Note : Les descriptions sont présentées dans la langue officielle dans laquelle elles ont été soumises.
WO 2022/232905
PCT/CA2022/050624
INDUSTRIAL HASHISH AND METHOD FOR PRODUCING SAME AT AN INDUSTRIAL
SCALE
CROSS REFERENCE TO RELATED APPLICATION
[0001] The present application claims the benefit of U.S. provisional patent
applications serial
number 63/183,385, 63/185,210 and 63/278,916 filed respectively on May 3,
2021, May 6, 2021,
and November 12, 2021. The contents of the above-referenced documents are
incorporated
herein by reference in their entirety.
TECHNICAL FIELD
[0002] This application generally relates to the field of industrial hashish
products and methods
of manufacturing hashish products at an industrial scale.
BACKGROUND
[0003] Hashish (or hash) is a concentrated derivative of cannabis plants, the
dried resin glands
of the flowering tops of mature and unpollinated female cannabis plants. The
resin glands are
known as trichomes. It contains the same active ingredients as the cannabis
plants ¨ including
cannabinoids ¨ yet at higher concentration levels than the un-sifted buds or
leaves from which
dried marijuana is made, which is tantamount to higher potency.
[0004] The cannabis trichomes are substantially isolated from cannabis plant
matter. The
isolated cannabis trichomes are usually collected by hand, by mechanical
beating of the cannabis
plants or by submersing the cannabis plants in icy water and then using small
sieves to isolate
the cannabis trichomes. Alternatively, mechanical isolation may be used to
isolate cannabis
trichomes from cannabis plant matter, such as sieving through a screen by hand
(i.e., dry sift) or
in motorized tumblers, as described for example in WO 2019/161509. Isolated
cannabis
trichomes have a powder appearance (typically referred to as "kief") and are
pressed to obtain
blocks of hashish.
[0005] The production of hashish is very labor intensive, and it is
practically an art, where the
skills of the individual play a key role in defining the quality and/or
physical characteristics of the
finished hashish product. The consistency and appearance of hashish vary
depending on the
manufacturing process and amount of leftover plant material (e.g.,
chlorophyll). Consumers often
associate the hash color or smell to quality and/or origin.
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[0006] Good-quality pressed dry-sift hashish ranges in appearance from light
blondish-brown,
to greenish or dark-brown. Examples thereof include "Lebanese" hashish, which
is from yellow to
reddish, and "Moroccan" hashish which is from greenish to darker brown.
[0007] Hand-rubbed pressed hashish is most commonly referred to as being
"Afghani" (from
Afghanistan) or "Charas" (from India and Pakistan). This form of hashish is
produced by rubbing
the living plants to remove the sticky resin, which is then rolled into balls
or eggs and left to cure
before being consumed or sold_ Hand-rubbed types of hash should be smooth,
black or brownish-
black, and often sticky to the touch. When opened, consumers expect the
interior to be a delicate
brown, perhaps with a slight green tinge (a very green interior indicates
excessive residual plant
material).
[0008] Current industrial hashish production requires multiple steps and often
lack automation.
For example, it has been reported that some companies employ several
individuals to produce
hand-rubbed hashish, which is not easily scaled and very costly for commercial
production.
Industrial presses have been reported for producing pressed dry-sift hashish,
but difficulties in
matching the traditionally hand-made hashish products in terms of appearance,
malleability and
more specifically color and shininess, have rendered this approach less
appealable to the
industry. The current methods for manufacturing hash at an industrial scale
thus remain
unsatisfactory.
[0009] Considering the above, it would be highly desirable to be provided with
an industrial
hashish product and manufacturing method for making same that would at least
partially alleviate
the disadvantages of the existing technologies.
SUMMARY
[0010] This Summary is provided to introduce a selection of concepts in a
simplified form that are
further described below in the Detailed Description. This Summary is not
intended to identify key
aspects or essential aspects of the claimed subject matter.
[0011] The present inventors have developed a hashish that matches the
consumer appealing
hand-made products where the manufacturing method can be at least partially
automated and
which does not require use of coloring agents or post-processing steps to
artificially impart desired
visual characteristics that are typically associated with good quality
hashish.
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[0012] In a broad aspect, the present disclosure relates to a process of
making a hashish product,
comprising providing isolated cannabis trichomes; mixing the isolated cannabis
trichomes while
adding mechanical or thermal energy under conditions sufficient to obtain a
resinous mixture; and
retrieving at least a portion of the resinous mixture through an extrusion die
to obtain the hashish
product, wherein the hashish product is a substantially homogeneous cohesive
mass of the
isolated trichomes having a c/o reflectance of at least 4%85.
[0013] In specific embodiments, the process may include one or more of the
following features:
= the hashish product has a lightness value L* 50 on CI ELAB scale,
preferably from 0 to
about 40, or of from about 10 to about 30, or of from about 15 to about 25.
= the hashish product has a % reflectance of at least 4.5%85, at least
5%85, or at least
5.5%85.
= the mixing includes applying compression and shear forces to the isolated
trichomes via
a plurality of interpenetrate helicoidal surfaces within an elongated
enclosure.
= the interpenetrate helicoidal surfaces are on at least two screws
extending along at least
a portion of a longitudinal axis of the elongated enclosure.
= the process further comprising adjusting a rotational speed of the at
least two screws to
obtain the resinous mixture.
= the rotational speed of the at least two screws is between about 10 rpm
and about 1000
rpm, preferably between 100 rpm and 200 rpm.
= said elongated enclosure comprises a plurality of sections corresponding
to longitudinal
segments of the at least two screws.
= the process further comprising controlling a temperature in at least one
section of the
plurality of sections.
= the temperature in each section of the plurality of sections is
independently selected in the
range of from about 20 C to about 170 C.
= the plurality of sections includes at least one mixing section and at
least one conveying
section.
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= the at least one mixing section is maintained at a first temperature and
the least one
conveying section is maintained at a second temperature, the first and second
temperatures being
different.
= the plurality of sections includes at least one reverse flow section.
= at least a first section of the plurality of sections comprises a first
inlet for providing the
isolated trichomes.
= at least a second section of the plurality of sections comprises a second
inlet for providing
one or more additional component(s).
= the one or more additional component(s) include one or more cannabinoid,
one or more
terpene, one or more flavonoid, one or more flavoring agent, water, one or
more non-toxic coloring
agent, or a mixture thereof.
= the one or more cannabinoid(s) is in the form of a crude cannabis
extract, a cannabis
isolate, a cannabis distillate, a winterized cannabis plant extract, cannabis
rosin, cannabis resin,
cannabis wax, cannabis shatter, or any combination thereof.
= the one or more cannabinoid(s) includes a plurality of cannabinoids.
= the one or more cannabinoid(s) includes tetrahydrocannabinol (THC),
cannabidiol (CBD),
cannabinol (CBN), or any combinations thereof.
= the process further comprising cutting the hashish product according to a
pre-established
cutting operational parameter.
= the cutting pattern includes cutting the hashish product along a
transverse axis to obtain
pieces thereof of identical length and/or weight.
= the hashish product comprises a cannabinoid content of from about 5 wt.%
to about 90
wt.%.
= the isolated cannabis trichomes are from a single cannabis strain.
= the isolated cannabis trichomes are from a plurality of cannabis strains.
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= the hashish product comprises a moisture content of from about 2 wt.% to
about 8 wt.%,
or of from about 2 wt.% to about 5 wt.%.
= the isolated trichomes are dry-sift kief.
[0014] In a broad aspect, the present disclosure relates to a hashish product
comprising a
substantially homogeneous cohesive mass of isolated cannabis trichomes made by
the process
described above.
[0015] In a broad aspect, the present disclosure relates to a hashish product
comprising a
substantially homogeneous cohesive mass of isolated cannabis trichomes having
a % reflectance
of at least 4%85.
[0016] In specific embodiments, the hashish product may include one or more of
the following
features:
= the hashish product has a lightness value L* 50 on CI ELAB scale, or a
lightness value
L* from 0 to about 40, of from about 10 to about 30, of from about 15 to about
25.
= the hashish product has a % reflectance of at least 4.5%85, at least
5%85, or at least
5.5%85.
= comprising one or more additional component(s) selected from one or more
cannabinoid,
one or more terpene, one or more flavonoid, one or more flavoring agent, one
or more non-toxic
coloring agent, and any mixtures thereof.
= the one or more cannabinoid(s) is in the form of a crude cannabis
extract, a cannabis
isolate, a cannabis distillate, a winterized cannabis plant extract, cannabis
rosin, cannabis resin,
cannabis wax, cannabis shatter, or any combination thereof.
= the one or more cannabinoid(s) includes a plurality of cannabinoids.
= the one or more cannabinoid(s) includes tetrahydrocannabinol (THC),
cannabidiol (CBD),
cannabinol (CBN), or any combinations thereof.
= the hashish product comprises a cannabinoid content of from about 5 wt.%
to about 90
wt.%.
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= the isolated cannabis trichomes are from a single cannabis strain.
= the isolated cannabis trichomes are from a plurality of cannabis strains.
= the hashish product comprises a moisture content of from about 2 wt.% to
about 8 wt.%,
or of from about 2 wt.% to about 5 wt.%.
= the isolated trichomes are dry-sift kief.
[0017] In a broad aspect, the present disclosure relates to process of making
a hashish product,
comprising providing isolated cannabis trichomes; mixing the isolated cannabis
trichomes while
adding mechanical or thermal energy under conditions sufficient to obtain a
resinous mixture; and
retrieving at least a portion of the resinous mixture through an extrusion die
to obtain the hashish
product, wherein the hashish product has a moisture content of no more than
about 8 wt.%.
[0018] In another broad aspect, the present disclosure relates to a process of
making a hashish
product, comprising providing isolated cannabis trichomes; mixing the isolated
cannabis
trichomes while adding mechanical or thermal energy under conditions
sufficient to obtain a
resinous mixture; and retrieving at least a portion of the resinous mixture
through an extrusion die
to obtain the hashish product, wherein the hashish product is free of
exogenous water.
[0019] In specific embodiments, the processes described above may include one
or more of the
following features:
= the moisture content of the hashish product is less than 8 wt.%.
= the moisture content of the hashish product is less than 5 wt.%.
= the moisture content of the hashish product is at least 2 wt.%.
= the hashish product has a lightness value L* 50 on CI ELAB scale,
preferably from 0 to
about 40, or of from about 10 to about 30, or of from about 15 to about 25.
= the hashish product has a % reflectance of at least 4%85.
= the % reflectance of the hashish product is at least 4.5%85, at least
5%85, or at least
5.5%85.
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= the mixing includes applying compression and shear forces to the isolated
trichomes via
a plurality of interpenetrate helicoidal surfaces within an elongated
enclosure.
= the interpenetrate helicoidal surfaces are on at least two screws
extending along at least
a portion of a longitudinal axis of the elongated enclosure.
= the process further comprises adjusting a rotational speed of the at
least two screws to
obtain the resinous mixture.
= the rotational speed of the at least two screws is between about 10 rpm
and about 1000
rpm, preferably between 100 rpm and 200 rpm.
= the elongated enclosure comprises a plurality of sections corresponding
to longitudinal
segments of the at least two screws.
= the process further comprises controlling a temperature in at least one
section of the
plurality of sections.
= the temperature in each section of the plurality of sections is
independently selected in the
range of from about 20 C to about 170 C.
= the plurality of sections includes at least one mixing section and at
least one conveying
section.
= the at least one mixing section is maintained at a first temperature and
the least one
conveying section is maintained at a second temperature, the first and second
temperatures being
different.
= the plurality of sections includes at least one reverse flow section.
= at least a first section of the plurality of sections comprises a first
inlet for providing the
isolated trichomes.
= at least a second section of the plurality of sections comprises a second
inlet for providing
one or more additional component(s).
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= the one or more additional component(s) include one or more cannabinoid,
one or more
terpene, one or more flavonoid, one or more flavoring agent, one or more non-
toxic coloring agent,
or a mixture thereof.
= the one or more cannabinoid(s) is in the form of a crude cannabis
extract, a cannabis
isolate, a cannabis distillate, a winterized cannabis plant extract, cannabis
rosin, cannabis resin,
cannabis wax, cannabis shatter, or any combination thereof.
= the one or more cannabinoid(s) includes a plurality of cannabinoids.
= wherein the one or more cannabinoid(s) includes tetrahydrocannabinol
(THC), cannabidiol
(CBD), cannabinol (CBN), or any combinations thereof.
= the process further comprises cutting the hashish product according to a
pre-established
cutting operational parameter.
= the cutting pattern includes cutting the hashish product along a
transverse axis to obtain
pieces thereof of identical length and/or weight.
