifuge or a gravity fed separatory funnel. Unless
to a temperature between 60° C . and 78° C . for still further 40 99. 9999 % purity solvents are used , there is always a water
treatment. In other embodiments it is possible to omit this content that extracts solubles ( i. e. sugars ) from the raw
step and perform the subsequent treatment and filtration cannabis plant material in the primary extraction stage .
steps at room temperature or even using the crude oil and These water - soluble compounds need to be removed
ethanolmixture in its previously chilled state , or at another through a liquid to liquid extraction brine wash .
chilled temperature , e . g . as low as - 40° C . 45 As an example , 500 ml of hexane, pentane or heptane is
In step 448, the crude oil and ethanol mixture is then added to 500 ml of oil and then homogenized by means of
treated with magnesium oxide . The magnesium oxide , in an overhead stirrer. Then , 1000 ml of distilled water satu
particulate form , is first added to the heated crude oil and rated with kosher sodium chloride at 60 - 100 % saturation is
ethanol mixture and then the mixture is agitated . The aver - added to the oil and solvent mixture (i. e . the ratio of
age size of the magnesium oxide particles is in the range 50 non -polar solvent to oil to brine is 1 : 1 : 2 ) and agitated for 5
0 .25 - 150 um , although other sizes are possible in other to 30 min with an overhead stirrer.
embodiments. After the brine has been removed from the oil, the
The crude oil and ethanol mixture is then allowed to cool remaining traces of water , if any, are then removed from the
to a temperature of between 10 -50° C . in step 450. Any oil with a magnesium sulfate treatment, in step 463, in which
magnesium oxide that is in the crude oil and ethanolmixture 55 powdered MgSO4 is swirled around in the oil and then
is removed by filtering it out in step 452 , using lenticular filtered off , e .g . by gravity filtration .
depth filtration apparatuses and /or column housing filters In step 464, the oil and solvent mixture is then processed
with insert cartridges. with a rotovap to remove and reclaim the non -polar solvent.
In one embodiment, the filtering off of the charcoal ( step The temperature of the rotovap is 43 -49° C ., and it is
436 ) , the clay ( step 444 ) and the MgO ( step 452) are all 60 operated at a pressure of 83 - 101 kPa ( 25 - 30 inHg, 635 - 760
performed as a single step after the treatment with Mgo . mmHg ). The non -polar solvent such as hexane , heptane
In a further embodiment, a silica gel is used as a media and /or pentane that is reclaimed may be used for future brine
treatment, after the clay treatment and before the Mgo wash applications. About 75 % of the non -polar solvent is
treatment. reclaimed for further use .
In step 454 , the resulting oil and ethanol mixture is then 65 After the non - polar solvent has been removed using the
processed with a rotovap to remove and reclaim the ethanol rotovap , decarboxylation is performed on the resulting oil in
from the mixture . The temperature of the rotovap is 43 -49° step 466 . Decarboxylation is carried out to convert THCa
 US 10 ,406 ,453 B2
13 14
into THC , releasing CO2 in the process. In the process , the temperature is above this range, then product degrada
residual solvents that may be present are evaporated off . tion occurs. This method of decarboxylation process typi
In one embodiment, the oil is first run through a short-path cally takes several hours.
distillation film wipe apparatus 592 to convert THCa to There are other ways in which the decarboxylation pro
THC . The temperature of the feed tank 584 ( FIG . 6B ) to the 5 cess can be carried out. For example , the cannabis resin is
film wipe is set in the range 100 - 115º C . The temperatures heated while on the plant biomass in ovens similar to the
vacuum ovens used to dry the cannabis plant, prior to adding
of the pump 586 and feed line 588 to the film wipe apparatus
592 are set at the same value as the feed tank 584 . The the heat
ethanol for primary extraction . The process is to simply
the biomass to 90° C . for a period of time subject to the
temperature of the residue discharge arm 604 and its asso 10 quantity of biomass being heated .