= the hashish product comprises a cannabinoid content of from about 5 wt.%
to about 90
wt.%.
= the isolated cannabis trichomes are from a single cannabis strain.
= the isolated cannabis trichomes are from a plurality of cannabis strains.
= the isolated trichomes are dry-sift kief.
= the hashish product is free of mold after a plurality of weeks.
[0020] In a broad aspect, the present disclosure relates to a hashish product
comprising a
substantially homogeneous cohesive mass of isolated cannabis trichomes made by
one of the
processes described above.
[0021] In a broad aspect, the present disclosure relates to a hashish product
comprising an
extruded, substantially homogeneous cohesive mass of isolated cannabis
trichomes having a
moisture content of no more than about 8 wt.%.
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[0022] In another broad aspect, the present disclosure relates to a hashish
product comprising
an extruded, substantially homogeneous cohesive mass of isolated cannabis
trichomes that is
free of exogenous water during extrusion.
[0023] In specific embodiments, the hashish products may include one or more
of the following
features:
= the moisture content of the hashish product is less than 8 wt.%.
= the moisture content of the hashish product is less than 5 wt.%.
= the moisture content of the hashish product is at least 2 wt.%.
= the hashish product has a lightness value L* 50 on CI ELAB scale,
preferably from 0 to
about 40, or of from about 10 to about 30, or of from about 15 to about 25.
= the hashish product has a % reflectance of at least 4%85.
= the % reflectance of the hashish product is at least 4.5%85, at least
5%85, or at least
5.5%85.
= the hashish product comprises one or more additional component(s)
selected from one or
more cannabinoid, one or more terpene, one or more flavonoid, one or more
flavoring agent, one
or more non-toxic coloring agent, and any mixtures thereof.
= the one or more cannabinoid(s) is in the form of a crude cannabis
extract, a cannabis
isolate, a cannabis distillate, a winterized cannabis plant extract, cannabis
rosin, cannabis resin,
cannabis wax, cannabis shatter, or any combination thereof.
= the one or more cannabinoid(s) includes a plurality of cannabinoids.
= the one or more cannabinoid(s) includes tetrahydrocannabinol (THC),
cannabidiol (CBD),
cannabinol (CBN), or any combinations thereof.
= the hashish product comprises a cannabinoid content of from about 5 wt.%
to about 90
wt.%.
= the isolated cannabis trichomes are from a single cannabis strain.
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= the isolated cannabis trichomes are from a plurality of cannabis strains.
= the isolated trichomes are dry-sift kief.
[0024] All features of exemplary embodiments which are described in this
disclosure and are not
mutually exclusive can be combined with one another. Elements of one
embodiment can be
utilized in the other embodiments without further mention. Other aspects and
features of the
present invention will become apparent to those ordinarily skilled in the art
upon review of the
following description of specific embodiments.
BRIEF DESCRIPTION OF THE DRAWINGS
[0025] The patent or application file contains at least one drawing executed
in color. Copies of
this patent or patent application publication with color drawing(s) will be
provided by the Office
upon request and payment of the necessary fee.
[0026] A detailed description of specific exemplary embodiments is provided
herein below with
reference to the accompanying drawings in which:
[0027] FIG. 1 illustrates a non-limiting flowchart example of a process for
making a hashish
product in accordance with an embodiment of the present disclosure;
[0028] FIG. 2 illustrates a non-limiting flowchart example of steps for
obtaining isolated cannabis
trichomes in accordance with an embodiment of the present disclosure;
[0029] FIG. 3 illustrates a non-limiting flowchart example of a process for
working the resinous
mixture from FIG 1 in accordance with an embodiment of the present disclosure;
[0030] FIG. 4 illustrates a non-limiting system implementing a process for
making a hashish
product in accordance with an embodiment of the present disclosure;
[0031] FIG. 5 illustrates a non-limiting schematic of a setting for performing
a gloss and
reflectance measurement;
[0032] FIG. 6A-6E are images of hashish product samples manufactured in
accordance with
Examples described herein;
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[0033] FIG. 7A is a comparative image comparing hashish product samples
manufactured with
a single-screw extruder (I) and a double-screw extruder (II); and
[0034] FIG. 7B is a comparative image comparing hashish product samples
manufactured with
pressing (I), single-screw extruder (II), and double-screw extruder (III).
[0035] In the drawings, exemplary embodiments are illustrated by way of
example. It is to be
expressly understood that the description and drawings are only for the
purpose of illustrating
certain embodiments and are an aid for understanding. They are not intended to
be a definition
of the limits of the invention.
DETAILED DESCRIPTION
[0036] A detailed description of one or more embodiments is provided below
along with
accompanying figures that illustrate principles of the disclosure. The
invention is described in
connection with such embodiments, but the invention is not limited to any
embodiment. The scope
of the invention is limited only by the claims. Numerous specific details are
set forth in the following
description to provide a thorough understanding of the invention. These
details are provided for
the purpose of non-limiting examples and the invention may be practiced
according to the claims
without some or all these specific details. Technical material that is known
in the technical fields
related to the invention has not been described in detail so that the
disclosure is not unnecessarily
obscured.
[0037] The present inventors have developed a hashish product and industrial
method of
manufacturing same that addresses at least some of the above-identified
problems.
[0038] For example, it has been observed that the hashish product according to
the present
disclosure has a visual appearance that substantially matches the consumer
appealing hand-
made products without systematic use of exogenous ingredients (such as
coloring agents, oils,
etc.) and/or additional post-manufacturing processing performed by the
manufacturer or user to
artificially impart such visual appearance. For example, the industrial hash
of the present
disclosure can be characterized with dark color and shiny appearance, as would
be expected
from a hand-rubbed hashish, or bubble hashish, or hash made with high potency
kief.
[0039] The present inventors have developed an industrial manufacturing
process to produce
such hash product that includes mixing isolated cannabis trichomes under
specific conditions that
are sufficient to obtain a resinous mixture which upon retrieval through an
extrusion die affords a
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hashish product having the desired appearance. In other words, the process
allows to have a
shiny hash straight out of the die, without requiring further processing
(e.g., rolling up as a ball,
adding exogenous ingredients such as oils, etc.). Further, and in contrast to
previous processes
developed by the Applicant, it was surprisingly and unexpectedly discovered
here that
incorporating water into the kief was not necessary to produce hashish product
having the
desirable characteristics. This was surprising in view of specific pressing
embodiments described
in PCT Application Publication W02021/119817, filed on December 16, 2020, and
specific mixing
embodiments described in PCT Application Publication W02021/226725, filed on
May 17, 2021,
which both incorporated water into kief to impart desirable characteristics to
the resulting hash
product
[0040] Such difference also afforded a technical effect in that the resulting
hash product can
also be characterized as having a low moisture content, which can reduce or
avoid likelihood of
mold growth over time, thus affording advantageous extended shelf life to the
hashish product
compared to other industrial hashish with higher moisture content.
[0041] Such extended shelf life, observed with the hash of the present
disclosure may also
afford a technical effect in that this may avoid or minimize the need for
irradiation (e.g., electron
beams, x-rays or gamma rays). While irradiation is commonly used on food
products to eliminate
microorganism and thus extend shelf life, using irradiation on hashish
products may be
problematic for a number of reasons. For example, irradiation can be costly
and time-consuming,
especially multiple steps/doses of irradiation are implemented and/or if
irradiation treatments are
performed at an offsite location, which adds logistics to the overall costs.
[0042] These and other advantages may become apparent to the person of skill
in view of the
present disclosure.
Hashish Product
[0043] The hashish product of the present disclosure comprises a cohesive mass
of isolated
cannabis trichomes.
[0044] For example, the cohesive mass may be a substantially homogeneous
cohesive mass
of isolated trichomes. By "substantially homogeneous", it is meant that the
hashish product has a
constant or uniform distribution of isolated trichomes throughout its cohesive
mass. In other
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words, the manufacturing procedures described herein, process the isolated
trichomes in such
fashion to result in mixing thereof into a substantially constant, uniform
cohesive mass.
[0045] As used herein, the term "cannabis trichomes" generally refers to
crystal-shaped
outgrowths or appendages (also called resin glands) on cannabis plants
typically covering the
leaves and buds. Trichomes produce hundreds of known cannabinoids, terpenes,
and flavonoids
that make cannabis strains potent, unique, and effective.
[0046] As used herein, the term "isolated cannabis trichomes" refers to
trichomes that have
been separated from cannabis plant material using any method known in the art.
The details of
various methods for separating trichomes from the cannabis plant are well-
known in the art. For
example, and without wishing to be limiting in any manner, the isolated
cannabis trichomes may
be obtained by manual processes like dry sifting or by water extraction
methods. Solvent-less
extraction methods can include mechanical separation of trichomes from the
plant, such as
sieving through a screen by hand or in motorized tumblers (see for example WO
2019/161509),
or by submerging the cannabis plants in icy water (see for example
US2020/0261824, which is
herein incorporated by reference) and agitating to separate the trichomes from
the plant and
drying the trichomes. Because of inherent limitations to existing separation
methods, some plant
matter or other foreign matter can be present in isolated cannabis trichomes.
[0047] Isolated cannabis trichomes obtained by mechanical separation of
trichomes from the
cannabis plant biomass is typically referred to as "kief' (also "keef" or
"kir) and has a powdery
appearance. Typically, some residual plant material remains in the finished
kief and thus in the
resulting hashish product. In some embodiments, the isolated trichomes are dry-
sift kief.
[0048] The isolated cannabis trichomes forming the hashish product of the
present disclosure
may originate from one or more than one strain of cannabis plant. It is known
amongst consumers
of hashish and other cannabis products that using isolated cannabis trichomes
produced from
more than one strain of cannabis plant allows a user to tune the psychoactive
and/or entourage
effect obtained by consuming the product. The mixing of cannabis plant strains
may also allow to
adjust the final concentration of a component of the product, for example but
not limited to the
cannabinoid content. Additionally, use of more than one strain allows for
improved product and
waste management ¨ important in commercial production.
[0049] As used herein, the term "cannabis" generally refers to a genus of
flowering plants that
includes several species. The number of species is currently being disputed.
There are three
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different species that have been recognized, namely Cannabis sativa, Cannabis
indica and
Cannabis ruderalis. Hemp, or industrial hemp, is a strain of the Cannabis
sativa plant species that
is grown specifically for the industrial uses of its derived products. In
terms of cannabinoids
content, hemp has lower concentrations of tetrahydrocannabinol (THC) and
higher concentrations
of cannabidiol (CBD), which decreases or eliminates the THC-associated
psychoactive effects.
[0050] In some embodiments, the hashish product of the present disclosure is
characterized as
having a desirable dark color, such as having a lightness value L* 50 on CI
ELAB scale.
[0051] The person of skill will readily understand that assessing and/or
measuring the color can
be performed quantitatively using a colorimeter, a spectrophotometer, or
qualitatively with the
human eye. For example, for quantitative assessment / measurement, the color
can be measured
by reflectance spectrophotometer ASTM standard test methodology. Tristimulus
L*, a*, b* values
are measured from the viewing surface of the hashish product. These L*, a*, b*
values are
reported in terms of the CIE 1976 color coordinate standard (CI ELAB scale).
L* is lightness which
is the relative brightness of a surface with a range from 0-100, wherein L*=0
translates as darkest
black and L*=100 translates as lightest white.
[0052] In some embodiments, the hashish product of the present disclosure has
a lightness
value L* 50 based on the CIELAB scale ¨ e.g., the reader will readily
recognize that such
lightness value range leaves flexibility to the producer, as the product can
be made darker through
other means if desirable to favor consumer appeal.
[0053] For example, the hashish product may have a lightness value L* from 0
to about 50 or
any value therebetween, or in a range of values defined by any values
therebetween. For
example, the hashish product may have a lightness value L* up to about 50, up
to about 45, up
to about 40, up to about 35, up to about 30, up to about 25, up to about 20,
up to about 15, up to
about 10, up to about 5 or any value therebetween. For example, the hashish
product may have
a lightness value L* of from about 5 to about 45, of from about 10 to about
40, from about 15 to
about 35, from about 20 to about 30. For example, the hashish product may have
a lightness
value L* of about 5, of about 10, of about 15, of about 20, of about 25, of
about 30, of about 35,
of about 40, of about 45, or about 50.
[0054] In some embodiments, the hashish product of the present disclosure is
characterized as
having a desirable shininess, such as having a % reflectance of at least about
5%85.
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[0055] The person of skill will readily understand that reflectance is the
proportional amount of
reflected light measured from a sample surface, relative to the amount of
reflected light measured
from a reference plate and can thus serve to characterize the shininess of a
hashish product.
[0056] %Reflectance can be determined in several ways all of which are known
to the person
skilled in the art. For example, %Reflectance could be determined by a
glossmeter which initially
determines shininess in terms of gloss by directing a constant intensity light
beam, at a fixed angle
Y, on to the test surface and monitoring the amount of reflected light from
the same angle. The
determined gloss value (also known as Gloss Unit or GU) is in turn translated
to %reflectance.
Whilst the Gloss Unit (GU) scale is linear, each angle of incidence has a
different gloss
measurement range; 0 ¨ 2000 GU (for 20 ), 0 ¨ 1000 GU (for 60 ) and 0 ¨ 160 GU
(for 85 ).
%Reflectance compares the amount of light energy transmitted and received by a
glossmeter and
expresses the value as a percentage of the angle of incident's full
measurement range and the
value is displayed as a percentage relative to the selected angle of
incidence. For example, as
the measurement range for a 20 glossmeter is 0-2000 GU; a value of 1000 GU at
200 would be
expressed in terms of %reflectance as 50%20, and a value of 500 GU would be
expressed as
25%20. However, A value of 500 GU at 60 , but would be expressed as 50%60 as
the
measurement range for the 60 is 0 ¨ 1000 GU.
[0057] In one practical example gloss can be determined with the ElcometerTM
480 Model T
glossmeter with integrated ElcoMasterTm software (Elcometer, USA). In order to
determine the
most appropriate measurement angle start with a gloss meter set at 60 degrees
angle of
incidence. If the result is between 10-70GU, the coating is termed 'semi-
gloss' and should be
measured using the 60 degrees angle. If the result is less than 10G U, the
product is low gloss'
and should be measured using the 85 degrees angle and if it is greater than
70GU, the product
is known as 'high gloss' and should be measured using the 20 degrees angle.
[0058] In some embodiments, the hashish product according to the present
disclosure has a
gloss value of at least 6 GU, at least 7 GU, at least 8 GU, or even greater
(e.g., at least 9 GU, at
least 10 GU, or more).
[0059] For instance, in some embodiments, the hashish product according to the
present
disclosure has a %reflectance of at least 4%85, at least 4.5%85, at least
5%85, at least 5.5%85,
or even greater (e.g., at least 6%85, at least 7%85, or more).
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[0060] Without being bound by any theory, it is believed that hashish
shininess may depend on
several factors, for example, the potency of the base materials, i.e., for
example water and ice
isolation of kief has been reported to isolate kief of higher potency and
higher purity, thus higher
amounts of resin content capable of being oozed out which can favor obtaining
shinier hash; the
processing parameters to obtain the hash can affect the level of how much
resin can be extracted
from the trichomes, for example hand rubbing the hash may impart more
mechanical / thermal
energy to the kief thus extracting more resin therefrom compared to simply
pressing the kief in an
industrial press; post processing steps performed by the manufacturer and/or
users, such as
rolling the hashish product into a ball which has been reported to enhance the
shiny aspect of
hashish product that have sufficient resin content to expose at the outer
surface of the hashish
product; and the like. A common trait being that higher potency / higher resin
content correlates
with better cohesion and smoothness as well as desired color and/or shininess.
It was thus
surprising to the inventors to be able to obtain hash with such desirable
shininess without recourse
to such procedures known to favor shininess. For example, the present
inventors were able to
obtain hand-rubbed hash shininess levels using dry-sift kief with an extruder
device, where dry-
sift kief is known to produce less shiny hash.
[0061] While the manufacturing process described herein does not require
incorporating water
into kief, thus resulting in a hashish product having low moisture content ¨
the resulting hash
product can include a residual moisture content, which can originate for
example from
endogenous water present in the kief or other liquids, such as terpenes. In
some embodiments,
the hashish product of the present disclosure can comprise a moisture content
of no more than
about 8 wt.% (e.g., less than 8 wt.%), such as from about 2 wt.% to about 8
wt.% or any value
therebetween, or in a range of values defined by any values therebetween. For
example, the
hashish product may have a moisture content of up to about 8 wt %, of up to
about 7 wt.%, of up
to about 6 wt.%, of up to about 5 wt.%, of up to about 4 wt.%, of up to about
3 wt.%, or of up to
about 2.5 wt.% or any value therebetween. For example, the hashish product may
have a
moisture content of from about 2.5 wt.% to about 4.5 wt.%, from about 2.8 wt.%
to about 4.2 wt.%,
from about 3.0 wt.% to about 4.0 wt.%, from about 3.2 wt.% to about 3.8 wt.%,
or from about 3.4
wt.% to about 3.6 wt.%.
[0062] In specific implementations, the present inventors measured an about
2.5 wt.% drop in
moisture from processing the kief through the mixing process described herein
to obtain a hash
product having the desired characteristics (e.g., dark black, shiny, and
malleable). For example,
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in a specific embodiment, the present inventors obtained a hash product having
moisture content
of 3-5 wt.% using a dry-sift kief having an initial moisture content of 7.4
wt.%.
[0063] In some embodiments, water can be added into the process depending on
specific
applications. For example, water could be added to help more efficiently
conduct thermal energy
to the product and/or help form cohesive forces leading to a more malleable
and soft texture. For
example, water could be added in the form of liquid water, steam, or ice. For
example, the water
being added can be water purified using any known process, such as capacitive
deionization,
reverse osmosis, carbon filtering, microfiltration, ultrafiltration,
ultraviolet oxidation,
electrodeionization, distillation, and the like.
[0064] The moisture content of the hashish product can be determined by
several methods
known to the person skilled in the art including but not limited to
Thermogravimetry Analysis (TGA)
and equipment such as Mettler ToledoTm Hal. Moisture Analyzer HC103 (Fisher
Scientific, USA)
or MA160 Thermogravimetric Moisture Balance-type Analyzer (Sartorius Canada
Inc).
Cannabinoid content
[0065] The hashish product of the present disclosure comprises one or more
cannabinoid(s).
The one or more cannabinoid(s) may be present endogenously in the isolated
trichomes used to
make the hash product or may be added in the form of an additional component
(as described
later in this text).
[0066] As used herein, the term "cannabinoid" generally refers to any chemical
compound that
acts upon a cannabinoid receptor such as CBI and CB2. Examples of cannabinoids
include, but
are not limited to, cannabichromanon (CBCN), cannabichromene (CBC),
cannabichromevarin
(CBCV), cannabicitran (CBT), cannabicyclol (CBL), cannabicyclovarin (CBLV),
cannabidiol (CBD,
defined below), cannabidiolic acid (CBDA), cannabidiol monomethylether (CBDM),
cannabidiol-
C4 (CBD-C4), cannabidiorcol (CBD-C1), cannabidiphorol (CBDP), cannabidivarin
(CBDV),
cannabielsoin (CBE), cannabifuran (CBF), cannabigerol (CBG), cannabigerol
monomethylether
(CBGM), cannabigerolic acid (CBGA), cannabigerovarin (CBGV), cannabinodiol
(CBND),
cannabinodivarin (CBVD), cannabinol (CBN), cannabinol methylether (CBNM),
cannabinol propyl
variant (CBNV), cannabinol-C2 (CBN-02), cannabinol-04 (CBN-C4), cannabiorcol
(CBN-C1),
cannabiripsol (CBR), cannabitriol (CB0), cannabitriolvarin (CBTV),
cannabivarin (CBV),
dehydrocannabifuran (DCBF), A7-cis-iso tetrahydrocannabivarin,
tetrahydrocannabinol (THC,
defined below), A9-tetrahydrocannabionolic acid B (THCA-B), A9-
tetrahydrocannabinolic acid A
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(THCA-A), A9-tetrahydrocannabiorcol (THC-C1), tetrahydrocannabivarinic acid
(THCVA),
tetrahydrocannabivarin (THCV), ethoxy-
cannabitriolvarin (CBTVE), trihydroxy-A9-
tetrahydrocannabinol (tri0H-THC), 10-ethoxy-9hydroxy-A6a-tetrahydrocannabinol,
8,9-
dihyd roxy-A6a-tetrahydrocannabinol, 10-oxo-A6a-tetrahydrocannabionol (OTHC),
3,4,5,6-
tetrahydro-7-hydroxy-a-a-2-trimethy1-9-n-propy1-2,
6-methano-2H-1-benzoxocin-5-methanol
(OH-iso-HHCV), A6a,10a-tetrahydrocannabinol (A6a,10a-THC), A8-
tetrahydrocannabivarin (A8-
THCV), A9-tetrahydrocannabiphorol (69-THCP), A9-tetrahydrocannabutol (A9-
THCB),
derivatives of any thereof, and combinations thereof. Further examples of
suitable cannabinoids
are discussed in at least W02017/190249 and U.S. Patent Application Pub. No.
US2014/0271940, which are each incorporated by reference herein in their
entirety.
[0067] Cannabidiol (CBD) means one or more of the following compounds: A2-
cannabidiol, A5-
cannabidiol (2-(6-isopropeny1-3-methyl-5-cyclohexen-l-y1)-5-pentyl-
1,3-benzenediol); .. A4-
cannabidiol (2-(6-isopropeny1-3-methyl-4-cyclohexen-l-y1)-5-pentyl-
1,3-benzenediol); A3-
cannabidiol
(2-(6-isopropeny1-3-methy1-3-cyclohexen-l-y1)-5-pentyl-1,3-benzenediol);
A3,7-
cannabidiol
(2-(6-isopropeny1-3-methylenecyclohex-1-y1)-5-penty1-1,3-benzenediol); A2-
cannabidiol (2-(6-isopropeny1-3-methyl-2-cyclohexen-l-y1)-5-pentyl-
1,3-benzenediol); A1-
cannabidiol (2-(6-isopropeny1-3-methyl-l-cyclohexen-l-y1)-5-penty1-1,3-
benzenediol); and A6-
cannabidiol (2-(6-isopropeny1-3-methyl-6-cyclohexen-l-y1)-5-pentyl-1,3-
benzenediol). In a
preferred embodiment, and unless otherwise stated, CBD means A2-cannabidiol.
[0068] Tetrahydrocannabinol (THC) means one or more of the following
compounds: A8-
tetrahydrocannabinol (A8-THC), A8-
tetrahydrocannabivarin (A8-THCV), A9-cis-
tetrahydrocannabinol (cis-THC), A9-tetrahydrocannabinol (A9-THC), A10-
tetrahydrocannabinol
(A10-THC), A9-tetrahydrocannabinol-C4 (THC-C4), A9-tetrahydrocannabinolic acid-
C4 (THCA-
C4), synhexyl (n-hexyl-A3THC). In a preferred embodiment, and unless otherwise
stated, THC
means one or more of the following compounds: A9-tetrahydrocannabinol and A8-
tetrahydrocannabinol.
[0069] In one embodiment, the hashish product of the present disclosure
contains the one or
more cannabinoid(s) in an amount sufficient for the user to experience a
desired effect when
consuming the product. For example, the hashish product may comprise from
about 5 wt.% to
about 90 wt.% cannabinoid or any value therebetween, or in a range of values
defined by any
values therebetween. For example, the hashish product may comprise up to about
90 wt.%, up
to about 80 wt.%, up to about 70 wt.%, up to about 60 wt.%, or up to about 50
wt.%, or up to
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about 40 wt.%, or up to about 30 wt.% or any value therebetween, or in a range
of values defined
by the aforementioned values. For example, the hashish product may comprise
from about 10
wt.% to about 60 wt.%, more preferably from about 20 wt.% to about 50 wt.%. In
another
embodiment, the hashish product may include up to 1000 mg/g THC, depending on
specific
implementations of the present disclosure.
[0070] In some embodiments, alternatively or additionally, the hashish product
of the present
disclosure may include one or more cannabinoid, such as THC, CBD, CBG, CBN, or
any
combinations thereof. For example, the THC can be delta-9-THC and/or delta-8-
THC. The
cannabinoids can be in similar or different amounts, depending on specific
implementations of
the present disclosure.
[0071] A cannabinoid may be in an acid form or a non-acid form, the latter
also being referred
to as the decarboxylated form since the non-acid form can be generated by
decarboxylating the
acid form.
[0072] The content in the acid form and the decarboxylated form of a specific
cannabinoid can
be determined using suitable methods known to the person skilled in the art,
such as but not
limited to Gas Chromatography/ Mass Spectrometry (GC/MS), High Performance
Liquid
Chromatography (HPLC), Gas Chromatography/ Flame Ionization Detection
(GC/FID), Fourier
transform infrared (FT-IR) spectroscopy, and the like. Various suitable
methods are described,
for example, in Formato et al. (¨)-Cannabidiolic Acid, a Still Overlooked
Bioactive Compound: An
Introductory Review and Preliminary Research. Molecules. 2020 Jun
5;25(11):2638.