ciated pump, not shown, is also set in the range 100 - 115° C ., The decarboxylated oil is run through the short-path
and is also more usually set in the range 107 - 110° C . The distillation film wipe apparatus 592 once again , this time to
temperature of the target heater, which controls the tempera remove some volatile terpenes . The temperature of the feed
ture of the inner wall 594 , is set within a range of 140 - 1750 tank 584 to the film wipe 592 is set in the range 100 - 115° C .,
C ., usually 170° C . 15 and is more usually set in the range 107 - 110° C . The
The temperature of the inner wall isis controlled
iner wall controlled by
by setting
setting temperatures of the pump 586 and feed line 588 to the film
the temperature of a bath 595 . A pump then circulates fluid wipe 592 are set at the same value as the feed tank 584 . The
that is heated to the bath temperature through a jacket around temperature of the residue discharge arm 604 and its asso
the outside of the wall. As such , it is to be expected that the ciated pump, not shown , is also set in the range 100 - 115° C .,
inner wall temperature is slightly below that of the bath 20 and is also more usually set in the range 107 - 110° C . The
temperature, depending on , for example , the temperature temperature of the target heater, which controls the tempera
and rate at which the oil is wiped onto the inner wall 594 . ture of the inner wall 594 , is set within a range of 140 - 145°
Other temperatures of the film wipe apparatus are set in a C ., usually 145º C . The condensing coil 598 is set at a
similar way. These other temperatures are also expected to temperature of 0 to - 20° C ., as is the target or distillate
be slightly different to the bath setting , but not to a signifi - 25 discharge arm 600 and its associated pump ( not shown ), via
cant level. The condensing coil 598 is set at a temperature of which the terpenes are removed . Liquid nitrogen is used to
0° C . to - 20° C ., as is the target or distillate discharge arm maintain cryogenic temperatures of a cold trap between the
600 and its associated pump (not shown ). vacuum port 608 and the vacuum pump at - 180 to - 196° C .
Liquid nitrogen is used to maintain cryogenic tempera This film -wipe process is performed at a pressure of 0 .001
tures in a cold trap between the vacuum port 608 and the the 30 0 .01 mbar.
vacuum pump (not shown ) of - 180° C . to - 196° C . Use of runThe residual oil from the preceding film wipe step is again
these temperatures allows for a deep vacuum to be main 592 to removethesome
through short -path distillation film wipe apparatus
tained . The film -wipe process is performed at a pressure of terpenes are removednonin - volatile terpenes . Mostly volatile
the prior step and mostly non
150 - 200 mbar. The decarboxylated oil is collected via the 35 volatile terpenes removed in this step , as there is no sharp
distillate arm . cut-off between volatile and non -volatile terpenes. The tem
While the film wipe temperature is higher than the mini perature of the feed tank 584 to the film wipe is set in the
mum 90° C . required for THCa conversion under vacuum , range 100 - 115° C ., and is more usually set in the range
and in the range where product degradation may occur, the 107 - 110° C . The temperatures of the pump 586 and feed line
dwell time at these elevated temperatures in the film is low 40 588 to the film wipe 592 are set at the same value as the feed
enough that insignificant amounts of product degradation tank 584. The temperature of the residue discharge arm 604
occur. Also, the temperature settings do not actually repre - and its associated pump, not shown, is also set in the range
sent the contact temperature , as the settings are set on the 100 -115° C ., and is also more usually set in the range
circulation bath fluid and do not represent the temperature of 107 - 110° C . The temperature of the target heater , which
the oil that is in contact with the glass surface area of the 45 controls the temperature of the inner wall 594 , is set within
evaporator. The glass acts as an insulator between the heat a range of 145 - 159° C ., usually 155° C . The condensing coil
transfer fluid and the oil. The temperature difference 598 is set at a temperature of 20 to 60° C ., as is the target
between the heat transfer fluid from the bath and the heated or distillate discharge arm 600 and its associated pump (not
oil is expected to be in the range of 1 -5° C . shown ), via which the terpenes are removed . Liquid nitrogen
Decarboxylation is performed under vacuum to lower the 50 is used to maintain cryogenic temperatures of a cold trap
temperature required to convert the THCa to THC . It can between the vacuum port 608 and the vacuum pump at - 180
either be done in the film wipe apparatus 592 effectively as to - 196° C . Use of the cryogenic temperatures allows for a
a decarboxylation pass or done in a heated reactor ( e . g . 504 ), deeper vacuum to be maintained . This film -wipe process is
for example . The oil itself needs to reach temperatures of at performed at a pressure of 0 .001- 0 .01 mbar.