Additional components
[0073] The hashish product according to the present disclosure may also
comprise one or more
additional components.
[0074] In some embodiments, the one or more additional components may be added
to alter
the characteristics of the hashish product, such as cannabinoid content,
potency, entourage
effect, odor, color, shine, consistency, texture, malleability, and the like.
[0075] In some embodiments, the one or more additional components may be
substantially
homogeneously distributed on at least a portion of a surface of the hashish
product, for example
as a coating, and/or the one or more additional components may be
substantially homogeneously
distributed throughout the cohesive mass forming the hash product. For
example, the portion of
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the surface of the hashish product may include at least 20%, at least 30%, at
least 40%, at least
50%, at least 60%, at least 70%, at least 80%, at least 90%, or 100% of the
surface of the hashish
product.
[0076] The one or more additional component may be any suitable food grade
and/or non-toxic
composition or component known in the art. As will be recognized by those of
skill in the art, the
toxicity of each type of additional component may be dependent on the method
of consumption
of the hashish product. For example, in applications where smoke! vapor
produced by the hashish
product is to be inhaled, suitable additional components may include, but are
not limited to one
or more cannabinoid, one or more terpene (also referred to herein as a
"terpene blend"), water,
one or more flavonoid, or any combination thereof.
[0077] The one or more additional component may be a cannabinoid. The
cannabinoid may be
extracted from any suitable source material including, but not limited to,
cannabis or hemp plant
material (e.g., flowers, seeds, and trichomes) or may be manufactured
artificially (for example
cannabinoids produced in yeast, as described in WO W02018/148848).
Cannabinoids can be
extracted from a cannabis or hemp plant material according to any procedure
known in the art.
For example, and without wishing to be limiting, a "crude extract" containing
a cannabinoid may
be obtained by extraction from plant materials using for example aliphatic
hydrocarbons (such as
propane, butane), alcohols (such as ethanol), petroleum ether, naphtha, olive
oil, carbon dioxide
(including supercritical and subcritical CO2), chloroform, or any combinations
thereof. Optionally,
the crude extract may then be "winterized", that is, extracted with an organic
solvent (such as
ethanol) to remove lipids and waxes (to produce a "winterized extract"), as
described for example
in US 7,700,368, US 2004/0049059, and US 2008/0167483, which are each herein
incorporated
by reference in their entirety. Optionally, the method for obtaining the
cannabinoid may further
include purification steps such as a distillation step to further purify,
isolate or crystallize one or
more cannabinoids, which is referred to in the art and herein as a
"distillate"; US20160346339,
which is incorporated herein by reference, describes a process for extracting
cannabinoids from
cannabis plant material using solvent extraction followed by filtration, and
evaporation of the
solvent in a distiller to obtain a distillate. The distillate may be cut with
one or more terpenes. The
crude extract, the winterized extract or the distillate may be further
purified, for example using
chromatographic and other separation methods known in the art, to obtain an
"isolate".
Cannabinoid extracts may also be obtained using solvent-less extraction
methods; for example,
cannabis plant material may be subjected to heat and pressure to extract a
resinous sap ("rosin")
containing cannabinoids; methods for obtaining rosin are well-known in the
art.
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[0078] The one or more additional component may thus include one or more
cannabinoid in the
form of a crude cannabis extract, a cannabis distillate, a cannabis isolate, a
winterized cannabis
plant extract, cannabis rosin, cannabis resin, cannabis wax, cannabis shatter,
or any combination
thereof.
[0079] The one or more additional component may be a terpene. As used herein,
the term
"terpene" generally refers to a class of chemical components comprised of the
fundamental
building block of isoprene, which can be linked to form linear structures or
rings. Terpenes may
include hemiterpenes (single isoprenoid unit), monoterpenes (two units),
sesquiterpenes (three
units), diterpenes (four units), sesterterpenes (five units), triterpenes (six
units), and so on. At
least some terpenes are expected to interact with, and potentiate the activity
of, cannabinoids.
Any suitable terpene may be used in the hashish product of the present
invention. For example,
terpenes originating from cannabis plant may be used, including but not
limited to
aromadendrene, bergamottin, bergamotol, bisabolene, borneol, 4-3-carene,
caryophyllene,
cineole/eucalyptol, p-cymene, dihydroj asmone, elemene, farnesene, fenchol,
geranylacetate,
guaiol, humulene, isopulegol, limonene, linalool, menthone, menthol,
nnenthofuran, myrcene,
nerylacetate, neomenthylacetate, ocimene, perillylalcohol, phellandrene,
pinene, pulegone,
sabinene, terpinene, terpineol, 4-terpineol, terpinolene, and derivatives
thereof. Additional
examples of terpenes include nerolidol, phytol, geraniol, alpha-bisabolol,
thymol, genipin,
astragaloside, asiaticoside, camphene, beta-amyrin, thujone, citronellol, 1,8-
cineole, cycloartenol,
hashishene, and derivatives thereof. Further examples of terpenes are
discussed in US Patent
Application Pub. No. US2016/0250270, which is herein incorporated by reference
in its entirety
for all purposes. The hashish product of the present disclosure may contain
one or more
terpene(s). The one or more terpene(s) may originate from the hashish, from an
additional
component, or both. In some embodiments, the hashish product of the present
disclosure may
include the one or more terpene(s) in an amount (the "terpene content")
sufficient for the user to
experience a desired entourage effect when consuming the product. For example,
the hashish
product may comprise from about 0.5 wt.% to about 15 wt.% terpene, for example
up to about 15
wt.%, or up to about 10 wt.%, or up to about 5 wt.%, or up to about 4 wt.%, or
up to about 3 wt.%,
or up to about 2 wt.%, or up to about 1 wt.%. For example, the one or more
terpene(s) may include
hashishene. Without wishing to be bound by theory, hashishene is believed to
be a terpene
produced by rearrangement of myrcene that may be found in hashish after
mechanical
processing, and that may be responsible for the typical desirable "hashish
flavour".
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[0080] The one or more additional component may be a flavonoid. The term
"flavonoid" as used
herein refers to a group of phytonutrients comprising a polyphenolic
structure. Flavonoids are
found in diverse types of plants and are responsible for a wide range of
functions, including
imparting pigment to petals, leaves, and fruit. Any suitable flavonoid may be
used in the hashish
product of the present invention. For example, flavonoids originating from a
cannabis plant may
be used, including but not limited to: apigenin, cannflavin A, cannflavin B,
cannflavin C, chrysoeril,
cosmosiin, flavocannabiside, homoorientin, kaempferol, luteolin, myricetin,
orientin, quercetin,
vitexin, and isovitexin.
[0081] The reader will readily understand that in some implementations, the
one or more
additional component may include a combination of any one of the one or more
additional
component described herein.
Consumer use of hashish products
[0082] As is known in the art, hashish is typically used for recreational or
medicinal uses. For
example, hashish products can be used to achieve a desired effect in a user,
such as a
psychoactive effect, a physiological effect, or a treatment of a condition. By
"psychoactive effect",
it is meant a substantial effect on mood, perception, consciousness,
cognition, or behavior of a
subject resulting from changes in the normal functioning of the nervous
system. By "physiological
effect", it is meant an effect associated with a feeling of physical and/or
emotional satisfaction. By
"treatment of a condition", it is meant the treatment or alleviation of a
disease or condition by
absorption of cannabinoid(s) at sufficient amounts to mediate the therapeutic
effects.
[0083] The terms "treating", "treatment" and the like are used herein to mean
obtaining a desired
pharmacologic and/or physiologic effect. The effect may be prophylactic, in
terms of completely
or partially preventing a disease, condition, or symptoms thereof, and/or may
be therapeutic in
terms of a partial or complete cure for a disease or condition and/or adverse
effect, such as a
symptom, attributable to the disease or disorder. "Treatment" as used herein
covers any treatment
of a disease or condition of a mammal, such as a dog, cat or human, preferably
a human.
[0084] In certain embodiments, the disease or condition is selected from the
group consisting
of pain, anxiety, an inflammatory disorder, a neurological disorder, a
psychiatric disorder, a
malignancy, an immune disorder, a metabolic disorder, a nutritional
deficiency, an infectious
disease, a gastrointestinal disorder, and a cardiovascular disorder.
Preferably the disease or
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condition is pain. In other embodiments, the disease or condition is
associated with the feeling of
physical and/or emotional satisfaction.
[0085] In the context of recreational use, the "effective amount" administered
and rate and time-
course of administration, will depend on the desired effect associated with a
feeling of physical
and/or emotional satisfaction in the subject.
[0086] In the context of health and wellness use, the "effective amount"
administered, and rate
and time-course of administration will depend on the nature and severity of
the disease or
condition being treated and typically also takes into consideration the
condition of the individual
subject, the method of administration and the like.
Manufacturina process
[0087] The hashish product may be produced by mixing the components thoroughly
to provide
a resinous mixture having desired characteristics.
[0088] For example, the mixing may be performed by mechanically mixing. By the
term
"mechanically mixing" or "mechanical mixing", it is meant mixing using any
suitable mechanical
means. The mechanical means may be, for example, a plurality of interpenetrate
helicoidal
surfaces within an elongated enclosure or barrel, a non-limiting example of
which is an extruder
apparatus.
[0089] An extruder apparatus is a machine used to perform an extrusion
process. Manufacturing
by extrusion occurs when a material (usually pellets, dry powder, rubber,
plastic, metal bar stock
or food) is heated and pushed through a die assembly. A die is a mold that
shapes the heated
material as it is forced through a small opening from the inside of the
extruder to the outside.
Using a system of barrels or cylinders containing interpenetrate helicoidal
surfaces, e.g., screw
pumps or extruder screws, the extruder can mix the ingredients, and optionally
adding heating,
while propelling the extrudate through the die, for example to impart a
desired shape to the
hashish product. Extruders use in the industry are often of single-screw or
twin-screw type.
[0090] Twin-screw extruders are known in the art - screws of such extruders
may be parallel or
non-parallel, converging or non-converging, with or without differential
speed, counter or non-
counter rotating as described for example in US 6,609,819, WO 2020/220390, WO
2020/220495
and US 2010/0143523, where each of which is herein incorporated by reference
in its entirety. It
will be readily appreciated that extruders have flexible configuration (in
terms of mixing zones,
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temperature zones, input zones, etc.) and that any suitable configuration of
an extruder apparatus
capable of producing a hashish product may be used within the context of the
present disclosure.
[0091] A twin-screw extruder can be configured to have one or more mixing
zones, one or more
conveying zones, or one or more compression zones. Each of the zones may have
input ports
used for introduction of material. The mixing zones apply shear forces to the
input materials,
blending until they are homogenized. The extruder die assembly may perform a
variety of
functions: it may form or shape the extrudate, it may divide the extrudate
into multiple extrudates,
it may inject one or more component into the extrudate, and it may compress
and reduce the
cross-sectional area of the extrudate. It will be readily appreciated that
extruders have flexible
configuration (in terms of mixing zones, conveying zones, compression zones,
etc.) and that any
suitable configuration of an extruder apparatus (with any axial temperature
profile or with any
number of input ports) capable of producing a hashish product may be used
within the context of
the present disclosure.
[0092] As discussed later in this text, double screw extruders tested herein
were more efficient
than single screw extruders or industrial presses to impart the desired
characteristics to the
hashish in absence of water addition to the kief. Without being bound by any
theory, it is believed
that water addition when pressing or mixing may be required to provide a means
to enhance heat
transfer, which is necessary for trichome resin to ooze out, thus affording
better product cohesion
and smoothness, and for facilitating cannabinoid decarboxylation. In the
present case, it was
surprisingly discovered that the manufacturing process described herein
manages to increase
heat transfer efficiency without addition of water. For example, the present
manufacturing process
can achieve high heat and shear sufficient to obtain the desired hashish
characteristics. In some
embodiments, such high heat and shear can be created from mechanical mixing
elements such
as mixing pins and/or reverse flow elements. The reverse flow elements can
increase the
retention time of material on the mixing elements that it precedes. The mixing
pins and reverse
flow elements collectively can result in a tightly packed area that
contributes to an increase in
heat transfer efficiency. Such configurations can thus afford darker and
shinier hashish product
compared to hashish product manufactured with industrial press or single screw
extruder.
[0093] FIG. 1 is a non-limiting flowchart of a process 100 for making a
hashish product in
accordance with an embodiment of the present disclosure. The process 100
comprises a first step
110 of providing isolated cannabis trichomes.
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[0094] In one non-limiting example, the isolated cannabis trichomes may
include trichomes
isolated from a single cannabis strain. In another non-limiting example, the
isolated cannabis
trichomes may include trichomes isolated from a plurality of distinct cannabis
strains, which may
have different respective cannabinoid(s) and/or terpene(s) content. The choice
of one over the
other may be driven by practical considerations, such as but not limited to
inventory management
considerations, the desired cannabinoid content of the hashish product, the
desired user
experience, and the like. It is known amongst consumers of hashish and other
cannabis products
that using isolated cannabis trichomes produced from more than one strain of
cannabis plant may
allow a user to tune the psychoactive, medical and/or entourage effect
obtained by consuming
the product. The mixing of cannabis plant strains may also allow adjustments
to the final
concentration of a component of the product, for example but not limited to
the cannabinoid
content. Additionally, use of more than one strain allows for improved product
and waste
management ¨ important in commercial production.
[0095] The isolated cannabis trichomes may be obtained in several ways.
[0096] The producer implementing the process 100 may obtain the isolated
cannabis trichomes
from another producer. The step 110 may thus include a sub-step of obtaining
the isolated
cannabis trichomes from another producer (not shown in figures).
[0097] Alternatively, the producer implementing the process 100 may obtain the
isolated
cannabis trichomes via the following variants of step 110.
[0098] FIG. 2 is a variant 110' which includes starting from cannabis plant
material to isolate the
cannabis trichomes therefrom. In this variant, a first step 210 includes
providing cannabis plant
material comprising cannabis trichomes. The cannabis plant material may
comprise cannabis
flowers / buds, cannabis trim, cannabis leaves, or any combination thereof.
The producer
implementing the first variant step 110' may also produce the cannabis plant
material or may
obtain the cannabis plant material from another producer. In a second step
220, cannabis
trichomes are isolated therefrom, thus resulting in the isolated cannabis
trichomes. As discussed
previously, various processes for isolating cannabis trichomes from cannabis
plant material are
known and as such, will not be further described here.
[0099] In some embodiments, the variant step 110' may be performed at a first
location while
the remaining steps of process 100 may be performed at a second location,
where the first and
second locations may be within the same licensed producer site or within
different licensed
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producer sites. In some embodiments, all steps of process 100 may be performed
at the same
location.
Mixing isolated cannabis trichomes and retrieving through a die
[0100] Returning to Fig. 1, the process 100 further comprises a step 130 of
mixing the isolated
cannabis trichomes. In one practical implementation, the mixing includes
applying compression
and shear forces to the isolated cannabis trichomes via a plurality of
interpenetrate helicoidal
surfaces within an elongated enclosure. Preferably, the elongated enclosure is
an extruder device
having at least two screws. The isolated cannabis trichomes are mixed while
adding mechanical
or thermal energy under conditions sufficient to obtain a resinous mixture.
[0101] For example, the resinous mixture is a substantially homogeneous
mixture.
[0102] The conditions to form the resinous mixture at the mixing step 130
comprise shear,
pressure, and temperature, which may be varied to alter the characteristics of
the hashish
product. Such characteristics may include, but without being limited to
homogeneity, lightness,
%reflectance, stiffness (i.e., characteristic that defines the level of
malleability of the hashish
product), hardness or resistance to localized deformation (i.e.,
characteristic that determines how
easy it is to cut or separate the hashish product), toughness (i.e.,
characteristic that determines
the likelihood that the hashish product deforms rather than fractures under an
applied force),
color, tactual characteristics, and the like.
[0103] For example, the pressure being applied at the mixing step 130 may be
at a value of
about 1 bar or more. For example, a pressure of from about 1 bar to about 70
bar, including any
ranges therein or any value therein. For example, a pressure of from about 1
bar to about 65 bar,
from about 3 bar to about 60 bar, from about 4 bar to about 55 bar, from about
6 bar to about 50
bar, from about 8 bar to about 45 bar, from about 10 bar to about 40 bar, from
about 12 bar to
about 35 bar, from about 12 bar to about 32 bar, from about 14 bar to about 30
bar, from about
16 bar to about 28 bar, from about 18 bar to about 26 bar, or from about 20
bar to about 24 bar
including any ranges therein or any value therein. For example, a pressure of
about 1 bar, about
3 bar, about 4 bar, about 5 bar, about 8 bar, about 10 bar, about 12 bar,
about 14 bar, about 16
bar, about 18 bar, about 22 bar, about 22 bar, about 24 bar, about 26 bar,
about 28 bar, about 30
bar, about 32 bar, about 35 bar, about 40 bar, about 45 bar, about 50 bar,
about 55 bar, about 60
bar, or around 65 bar. The person of skill will readily understand that a
given pressure value may
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be selected depending on the die that is used to form the hashish product, as
described elsewhere
in this text.
[0104] For example, the temperature being applied at the mixing step 130 may
be at a value of
about 170 C or less. For example, a temperature of from about 20 C to about
170 C, including
any ranges therein or any value therein. For example, a temperature of about
20 C, about 25 C,
about 30 C, about 35 C, about 40 C, about 45 C, about 50 C, about 55 C, about
60 C, about
65 C, about 70 C, about 80 C, about 90 C, about 100 C, about 110 C, about 120
C, about
130 C, about 140 C, about 150 C, about 160 C, or about 170 C. It will be
readily apparent to the
person skilled in the art that different temperatures corresponding to the
abovementioned
temperature values or ranges may be used in different zones during the process
as described
elsewhere in this text.
[0105] The mixing shear and compressive forces can be controlled by modulating
the rotational
speed of the screws within the extruder. In such embodiments, the extruder
screws rotation per
minute (rpm) can be selected to perform the mixing step 130 at a value of for
example about 10
rpm or more. For example, extruder screws rpm can be selected in a range of
from about 10 rpm
to about 1000 rpm, including any ranges therein or any value therein. For
example, from about
15 to about 500 rpm, or from about 25 to about 450 rpm, or from about 30 to
about 400 rpm, or
from about 45 to about 450 rpm including any value within any of these ranges
and preferably
between 100 rpm and 200 rpm.
[0106] In embodiments where the heating and mixing are performed in a twin-
screw extruder,
the residence time within the extruder barrel can be directly related to the
length of the barrel and
the rotational speed of the twin screws. To increase mixing time of the
components within the
barrel, the components can travel through at least one zone of the barrel in a
distal direction, and
then be redirected to at least one zone of the barrel in a proximal direction
(i.e., towards the inlet
rather than towards the die).
[0107] Optional step 120 includes incorporating one or more additional
component at one or
more steps during the process 100. For example, one or more additional
component can be added
to the isolated trichomes prior to, simultaneously with, or following step
110, or prior to,
simultaneously with, or following the mixing step 130. Multiple additional
components may be
added in a single step or may be added separately in one or more consecutive
steps or at different
times or points along the process 100. The one or more additional components
can be one or
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more cannabinoids, one or more terpenes, one or more flavonoids, one or more
flavoring agents,
one or more non-toxic coloring agents, or any combination thereof. When the
one or more
component comprises a cannabinoid, the cannabinoid may be provided in the form
of a cannabis
extract (including a crude extract, or a winterized extract), a distillate, an
isolate, cannabis rosin,
cannabis resin, cannabis wax, or cannabis shatter.
[0108] In some embodiments, the one or more additional component may be
incorporated
during the process (through one or more input ports located at each of the
zones within the
extruder length, as described elsewhere in this text) to produce the hashish
product.
[0109] For example, the one or more additional component may be substantially
homogeneously distributed throughout the hashish product.
[0110] Once the resinous mixture is obtained at step 130, at least a portion
of the resinous
mixture is retrieved at step 140 to obtain an individual unit of hashish
product having a cohesive
mass of the isolated trichomes.
[0111] For example, the hashish product may have a substantially homogeneous
cohesive
mass of the isolated trichomes.
[0112] FIG. 3 includes additional steps that can follow step 140 of the
process 100 in FIG. 1.
For example, the at least portion of the resinous mixture can be passed
through a die at step 150,
which may be configured to impart a pre-determined shape thereto. Optionally,
and prior to
passing through the die, the at least portion of the resinous mixture may be
cooled at step 145.
The solid or semi-solid hashish product from step 150, may optionally further
undergo post-
processing steps. For example, the solid or semi-solid hashish product from
step 150 may be cut
to a pre-determined cutting pattern, a pre-determined weight, or a pre-
determined length to obtain
smaller units of hashish product for a pre-determined packaging size (not
shown in the figures).
Practical implementation
[0113] There are several options to implement the herein described process
100.
[0114] FIG. 4 illustrates a system 400 for implementing the process 100 to
make a coherent and
cohesive mass 480 in accordance with an embodiment. The system 400 includes an
extruder
apparatus 410 that uses mechanical mixing means to amalgamate the isolated
cannabis
trichomes 420 into the coherent and cohesive mass 480.
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[0115] In this embodiment, the system 400 comprises a feed hopper 425 through
which the
isolated cannabis trichomes 420 are fed. Optionally, one or more additional
component(s) 440
are fed through the feed hopper 425 and/or through one or more input port 445
located along the
length of the apparatus 410 at locations corresponding to one or more
predetermined portions or
zones 450A-G of the extruder apparatus 410. As discussed previously, non-
limiting examples of
such one or more additional component(s) 440 include, for example, terpenes,
flavonoids,
cannabinoids in the form of crude extracts, distillates, isolates, winterized
cannabis extracts, rosin,
shatter, or resins, or any combinations thereof.
[0116] The extruder apparatus 410 is powered by a motor (not shown) that
drives at least two
extruder screws 430 to apply pressure and mechanical shear on the isolated
cannabis trichomes
420 and optionally the one or more additional component(s) 440 entering the
extruder 410 (for
the sake of brevity only one screw of the twin-screw is illustrated in Fig.
4). For example, the
extruder screws 430 may be configured for applying compression and shear
forces to the isolated
cannabis trichomes 420 via a plurality of interpenetrate helicoidal surfaces
present along at least
a portion of the extruder screws 430.
[0117] The extruder apparatus 410 may also implement a pressure sensing
element 460 at the
die vicinity zone 455 which is a measure of the shear force applied on the
isolated cannabis
trichomes 420 packing them into a cohesive mass. The pressure may be at a
value of about 1
bar or more. For example, a pressure of from about 1 bar to about 70 bar,
including any ranges
therein or any value therein. For example, a pressure of from about 1 bar to
about 65 bar, from
about 3 bar to about 60 bar, from about 4 bar to about 55 bar, from about 6
bar to about 50 bar,
from about 8 bar to about 45 bar, from about 10 bar to about 40 bar, from
about 12 bar to about
35 bar, from about 12 bar to about 32 bar, from about 14 bar to about 30 bar,
from about 16 bar
to about 28 bar, from about 18 bar to about 26 bar, or from about 20 bar to
about 24 bar including
any ranges therein or any value therein. For example, a pressure of about 1
bar, about 3 bar,
about 4 bar, about 5 bar, about 8 bar, about 10 bar, about 12 bar, about 14
bar, about 16 bar,
about 18 bar, about 22 bar, about 22 bar, about 24 bar, about 26 bar, about 28
bar, about 30 bar,
about 32 bar, about 35 bar, about 40 bar, about 45 bar, about 50 bar, about 55
bar, about 60 bar,
or around 65 bar
[0118] When desired, the system 400 may also implement heating by maintaining
a set of
predetermined temperature within the one or more predetermined portions or
zones 450A-G of
the extruder apparatus 410, or throughout the length of the extruder apparatus
410, depending
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on specifics applications. For example, the temperature being applied within
each of the one or
more predetermined portions or zones 450A-G of the extruder apparatus 410 may
be at a value
of about 170 C or less, the temperature in one zone being selected
independently from another.
For example, each of the one or more predetermined portions or zones 450A-G
can
independently be at a temperature selected within the range of from about 20 C
to about 170 C,
including any ranges therein or any value therein. For example, each of the
one or more
predetermined portions or zones 450A-G can independently be at a temperature
of about 20 C,
about 25 C, about 30 C, about 35 C, about 40 C, about 45 C, about 50 C, about
55 C, about
60 C, about 65 C, about 70 C, about 80 C, about 90 C, about 100 C, about 110
C, about 120 C,
about 130 C, about 140 C, about 150 C, about 160 C, or about 170 C. Also,
depending on
specific application, heating is also implemented at the extruder die by
maintaining a
predetermined temperature at the die zone 455. The system 400 may also
implement several
zones across the length of the apparatus 410 each performing a single
functionality including but
not limiting to conveying, mixing, compressing, and reversing the flow
direction of the resinous
mixture (or isolated cannabis trichomes). The operating parameters of the
extruder apparatus
410, such as those discussed previously (e.g., temperature, pressure, and
extruder screws rpm),
can be selected to alter residence time of the resinous mixture (or isolated
cannabis trichomes
420) in the extruder apparatus 410 to obtain the cohesive mass 480.