least 105° C . at atmospheric pressure. If a vacuum reactor is 55 The residual oil from the preceding film wipe step is again
used the oil needs only to be heated to at least 90° C . The run through the short -path distillation film wipe apparatus
same temperature (90° C .) may also be used when the film 592 to remove the cannabinoids as a whole . The temperature
wipe apparatus 592 is used . The film wipe decarboxylation of the feed tank 584 to the film wipe is set in the range
process allows for a much lower heat residence time so that 100 - 115° C ., and is more usually set in the range 107 -110°
degradation of the oil is lower when compared to decar - 60 C . The temperatures of the pump 586 and feed line 588 to
boxylating in a reactor. the film wipe 592 are set at the same value as the feed tank
In other embodiments, decarboxylation is carried out by 584. The temperature of the residue discharge arm 604 and
heating the oil to 90 - 110° C . under vacuum in an oven . If the its associated pump, not shown , is also set in the range
temperature is below this range , then potentially there will 100 - 115° C . , and is also more usually set in the range
be some residual solvent. The majority of the CO2 that is 65 107 - 110° C . The temperature of the target heater, which
produced from decarboxylation is removed in order to controls the temperature of the inner wall 594 , is set within
ensure consistent vacuum levels later on in the process . If a range of 140 -165° C . The condensing coil 598 is set at a
 US 10,406 ,453 B2
15 16
temperature of 68 -73° C ., as is the target or distillate Each of the filter cartridges can be independently
discharge arm 600 and its associated pump (not shown ), via replaced . Further treatmentmedia and filter groups are used
which the cannabinoids are removed . Liquid nitrogen is for additional treatment media in other embodiments.
used to maintain cryogenic temperatures of a cold trap The resulting oil and ethanol mixture is then passed into
between the vacuum port 608 and the vacuum pump at - 180 5 a rotovap 554 . The oil and ethanol mixture 556 is maintained
to - 196° C . The film -wipe process is performed at a pressure at an elevated temperature in flask 558 , which is heated in
of 0 .0008 - 0 .003 mbar. This pass requires the use of a a temperature bath 560 . Flask 562 collects the ethanol 564 ,
diffusion pump to assist with achieving deeper vacuums. It which is evaporated from the oil and ethanol mixture 556 .
is installed on the film wipe apparatus 592 but not used for Hexane, heptane or pentane is then added to the oil and
the decarboxylation and terpene fraction passes. 10 ethanolmixture with a mixing ratio of 1 : 1 , to form an oil and
The result from the distillate discharge arm 600 is a solvent mixture , which is stirred with an overhead stirrer
tasteless , odorless oil that contains up to 99 % pure cannabi 566 . The brine solution is added to the solution of oil/
noids. Often , however, the resulting oil will require another solvents and homogenized by means of an overhead stirrer
568 . The water (as brine ) is then separated from the mixture
pass through the wiped - film apparatus 592 in order to 15 of brine/oil/solvent by means of a mechanical centrifuge
achieve purities of 90 % and over. 570 .
The oil and solvent mixture is then passed into a rotovap
F . Further Apparatus 572 . The oil and solvent mixture 574 is maintained at an
elevated temperature in flask 576 , which is heated in a
Referring to FIGS. 6A - B , an example of the apparatus for 20 temperature bath 578 . Flask 580 collects the solvent 582 .
the further exemplary process is shown schematically. which is evaporated from the oil and solvent mixture 574 .
Raw cannabis plant material is provided in a hopper 500 , After the solvents 582 have been reclaimed from the oil
for example , and is released in batches into container 502 . 574 , the oil is decarboxylated . In one embodiment, the oil
The raw cannabis plant material is dried in vacuum oven 574 is transferred to a feed chamber 584 of a film wipe
504 . Next, the dried plant material is placed into a grinder 25 apparatus 592 . At the bottom of the feed chamber 584 , a
506 . pump 586 pumps the oil via a feed line 588 and a check
After the grinding step , in one embodiment, the ground valve 590 into the short-path film wipe apparatus 592 . Pump
plant material is placed into a bag in one or more WSD rates are typically 1000 - 1500 ml/hr, and depend on the CO ,
separator units 508 . being given off, if any , the percentage of THCa converted to
After the raw cannabis plant material has been processed 30 THC , and the vacuum pressure of the short -path film wipe
in the ethanol, the ethanol, now with dissolved cannabi apparatus 592 . In the short -path film wipe apparatus 592 , the
noids, is drained out of the WSD separator 508 as a mixture oil is wiped in a thin film around the heated , inside wall 594
of crude oil and ethanol, via outlet pipe 510 into container of the film wipe apparatus 592 by a blade 596 . The inside
wall 594 is heated via a temperature -maintained jacket . A
512 . An example extraction vessel holds 5 -5 .5 kgs of cooler, condensing coil 598 condenses the target fraction ,
biomass in a single biomass cavity . Other capacities are also 35 which leaves the film wipe apparatus 592 as a distillate via
possible . The vessel is surrounded by an insulating jacket.
target
The crude oil and ethanol mixture is then fed into a The residual liquids discharge tube 600 and is collected in container 602 .
fall down the inside wall 594 of the film
charcoal treatment unit 514 and after being processed is then wipe 592 and exit through
fed into a lenticular depth filtration apparatus 516 via an inlet 4040 in container 606 . The film residual arm 604 to be collected
pipe 518 . The crude oil and ethanol mixture is filtered pressure provided by a vacuum pumpoccurs wiping under reduced
connected to port 608
through one or more lenticular depth filtration cartridges via a cold trap .
520 . The lenticular depth filtration cartridges 520 retain the Using the system of the present invention it is possible to
particles present in the crude oil and ethanolmixture within convert approximately 40 to 44 kg (88 to 97 lb ) of raw
its structure . The crude oil and ethanol mixture is further 45 cannabis plantmaterial into pure or nearly pure distillate oil
carried into the central column 522 of the lenticular depth over a period of 16 hours. The apparatus and process may
filtration apparatus 516 and collected through an outlet pipe also be used for the extraction , refinement and distillation of
524 in a container with a bentonite clay treatment media waste plant material from processes that do not succeed in
526 . extracting all the valuable extracts . The apparatus and pro
After processing with charcoal, the crude oil and ethanol 50 cess may be scaled up depending on the amount of raw
mixture is drained from the bentonite clay and then fed cannabis plant material to be treated .
through inlet pipe 528 into a further lenticular depth filtra
tion apparatus 530. The crude oil and ethanol mixture is then G . Variations
filtered through one or more lenticular depth filtration car
tridges 532 . The crude oil and ethanol mixture is further 55 While the best presently contemplated mode of carrying
carried into a central column 534 of the lenticular depth out the subjectmatter disclosed and claimed herein has been
filtration apparatus 530 and collected through an outlet pipe described , other modes are also possible .