Advantageously, it has been
observed that operating parameters such as heat and extrusion speed change the
pressure
experienced at the die and may alter the characteristics of the hashish
product discussed above.
For example, the pressure applied by the extruder screws can be accompanied by
different
temperature settings within each portions or zones 450A-G of the extruder to
enhance mixing of
the isolated cannabis trichomes, extract the resinous content of the trichomes
and obtain a
heated, cohesive, continuous, resinous mixture, preferably substantially
homogenous resinous
mixture. For example, the heating and mixing can continue until a desired
level of homogeneity
is obtained.
[0119] In some embodiments, the heating may additionally advantageously assist
in mixing the
isolated cannabis trichomes 420 and optional additional components 440 to form
the cohesive
mass 480. For example, the heating can assist in at least partially melting
optional additional
components 440, such as cannabinoid isolate.
[0120] In some embodiments, the heat may be applied through heating elements
(not shown)
embedded with the extruder screws 430 extending along the one or more
predetermined portions
or zones 450A-G across the length of the extruder 410. To control the amount
of heat input to the
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extruder and ensure that a predetermined temperature prevails in a certain
zone 450A-G within
the extruder 410, one or more temperature controlling units (not shown) can
also be associated
with the extruder apparatus 410 to monitor heat within the certain zone 450A-G
of the extruder
apparatus 410 and take any necessary action in the event of major deviations
from the intended
extrusion temperature.
[0121] At least a portion of the resinous mixture exits an extruder die 470 at
the outlet of the
extruder apparatus 410 in the form of an elongated, continuous solid or semi-
solid cohesive mass
480. The die 470 may impart any pre-determined shape to the cohesive mass 480.
At that point
in the process, the long and continuous solid or semi-solid cohesive mass 480
can be subjected
to ambient temperature and pressure.
[0122] A cutting means 485 may be placed downstream of the extruder die 470 to
cut the
cohesive mass 480 according to a pre-established cutting pattern. In a non-
limiting example of
implementation, the pre-established cutting pattern may comprise cutting the
cohesive mass 480
along a transverse axis and at pre-determined time intervals to obtain hashish
product units of a
pre-determined length and/or weight. For example, to obtain a plurality of
hashish product units
with consistent dimensions and/or weight, the cutting means can act
intermittently to cut the
cohesive mass 480 into individual units of hashish product 510. The individual
units of hashish
product could be further transferred onto a flat conveyor belt or fall under
gravity over an inclined
conveyor belt (not shown) and sent for packaging and/or storage.
Test procedure for assessing %reflectance
[0123] FIG. 5 illustrates a non-limiting schematic of a system 500 for
determining gloss and
%reflectance of the hashish product 520 using a glossmeter 510.
[0124] The hashish product 510 may lie on a flat surface and the glossmeter
510 is placed on
top of the hashish product. The glossmeter 510 has a built-in light emitter
530A that directs
incident light 540A onto the surface of the hashish product with an incidence
angle Y. The
incidence angle Y may vary depending on the level of gloss (GU) as well as the
particular industry
wherein these measurements are done. As described previously, typical values
for Y are 20 , 600
or 80 wherein typically, Y=20 is used for a high gloss surface (>70 GU),
Y=60 is used for a
semi-gloss surface (10-70 GU) and Y=85 is used for a low gloss/matt surface
(<10 GU).
Reflected light 540B is the light reflected from the surface of the hashish
product at the same
angle as the incident angle Y and is sensed by a built-in photodetector 530B.
Diffuse reflected
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lights 550 are lights reflected in all directions with angles #Y. The
glossmeter upon incidence of
light on the surface of the hashish product 510 with the angle Y, determines
the fraction of light
reflected from the surface at the same angle as incident light angle (Y for
540A) to calculate gloss
unit (GU) and further the %reflectance as discussed previously.
EXAMPLES
[0125] The following examples are for illustrative purposes only and are not
meant to limit the
scope of the compositions and methods described herein.
Comparative Example 1
[0126] In this Example, multiple batches of isolated cannabis trichomes (BBI-
038, NLxBB strain)
were separately loaded into the feed hopper of an ETPI Lab extruder (The
Bonnot Company,
USA) having a single extrusion screw. Water in different amounts was added
during extrusion of
each batch of isolated cannabis trichomes. The resulting hashish product from
each batch was
monitored for mold growth over time. The results are set forth in Table CX-1.
Table CX-1
Extruder Parameters:
Barrel temperature: 60 C Melt temperature: 60 C Die: custom
rectangular
Test Mass of Mass of Average Water
Mold growth
isolated water added moisture activity of
cannabis to the content of hashish
trichomes (g) extruder (g) hashish product
product
(wt.%)
BBE-028 120 7.7 8.77% 0.79 No mold
formed
BBE-029 120 11.8 8.86% 0.84 Mold
formed within
2 weeks
BBE-030 120 15.7 13.43% 0.86 Mold
formed within
1 week
BBE-031 120 20.5 15.35% 0.88 Mold
formed within
1 week
[0127] It was observed that hashish products having a moisture content above 8
wt.% relative
to total weight of the hashish product increased the likelihood of mold
formation within 1-2 weeks.
[0128] Examples of hashish products made according to principles described
herein are
discussed below. In these examples, for each hashish product, a sample of the
hashish product
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was prepared and tested to measure various characteristics of the hashish
product, such as
%reflectance, etc. The sample was prepared by flattening a portion of the
hashish product for 30
seconds at a pressure of 9000 psi on a 3 in. x 5 in. area die. The
%reflectance of the hashish
product was determined by measuring gloss units (GU) using a LAN DTEK GM-268
glossmeter
set up with an 85 angle of incidence.
Example 1
[0129] In this example, a batch of isolated cannabis trichomes was processed
in a twin-screw
extruder to obtain a hashish product.
[0130] A batch of isolated cannabis trichomes (Meridian strain) was loaded
into the feed hopper
(zone 1) of a Pharma 11 twin-screw extruder (ThermoFisher ScientificTM, USA)
with parallel 11mm
diameter twin screws and length-to-diameter ratio (L/D) of 40:1 segmented into
7 processing
zones (zone 2 to zone 8). A chiller circulating water at 10 C was used to
implement temperature
control within the processing zones as well as the die. The initial extruder
setup (I) featured two
mixing zones ("MIX") within the middle part of the extruder (i.e., zones 4 and
6) and a compression
zone ("COMP") at the end of the screw (zone 8), as set forth in Table EX-1-1:
Table EX-1-1
Extruder setup (I)
Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
1.5 LID COMP + CONV CONV MIX CONV MIX CONV CONV
[0131] The isolated cannabis trichomes were fed in the twin-screw extruder
with a feed rate of
1.7 g/min. The twin-screw extruder having a torque of 5-8%, an rpm of 300 and
a 7mm die
(pressure of 0-1 bar, temperature 70 C or 90 C). The temperature profile
across the extruder
length was according to Table EX-1-2:
Table EX-1-2
Die (7mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
70 C or 90 C 70 C 90 C 140 C 140 C 140 C 80 C 50 C
Hashish product batch#: BBE-062
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[0132] The resulting hashish product (see FIG. 6A) made from isolated cannabis
trichomes at
a die temperature of 70 C had a shredded (non-cohesive) appearance whereas
increasing the
die temperature to 90 C resulted in a hashish product with smooth and
malleable texture that was
brown in color. Without being bound by any theory, it seemed that the larger
the temperature
difference between the die temperature and resinous mixture temperature, the
hashish product
output from the die would be susceptible to more deformation. Interestingly,
no mold has formed
on the hashish products made in this example over a period of at least 2
weeks. The hashish
products were kept in sealed ZipIOCTM bags, placed in a plastic container, at
room temperature
with exposure to daylight. The hashish product had a reflectance of 6.4 GU,
corresponding to a
%reflectance of 4%85.
Example 2
[0133] In this example, extruder setup (I) from Example 1 was maintained while
a die with
smaller diameter (4.5 mm) was employed resulting in an increase in
cohesiveness and darker
color of the extruded hashish product.
[0134] Isolated cannabis trichomes (Meridian strain) with a feed rate
of 2.5 g/min were fed to
the twin-screw extruder at an rpm of 300. The temperature profile across the
extruder length was
according to Table EX-2-1:
Table EX-2-1
Die (4.5mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
90 C 80 C 80 C 140 C 140 C 140 C 80 C 50 C
Hashish product batch#: BBE-063
[0135] It was observed that decreasing the die diameter resulted in gradual
clogging and
pressure build up at the die, which halted the extrusion operation upon steady
state. This was
attributed to separation of resins from the isolated cannabis trichomes at the
die (due to high
temperature at the die) which resulted in the passage of resin material
through the die leaving the
non-viscous plant material behind the die which in turn led to clogging.
Interestingly, no mold has
formed on the hashish products made in this example over a period of at least
2 weeks. The
hashish products were kept in sealed ZiplocTM bags, placed in a plastic
container, at room
temperature with exposure to daylight. The hashish product had a reflectance
of 7.2 GU,
corresponding to a %reflectance of 4.5%85.
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Example 3
[0136] In this example, extruder setup (I) from Example 1 and die diameter of
Example 2 (4.5
mm) were maintained while the extruder feed was 94 wt.% isolated cannabis
trichomes and 4%
water to further assist flow through the extruder. Also, the temperature at
the die and within the
mixing zones were lowered to lessen the separation of resin from the
trichomes.
[0137] Isolated cannabis trichomes (Meridian strain) with a feed rate of 2.5
g/min (94 wt%
isolated cannabis trichomes and 4% water) were fed to the twin-screw extruder
at an rpm of 300,
a 10% torque, die temperature and pressure of 80 C and 1 bar, respectively.
The temperature
profile across the extruder length was according to Table EX-3-1:
Table EX-3-1
Die (4.5mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
80 C 80 C 80 C 120 C 120 C 120 C 80 C 50 C
Hashish product batch#: BBE-064
[0138] It was observed that adding water to the isolated cannabis trichomes
did not have a
significant impact on clog prevention (as compared to Example 2) and only
delayed the clogging
after reaching steady state by -30 minutes. The combined feeding of water and
isolated cannabis
trichomes also resulted in a clumpy mix that further contributed to clogging.
Moreover, the
separation of resins from the isolated cannabis trichomes at the die (due to
high temperature at
the die) repeated and the resulting hashish product was less pliable (harder)
as compared to the
hashish product obtained in Example 2. Interestingly, no mold has formed on
the hashish products
made in this example over a period of at least 2 weeks. The hashish products
were kept in sealed
ZiploCTM bags, placed in a plastic container, at room temperature with
exposure to daylight. The
hashish product had a reflectance of 6.5 GU, corresponding to a %reflectance
of 4%85.
Example 4
[0139] In this example, identical process parameters as those of Example 3
were implemented
except that water was not added in the feed stream. Also, to analyze the
effects of torque, die
temperature, die pressure and temperature across extruder zones on the hashish
product, these
conditions were also varied in this example.
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[0140] Isolated cannabis trichomes (Meridian strain) with a feed rate of 2.5
g/min were fed to
the twin-screw extruder at a reduced rpm of 100 and under the following
conditions as set forth
in Tables EX-4-1 to EX-4-3:
[0141] Operating condition I)
Table EX-4-1
Torque: 55% die pressure: 70 bar
Die (4.5mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
40 C 30 C 30 C 30 C 70 C 70 C 70 C 30 C
Hashish product batch#: BBE-073-A
[0142] Operating condition II)
Table EX-4-2
Torque: 20% die pressure: 20 bar
Die (4.5mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
45 C 40 C 45 C 65 C 140 C 140 C 140 C 30 C
Hashish product batch#: BBE-073-C
[0143] Operating condition III)
Table EX-4-3
Torque: 11% die pressure: 5-8 bar
Die (4.5mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
60 C 40 C 45 C 65 C 140 C 140 C 140 C 30 C
Hashish product batch#: BBE-073-D
[0144] It was observed that increased temperature in mixing zones (operating
condition I vs. III)
or die (operating condition ll vs. III) decreased the required mechanical work
(as evidenced by
torque and die pressure) to extrude the isolated cannabis trichomes and output
the hashish
product. Meanwhile, the colors of the obtained hashish products across
operating conditions I) to
III) varied from beige/brown to dark brown albeit, all products lacked the
desirable shininess.
Interestingly, no mold has formed on the hashish products made in this example
over a period of
at least 2 weeks. The hashish products were kept in sealed ZiplocTM bags,
placed in a plastic
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container, at room temperature with exposure to daylight. The hashish products
corresponding to
EX-4-1 to EX-4-3 had reflectance values of 7.7 GU, 6.9 GU and 6.8 GU,
respectively,
corresponding to %reflectance values of 4.8%85, 4.3%85 and 4.2%85,
respectively.
[0145]
Example 5
[0146] In this example, extruder setup (I) from Example 1 was maintained.
However, in order to
achieve a shiny hashish product, it was postulated to increase the mechanical
work by decreasing
the die diameter to 2 mm thus generating more pressure. Also, to analyze the
effects of extruder
rpm and zone temperatures on the hashish product, these conditions were varied
in this example.
[0147] Isolated cannabis trichomes (Meridian strain) with a feed rate of 2.5
g/min were fed to
the twin-screw extruder under the following conditions as set forth in Tables
EX-5-1 to EX-5-3
(variable zone temperatures in bold):
[0148] Operating condition I)
Table EX-5-1
rpm: 50, 100, then 200 die pressure: 30 bar
Die (2nnnn) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
70 C 70 C 80 C 150 C 150 C 150 C 80 C 30 C
Hashish product batch#: BBE-075-C
[0149] Operating condition II)
Table EX-5-2
rpm: 200 die pressure: 22 bar
Die (2mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
70 C 70 C 80 C 160 C 160 C 160 C 80 C 30 C
Hashish product batch#: BBE-075-D
[0150] Operating condition III)
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Table EX-5-3
rpm: 200 die pressure: 12 bar
Die (2mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
70 C 70 C 80 C 170 C 170 C 170 C 80 C 30 C
Hashish product batch#: BBE-075-E
[0151] It was observed from operating condition I) that feeding the isolated
cannabis trichomes
to the extruder at 50 rpm resulted in low product clearance from the screws
and therefore, hashish
product output was inconsistent (undesirable). While increased rpms resulted
in more steady
output of hashish product, all products lacked the desirable shine. It was
concluded that the rpm
must be adjusted to the feed rate to allow sufficient clearance of the
material in order to avoid
problems in feeding (such as bridging). It was postulated that an increase in
retention time of
isolated cannabis trichomes in the mixing zone (more mechanical and thermal
energy transfer)
would contribute to more desirable hashish product. Interestingly, no mold has
formed on the
hashish products made in this example over a period of at least 2 weeks. The
hashish products
were kept in sealed ZiplocTM bags, placed in a plastic container, at room
temperature with
exposure to daylight. The hashish products corresponding to EX-5-1 to EX-5-3
had reflectance
values of 6.8 GU, 6.9 GU and 7.3 GU, respectively, corresponding to
%reflectance values of
4.2%85, 4.3%85 and 4.6%85, respectively.
Example 6
[0152] In this example, an additional extruder setup (II) was tested. Extruder
setup (II)
distinguishes from extruder setup (I) in the presence of a reverse flow
segment ("REV") after the
first mixing zone with the aim of increasing retention time of isolated
cannabis trichomes in the
mixing zone (more mechanical and thermal energy transfer). The overall
breakdown for the
extruder setup (II) is set forth in Table EX-6-1:
Table EX-6-1
Extruder setup (II)
Zone 8 Zone 7 Zone Zone 5
Zone 4 Zone 3 Zone 2
6
1.5 L/D COMP + CONV MIX CONV +
MIX CONV CONV
CONV 0.5 LID REV
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[0153] Isolated cannabis trichomes (NLxBB strain) with a feed rate of 2.5
g/min were fed to the
twin-screw extruder and under the following conditions as set forth in Tables
EX-6-2 to EX-6-5 to
assess the impact of change in screw step and temperature variation at the die
and within different
zones:
[0154] Operating condition I)
Table EX-6-2
rpm: 100 Torque: 42% die pressure: 65 bar
Die (2mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
60 C 80 C 80 C 80 C 80 C 80 C 80 C 30 C
Hashish product batch#: BBE-080-A
[0155] Operating condition II)
Table EX-6-3
Torque: 38% die pressure: 35 bar rpm: 100
Die (2mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
70 C 80 C 80 C 80 C 80 C 80 C 80 C 30 C
Hashish product batch#: BBE-080-B
[0156] Operating condition III)
Table EX-6-4
Torque: 28% die pressure: 35 bar rpm: 100
Die (2mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
70 C 80 C 80 C 110 C 110 C 110 C 80 C 30 C
Hashish product batch#: BBE-080-C
[0157] Operating condition IV)
Table EX-6-5
Torque: 26% diepressure: 34 bar rpm: 100
Die (2mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
7000 80 C 80 C 140 C 140 C 140 C 80 C 30 C
Hashish product batch#: BBE-080-D
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[0158] It was observed from operating conditions I) to IV) that the obtained
hashish products
were darker in color and more malleable compared to those obtained in Examples
1 to 5 that
employed the initial screw setup (I) without a reverse flow element. Further,
comparing the
hashish products obtained across operating conditions I) to IV) of this
Example, the surface of the
hashish product from operating condition IV) was less smooth and less shiny
compared to that of
operating condition III). Hashish product obtained from operating condition
III) was the only one
exhibiting shiny characteristic. The overall improvement in product
characteristics in this Example
compared to previous Examples was attributed to increased residence time (due
to addition of
reverse flow element). Also, the observed increase in compaction within the
mixing zones seemed
to be due to an increase in heat and mechanical energy transfer to the
isolated cannabis
trichomes with the extruder setup (II). Further, increase of temperature in
variable zones (from
80 C to 140 C) showed to have a positive impact on hashish product quality (in
terms of
appearance) up to a certain point beyond which a degradation was observed. For
example, under
the conditions assessed here, this point was about 120 C.
[0159] Overall, it was concluded that extending the duration through which the
isolated cannabis
trichomes are subjected to compression and shear forces within the screw path
would lead to
hashish products with higher quality (specifically in terms of appearance).
The appearance
characteristics are shown in FIG. 6B (corresponding to operating conditions
HI) and IV)).
Interestingly, no mold has formed on the hashish products made in this example
over a period of
at least 2 weeks. The hashish products were kept in sealed ZiplOcTM bags,
placed in a plastic
container, at room temperature with exposure to daylight. The hashish products
corresponding to
EX-6-3 to EX-6-5 had reflectance values of 6.5 GU, 7.1 GU and 7.2 GU,
respectively,
corresponding to %reflectance values of 4%85, 4.4%85 and 4.5%85,
respectively).
Example 7
[0160] In this example, an additional extruder setup (III) was tested.
Extruder setup (III)
distinguishes from extruder setup (II) in the presence of a second compression
element after the
lead element while the two mixing sections were combined upstream of the
reverse flow element.
The mixing section was placed near the compression elements, spanning the last
two heated
zones as set forth in Table EX-7-1:
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Table EX-7-1
Extruder setup (III)
Zone 8 Zone 7 Zone Zone 5 Zone 4 Zone 3
Zone 2
6
3 LID COMP + MIX CONV CONV CONV CONV CONV
1 L/D CONV +
0.5 LID REV +
1 LID MIX
[0161] Isolated cannabis trichomes (NLxBB strain) with a feed rate of 2 g/min
were fed to the
twin-screw extruder and under the following conditions as set forth in Tables
EX-7-2 to EX-7-5 to
assess the impact of change in screw step and temperature variation at the die
and within variable
zones:
[0162] Operating condition I)
Table EX-7-2
Torque: 33-35% die pressure: 32-35 bar rpm: 200
Die (2mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
70 C 80 C 80 C 80 C 80 C 80 C 60 C 30 C
Hashish product batch#: BBE-083-A
[0163] Operating condition II)
Table EX-7-3
Torque: 30-31% die pressure: 35-38 bar rpm: 200
Die (2mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
75 C 85 C 100 C 100 C 80 C 80 C 60 C 30 C
Hashish product batch#: BBE-083-B
[0164] Operating condition III)
Table EX-7-4
Torque: 30-31% die pressure: 30-31 bar rpm: 200
Die (2mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
80 C 90 C 120 C 120 C 80 C 80 C 60 C 30 C
Hashish product batch#: BBE-083-C
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[0165] Operating condition IV)
Table EX-7-5
Torque: 28-29% die pressure: 20-24 bar rpm: 200
Die (2mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
90 C 100 C 120 C 120 C 80 C 80 C 60 C 30 C
Hashish product batch#: BBE-083-D
[0166] It was observed from operating conditions I) to IV) that the obtained
hashish product from
operating condition IV) was less shiny and less smooth (i.e., deformation on
the surface of the
product) compared to that obtained from operating condition III) which was in
turn found to be
less shiny and less smooth compared to that obtained from operating condition
II). Moreover, the
hashish product from operating condition IV) was pushed out of the die in an
inconsistent manner
with black resin dripping from the die (characteristic of a pre-clog event).
Overall, it was concluded
that by using appropriate temperature within zones that have increased product
compaction and
shear, it would be possible to obtain a hashish product with desired
characteristics (color and
malleability). For example, under the conditions assessed here, the preferred
temperature range
was from about 100 C to about 120 C. It is hypothesized that the product could
be made further
soft and malleable by increasing the shear forces experienced by the product
via the elongation
of compression and mixing segments or via an increase in retention time within
the mixing
segments. Interestingly, no mold has formed on the hashish products made in
this example over
a period of at least 2 weeks. The hashish products were kept in sealed
ZiplocTM bags, placed in
a plastic container, at room temperature with exposure to daylight. The
hashish products
corresponding to EX-7-2 to EX-7-5 had reflectance values of 6.9 GU, 7.1 GU,
7.3 GU and 7.1
GU, respectively, corresponding to %reflectance values of 4.3%85, 4.4%85,
4.5%85 and 4.4%85,
respectively.
Example 8: Extruded Hash Infused with CBD Distillate
[0167] In this Example, hashish product infused with CBD was manufactured
using the extruder
set up (II) as set forth in Table EX-8-1.
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Table EX-8-1
Screw setup (II)
Zone 8 Zone 7 Zone Zone 5 Zone 4 Zone 3 Zone 2
6
1.5 L/D COMP + CONV MIX CONV +
MIX CONV CONV
CONV 0.5 LID REV
[0168] Isolated cannabis trichomes (NLxBB strain) with a feed rate of 2 g/min
were fed to the
twin-screw extruder. CBD distillate was introduced via a liquid feeding port
in zone 3 through use
of a syringe that dispensed the molten product at 60 C at a programmed feed
rate. The extruder
was operated with the following operating conditions as set forth in Tables EX-
8-2, EX-8-4 and
EX-8-6:
[0169] Operating condition I): control with no CBD distillate infusion
Table EX-8-2
Torque: 28% die pressure: 35 bar
rpm=200
Feed: 2 g/min isolated cannabis trichomes
Die (2mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
70 C 80 C 80 C 120 C 120 C 120 C 80 C 30 C
Hashish product batch#: BBE-081-D
[0170] Analytical results of input isolated cannabis trichomes and output hash
corresponding to
operating condition I) are shown in Table EX-8-3 (n=15 samples of isolated
cannabis trichomes
and hashish products). CBD and THC levels were measured with high performance
liquid
chromatography (HPLC) while moisture content was determined via
Thermogravimetric Moisture
Balance-type Analyzer.
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Table EX-8-3
Input isolated cannabis trichomes Output Hashish Product
CBD THC Moisture CBD THC Moisture
Level Level content (%) Level
Level content
%=Null % = 27.2 6.15 %=Null % =
26.8 4.95
a = N/A, a = 0.61 a = N/A, a = 0.88
CV = N/A CV = 2.2 CV = N/A CV = 3.3
a = Standard Deviation, CV= Coefficient of Variation
[0171] Operating condition II) ¨ CBD distillate infusion
Table EX-8-4
Torque: 22% die pressure: 20-25
bar rpm=100
Feed: 2 g/min isolated cannabis trichomes + 0.29 g/min CBD Distillate (molten)
Die (2mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
70 C 80 C 80 C 120 C 120 C 120 C 80 C 30 C
Hashish product batch#: BBE-081-E
[0172] Analytical results of input isolated cannabis trichomes and output hash
corresponding to
operating condition II) are shown in Table EX-8-5 (n=15 samples of isolated
cannabis trichomes
and hashish products). CBD and THC levels were measured with high performance
liquid
chromatography (HPLC) while moisture content was determined via
Thermogravimetric Moisture
Balance-type Analyzer:
Table EX-8-5
Input isolated cannabis Input CBD Distillate ..