536 into a container with a magnesium oxide treatment In some embodiments , a spinning band fractional distil
media 538 . lation apparatus is used instead of the short-pass film wipe
The crude oil and ethanol mixture is drained from the 60 apparatus for one or more of the film -wipe steps .
magnesium oxide and then fed via an inlet pipe 540 into In some embodiments the ethanol is not chilled in step
another lenticular depth filtration apparatus 542 . The crude 112 , which is omitted, and the ethanol added to the raw
oil and ethanol mixture is then filtered through one or more cannabis plant material at a temperature of 15 - 30° C . in step
lenticular depth filtration cartridges 544 . The crude oil and 115 . In these embodiments, steps 127 , 132 and 137 are
ethanol mixture is further carried into a central column 546 65 omitted , as the ethanol is not chilled before paper filter
of the lenticular depth filtration apparatus 542 and then stages 128 , 133 and 138 . Filtration is particularly important
through an outlet pipe 550 into a container 552 . if the ethanol is used at room temperature . It has been found
 US 10,406 ,453 B2
18
that 10 % more extracts are obtained using room - temperature Throughout the description , specific details have been set
ethanol compared to using chilled ethanol, but that the forth in order to provide a more thorough understanding of
filtration stage is significantly more onerous . This is also the invention . However, the invention may be practiced
subjective to the type ofplant material used , but it is known without these particulars. In other instances , well known
that non - chilled ethanol has a greater miscibility , which 5 elements have not been shown or described in detail and
makes the ethanol less discriminative thus picking up more repetitions of steps and features have been omitted to avoid
unwanted materials . unnecessarily obscuring the invention . For example , various
Optionally , once the cannabinoids have been extracted in pumps , valves, jackets and lines are not shown for clarity .
step 180 or 468 , they may be further run through the filmd 10 regarded in ,an theillustrative
Accordingly specification and drawings are to be
, rather than a restrictive , sense .
wipe apparatus 592 in order to separate them into THC and It will be clear to one having skill in the art that further
CBD . In other embodiments, spinning band fractional dis variations to the specific details disclosed herein can be
tillation is used instead of the film wipe to separate the THC
made, resulting in other embodiments that are within the
and CBD . scope of the invention disclosed . Steps in the flowchart may
In other embodiments within the purview of the present 15 be performed in a different order, other steps may be added .
invention , other plant materials besides cannabis may be or one or more steps may be removed without altering the
processed . For example, hempmay be processed to result in main outcome of the process. All parameters, dimensions,
a 95 % pure CBD oil. The present invention has wide materials , and configurations described herein are examples
application in respect of other plants that produce phyto only and may be changed depending on the specific embodi
chemicals of interest, such as for the extraction of can - 20 ment. Accordingly , the scope of the invention is to be
nabimimetics from lavender. Phytochemicals of interest construed in accordance with the substance defined by the
include cannabinoids, terpenes , and flavonoids. following claims.
In some embodiments , the apparatus is portable so that it
can be taken to the different sites of various plant growers , The invention claimed is :
to be used on an as-needed basis . 25 1 . A process for extracting cannabinoids from raw can
In some embodiments , one or more further media treat - nabis plant material comprising the steps of:
ment steps making use of an attapulgite clay , a bentonite adding ethanol to dried and ground cannabis plantmate
clay and /or silica filtration media are added to the described rial to form an initial mixture ;
media treatment setups . centrifuging the initial mixture to separate a crude oil and
The mechanical centrifuge 570 used to separate the oil 30 ethanolmixture from the initial mixture ;
and solvent mixture from the brine can be replaced by a treating the crude oil and ethanol mixture with charcoal
gravity fed separatory funnel. particles, bentonite clay particles and magnesium oxide
As an alternative to the film wipe step 468, a vacuum particles to remove unwanted components therefrom ;
spinning band distillation or fractional distillation procedure evaporating ethanol from the treated crude oil and ethanol
can be used in order to remove four fractions, for example , 35 mixture to leave oil;
as opposed to the single fraction from the film wipe process. washing the oil with brine;
Ethanol of 99 % purity or more can be used for the heating the brine -washed oil to convert THCa ( tetrahy
extraction process . drocannabinolic acid ) in the brine-washed oil into THC
In some embodiments , to eliminate the brine wash step , (tetrahydrocannabinol), resulting in decarboxylated oil;
anhydrous ethanol ( 0 .005 % water) is used instead of the 40 and
more usual ethanol formula that is approximately 95 % pure distilling the decarboxylated oil to obtain cannabinoids.
with 5 % water . This reduces the need for more robust 2 . The process of claim 1, further comprising the steps of:
filtration post extraction. However, steps should be taken to adding a non -polar solvent to the oil before washing the
avoid instantaneous water contamination when the anhy oil with brine ; and
drous ethanol is exposed to air . 45 evaporating the non -polar solvent after washing the oil
In some embodiments, the media treatment is omitted if with brine.
a lower quality of cannabis oil is desired . 3 . The process of claim 2, wherein the non - polar solvent
Temperatures that have been given to the nearest degree comprises hexane, heptane or pentane .
include all temperatures within a range of + 0 .5° C . of the 4 . The process of claim 2 , further comprising, after
given value . Temperatures that have been given to the 50 washing the oil with brine and before evaporating the
nearest 0 . 1° C . include all temperatures within a range of non - polar solvent, drying the oil with magnesium sulfate .
+ 0 . 05° C . of the given value . 5 . The process of claim 2 , wherein :
Other pore sizes of filter cartridges are used in other the brine is 60 - 100 % saturated with kosher sodium chlo
embodiments. ride ;
In other embodiments , the vacuum pressure of the rotovap 55 the step of washing with brine comprises agitating the
in non -polar solvent reclamation step 464 is different from non -polar solvent, oil and brine for 5 -30 minutes ; and
the range given above . the brine is removed by a centrifuge or gravity - fed
In some embodiments it is not necessary to completely separatory funnel.
remove the ethanol from the oil in ethanol reclamation step 6 . The process of claim 5 , wherein the ratio of non -polar
454. It has been found that residual ethanol in the oil will 60 solvent to oil to brine is 1: 1 : 2 by volume.
absorb into the aqueous brine phase during the brine wash 7 . The process of claim 2, wherein the heating step
ing step 460 . There is therefore no need for absolute removal comprises passing the brine -washed oil through a short-path
of ethanol from the crude oil . film wipe apparatus.
In some embodiments , non -polar solvents other than 8 . The process of claim 7 ,wherein the film wipe apparatus
hexane, heptane and pentane are used . 65 has:
In general, unless otherwise indicated , singular elements a feed temperature of 100 - 115º C .;
may be in the plural and vice versa with no loss of generality. a residue discharge arm temperature of 100 - 115º C .;
 US 10 , 406 , 453 B2
19 20
an inner wall surrounded by a jacket with a circulating 17 . The process of claim 1 , wherein the unwanted com
fluid at a temperature of 160 - 175° C .; and ponents are one or more of pigments , chlorophyll, fats ,
a condensing coil temperature of 0° C . to - 20° C . waxes, lipids , heavy metals and particulates.
9 . The process of claim 2, wherein the heating step 18 . The process of claim 1 , wherein the distilling step
comprises heating the brine -washed oil to 90 - 110° C . in a 5 comp
subjecting the decarboxylated oil to a first film wipe to
vacuum oven .
10. The process of claim 1, further comprising the steps remove volatile terpenes and leave a first residue;
of: subjecting the first residue to a second film wipe to
drying the raw cannabis plant material; and remove non -volatile terpenes and leave a second resi
grinding the raw cannabis plant material to result in the 10 due; and
dried and ground plant material. subjecting the second residue to a third film wipe to obtain
11 . The process of claim 10 , wherein the raw cannabis cannabinoids.
plant material is: 19 . The process of claim 18 , wherein :
dried to a moisture content of 5 % ; and the first and second film wipes are performed at a pressure
ground to an average particle size of 59000 um . 15 theofthird
0 .001film- 0 .01 mbar
wipe ; and
is performed at a pressure of 0 . 0008
12 . The process of claim 1 , wherein the centrifuging step
occurs in a wash and spin - dry separator and has a duration 0 .003 mbar.
of 8 - 15 minutes. 20 . The process of claim 18 , further comprising subject
13. The process of claim 1 , wherein : ing the cannabinoids to a further film wipe process to
the ethanol is at a temperature between - 60° C and 1go 20 separate the cannabinoids into cannabidiol and tetrahydro
C . when it is added to the dried and ground cannabis cannabinol .
21 . The process of claim 18 , wherein :
plant material; and the first film wipe is performed with :
the ethanol is added to the dried and ground cannabis a feed temperature of 100 - 115º C . ;
plant material in a ratio of 6 .6 - 10 liters of ethanol to 1 a residue discharge arm temperature of 100 - 115º C .;
kg of ground plant material. 25
an inner wall surrounded by a jacket with a circulating
14 . The process of claim 1, wherein treating the crude oil fluid at a temperature of 140 - 145º C .; and
and ethanol mixture comprises the steps of : a condensing coil temperature of 0° C . to - 20° C .;
adding the charcoal particles to the crude oil and ethanol the second film wipe is performed with :
mixture, agitating the charcoal particles and crude oil
and ethanol mixture , and filtering off the charcoal 30 a feed temperature of 100 - 115º C .;
particles; then a residue discharge arm temperature of 100 - 115º C .;
adding the bentonite clay particles to the crude oil and an inner wall surrounded by a jacket with a circulating
ethanol mixture , agitating the bentonite clay particles fluid at a temperature of 145 - 159° C .; and
and crude oil and ethanolmixture , and filtering off the a condensing coil temperature of 20 -60° C .; and
bentonite clay particles; and then adding the magne - 3535 the third film wipe is performed with :
a feed temperature of 100 - 115º C .;
sium oxide particles to the crude oil and ethanol
mixture, agitating the magnesium oxide particles and a residue discharge arm temperature of 100 -115º C .;
crude oil and ethanol mixture, and filtering off the an inner wall surrounded by a jacket with a circulating
magnesium oxide particles. fluid at a temperature of 140 - 165° C .; and
15 . The process of claim 14 , wherein : a condensing coil temperature of 68 - 73° C .
filtering off the charcoal particles comprises filtering the 22 . The process of claim 1, wherein the raw cannabis
charcoal particles and crude oil and ethanol mixture Sture p lant material is cannabis flower.
with a lenticular depth filtration apparatus; 23 . The process of claim 1 , wherein the raw cannabis
filtering off the bentonite clay particles comprises filtering plant
P material is cannabis leaves and stems.
the bentonite clay and crude oil and ethanol mixture 45 24 . The process of claim 1, wherein the step of distilling
with a lenticular depth filtration apparatus ; and is performed using a spinning band distillation apparatus .
filtering off the magnesium oxide particles comprises 25 . The process of claim 1, wherein the adding and
filtering the magnesium oxide particles and crude oil centrifuging steps are performed simultaneously .
and ethanol mixture with a lenticular depth filtration 26 . The process of claim 1 , further comprising leaving
apparatus . 50 residual ethanol in the oil after the evaporating step , wherein
16 . The process of claim 15 , wherein : the step of washing with brine removes the residual ethanol
the crude oil and ethanol mixture is at a temperature from the oil . 27 . The process ofclaim 1 ,wherein terpenes are obtained
between - 10° C . and + 85° C . when charcoal particles in the step of distilling.
are added ;
the charcoal particles are filtered off at a temperature 55 28 . The process of claim 18 , further comprising subject
between - 10° C . and 50° C .; and ing the cannabinoids to a spinning band fractional distilla
the bentonite clay particles and the magnesium oxide and process
tion to separate the cannabinoids into cannabidiol
tetrahydrocannabinol.
particles are filtered off at a temperature between 10° C .
and 50° C .