Output Hashish Product
trichomes
CBD THC Moisture CBD THC CBD THC Moisture
Level Level content Level Level Level
Level content
(0/0) (%)
%=Null % = 27.2 6.15 % = % = 2.85
%=5.4 % = 25.1 3.58
a = N/A, a = 0.61 78.57 a = 0.35, a =
0.74
CV = CV = 2.2 CV = 6.39 CV 2.96
N/A
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[0173] Operating condition III) ¨ CBD distillate infusion
Table EX-8-6
Torque: - die pressure: - rpm=100
Feed: 2 g/min isolated cannabis trichomes + 0.5 g/min CBD Distillate (molten)
Die (2mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
70 C 80 C 80 C 120 C 120 C 120 C 80 C 30 C
Hashish product batch#: BBE-081-F
It was visually observed that the addition of molten distillate resulted in a
homogenous and shiny
hashish product while causing a reduction in torque and die pressure
(operating condition I vs II)
due to the lubricating effect during extrusion. Moreover, the moisture content
of the hashish
product under operating condition II) that entailed distillate addition was
lower than that of
operating condition I) wherein only isolated cannabis trichomes were fed to
the extruder. In
conclusion, CBD infusion during extrusion could be done in a homogenous manner
and resulted
in a shinier and more malleable hashish product. Interestingly, no mold has
formed on the hashish
products made in this example over a period of at least 2 weeks. The hashish
products were kept
in sealed ZiplocTM bags, placed in a plastic container, at room temperature
with exposure to
daylight. The hashish products corresponding to EX-8-2 and EX-8-4 had
reflectance values of
7.5 GU and 7.7 GU, respectively, corresponding to %reflectance values of
4.6%85 and 4.8%85,
respectively.
Example 9: Extruded Hash Infused with CBD Isolate
[0174] In this example, hashish product infused with CBD isolate was
manufactured in order to
compare the resulting hashish product characteristics with that of Example 8.
Same extruder
setup (II) as that one of Example 8 was used.
[0175] Isolated cannabis trichomes (NLxBB strain) and CBD isolate were mixed
using a
commercially available KitchenAidTM mixer and the mixture was fed to the twin-
screw extruder at
a rate of 2 g/min and under the following operating conditions as set forth in
Tables EX-9-1 to EX-
9-2:
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[0176] Operating condition I): control with no CBD isolate infusion
Table EX-9-1
Torque: 18-20% die pressure: 20-21 bar rpm=200
Feed: 2 g/min isolated cannabis trichomes
Die (2mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
70 C 80 C 80 C 110 C 110 C 110 C 80 C 30 C
Hashish product batch#: BBE-082-A
[0177] Operating condition II) ¨ CBD isolate infusion
Table EX-9-2
Torque: 16-18% die pressure: 15-18
bar rpm=200
Feed: 2 g/min of a mixture of isolated cannabis trichomes (87.5 wt%) and CBD
isolate (12.5 wt%)
Die (2mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
70 C
80 C 80 C 110 C 110 C 110 C 80 C 30 C
Hashish product batch#: BBE-082-B
[0178] Analytical results of input isolated cannabis trichomes and output hash
corresponding to
operating condition II) are shown in Table EX-9-3 (n=15 samples of isolated
cannabis trichomes
and hashish products). CBD and THC levels were measured with high performance
liquid
chromatography (HPLC) while moisture content was determined via
Thermogravimetric Moisture
Balance-type Analyzer:
Table EX-9-3
Input mixture of isolated cannabis Output Hashish Product
trichomes and CBD isolate
CBD THC Moisture CBD
THC Moisture
Level Level content (%) Level Level
content
(c)/0)
%=11.4 % = 23 5.41 %=11.5 % = 23.4
3.8
a = 0.37, a = 0.53 a = 0.55, a = 0.54
CV = 3.19 CV = 2.25 CV = 4.77
CV = 2.32
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[0179] It was visually observed that the addition of CBD isolate to isolated
cannabis trichomes
and feeding them as a mixture to the twin-screw extruder resulted in a lower
torque and die
pressure as the CBD isolate melted during extrusion and seemingly provided
lubrication to the
extruding material. Like Example 8, the resulting hashish product upon
addition of CBD isolate
was a shinier, softer and more malleable hashish product compared to the
control hashish product
obtained from operating condition l). Interestingly, no mold has formed on the
hashish products
made in this example over a period of at least 2 weeks. The hashish products
were kept in sealed
ZiploCTM bags, placed in a plastic container, at room temperature with
exposure to daylight. The
hashish products corresponding to EX-9-1 and EX-9-2 had reflectance values of
7.4 GU and 7.9
GU, respectively, corresponding to %reflectance values of 4.6%85 and 4.9%85,
respectively.
Example 10: Extruded Hash Infused with CBD Distillate
[0180] In this Example, hashish product infused with CBD was manufactured
using Extruder
setup (III) from Example 7.
[0181] Isolated cannabis trichomes (NLxBB strain) with a feed rate of 2 g/min
were fed to the
twin-screw extruder. CBD distillate was introduced via a liquid feeding port
in zone 3 through use
of a syringe that dispensed the molten product at 60 C at a programmed feed
rate. The extruder
was operated with the following operating conditions as set forth in Tables EX-
10-1, EX-10-3, EX-
10-5 and EX-10-6:
[0182] Operating condition I): control with no CBD distillate infusion
Table EX-10-1
Torque: 30-32% die pressure: 36-38 bar rpm=200
Feed: 2 g/min isolated cannabis trichomes
Die (2mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
70 C 80 C 110 C 110 C 80 C 80 C 6000 30 C
Hashish product batch#: BBE-084-A
[0183] Analytical results of THCA to THC conversion for input isolated
cannabis trichomes and
output hash corresponding to operating condition I) are shown in Table EX-10-2
(n=15 samples
of isolated cannabis trichomes and hashish products). THCA and THC levels were
measured with
high performance liquid chromatography (HPLC):
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Table EX-10-2
Input isolated cannabis trichomes Output Hashish Product
THCA Level THC Level THCA Level THC Level
%=26.2 % = 4.2 %=13.9 % = 14.6
a = 0.1 a = 0.3
CV = 2.2 CV = 2.4 CV = 2.3 CV = 2.4
a = Standard Deviation, CV= Coefficient of Variation
[0184] Operating condition II) ¨ CBD distillate infusion
Table EX-10-3
Torque: 23-25% die pressure: 16-17 bar rpm=200
Feed: 2 g/min isolated cannabis trichomes + 0.29 g/min CBD Distillate (molten)
Die (2mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
70 C 80 C 110 C 110 C 80 C 80 C 60 C 30 C
Hashish product batch#: BBE-084-B
[0185] Analytical results of THCA to THC conversion for input isolated
cannabis trichomes and
output hash corresponding to operating condition II) are shown in Table EX-10-
4 (n=15 samples
of isolated cannabis trichomes and hashish products). THCA and THC levels were
measured with
high performance liquid chromatography (HPLC):
Table EX-10-4
Input isolated cannabis trichomes Output Hashish Product
THCA Level THC Level THCA Level THC Level
%=26.2 % = 4.2 %=15.8 % = 10.5
o=0.6 o=0.1 o=0.3 o=0.4
CV = 2.2 CV = 2.4 CV = 2.2 CV = 3.5
a = Standard Deviation, CV= Coefficient of Variation
[0186] Operating condition III) ¨ CBD distillate infusion
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Table EX-10-5
Torque: 21-23% die pressure: 8-12 bar rpm=200
Feed: 2 g/min isolated cannabis trichomes + 0.5 g/min CBD Distillate (molten)
Die (2mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
7000 80 C 110 C 110 C 80 C 80 C 60 C 30 C
Hashish product batch#: BBE-084-C
[0187] Operating condition IV) ¨ CBD distillate infusion
Table EX-10-6
Torque: 20-21% die pressure: 8-12 bar rpm=200
Feed: 2 g/min isolated cannabis trichomes + 0.75 g/min CBD Distillate (molten)
Die (2mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
70 C 80 C 110 C 110 C 80 C 80 C 60 C 30 C
Hashish product batch#: BBE-084-D
[0188] It was visually observed that the control samples (without addition of
distillate) were
tougher (yet malleable) compared to those sample obtained with added
distillate. Increasing the
amount of added distillate resulted in softer and shinier hashish product. As
for the extruder, it
was observed that the addition of distillate beyond 0.5 g/min had no
significant effect on die
pressure. Moreover, the extrudate hashish products obtained under operating
conditions III) and
IV) were less smooth compared to those obtained under operating conditions I)
and II) which had
no or less distillate added. Finally, the conversion of THCA to THC during
extrusion was observed
to be less significant when infusing the product with distillate. The
appearance characteristics are
shown in FIG. 6D. Interestingly, no mold has formed on the hashish products
made in this
example over a period of at least 2 weeks. The hashish products were kept in
sealed ZiplocTM
bags, placed in a plastic container, at room temperature with exposure to
daylight. The hashish
products corresponding to EX-10-1, EX-10-3, EX-10-5 and EX-10-6 had
reflectance values of 7.4
GU, 7.9 GU, 8.8 GU and 8.9 GU, respectively, corresponding to %reflectance
values of 4.6%85,
4.9%85, 5.5%85 and 5.6%85, respectively.
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[0189] Also, without being bound by any theory, the present inventor believes
that there is a
change in product flow through the die upon increase in distillate feeding as
the product softens
and that the hashish product needs to exit the die at a cooler temperature in
order to remain
smooth
Example 11: Extruded Hash Infused with CBD Distillate
[0190] In this Example, the screw setup (III) from Example 10 was maintained
and the die
diameter was changed from 2mm to 4.5mm.
[0191] Isolated cannabis trichomes (NLxBB strain) with a feed rate of 2 g/min
were fed to the
twin-screw extruder. CBD distillate was introduced via a liquid feeding port
in zone 3 through use
of a syringe that dispensed the molten product at 60 C at a programmed feed
rate. The extruder
was operated with the following operating conditions as set forth in Tables EX-
11-1 to EX-11-3:
[0192] Operating condition I): control with no CBD distillate
infusion
Table EX-11-1
Torque: 27-28% die pressure: 7-8 bar rpm=200
Feed: 2 g/min isolated cannabis trichomes
Die (4.5mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
70 C 80 C 110 C 110 C 80 C 80 C 60 C 30 C
Hashish product batch#: BBE-085-A
[0193] Operating condition II) ¨ CBD distillate infusion
Table EX-11-2
Torque: 20-22% die pressure: 3-4 bar rpm=200
Feed: 2 g/min isolated cannabis trichomes+ 0.29 g/min CBD Distillate (molten)
Die (4.5mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
70 C 80 C 110 C 110 C 80 C 80 C 60 C 30 C
Hashish product batch#: BBE-085-B
[0194] Operating condition III) ¨ CBD distillate infusion
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Table EX-11-3
Torque: 19-20% die pressure: 1-3 bar rpm=200
Feed: 2 g/min isolated cannabis trichomes+ 0.5 g/min CBD Distillate (molten)
Die (4.5mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3 Zone 2
70 C 80 C 110 C 110 C 80 C 80 C 60 C 30 C
Hashish product batch#: BBE-085-C
[0195] It was visually observed that the control hashish products (operating
condition I)) were
malleable and had a shiny black and smooth appearance. However, they were
tougher compared
to the hashish product from operating condition II) which were in turn tougher
than those obtained
from operating condition III). In fact, hashish products obtained under
operating condition III) was
less smooth as it was becoming increasingly soft due to increase in distillate
feed rate. The
appearance characteristics are shown in FIG. 6E (corresponding to operating
conditions I) to III)).
Interestingly, no mold has formed on the hashish products made in this example
over a period of
at least 2 weeks. The hashish products were kept in sealed ZiplocTM bags,
placed in a plastic
container, at room temperature with exposure to daylight. The hashish products
corresponding to
EX-11-1, EX-11-2 and EX-11-3 had reflectance values of 7.3 GU, 8.7 GU and 8.7
GU,
respectively, corresponding to %reflectance values of 4.5%85, 5.4%85 and
5.4%85, respectively.
[0196]
Example 12
[0197] In this Example, hashish products are manufactured using a kief batch
from Meridian
strain by three distinct methods of extrusion with a twin-screw extruder
(Pharma 11 twin-screw
extruder (ThermoFisher ScientificTM, USA), extrusion with single-screw
extruder (ETPI Lab
extruder - Bonnot Company, USA as described for example in PCT/CA2021/050673)
and
pressing with an industrial press (for example as described in
PCT/CA2020/051733). The
following operating conditions were used in each case, as set forth in Table
EX-12-1.
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Table EX-12-1
Extruded Hashish Product (Twin Screw Extruder) ¨ Operating condition (I)
Torque: 19-20% die pressure: 1-3 bar rpm=200
Feed: 2 g/min isolated cannabis trichomes+ 0.5 g/min CBD Distillate
Die (2mm) Zone 8 Zone 7 Zone 6 Zone 5 Zone 4 Zone 3
Zone 2
70 C 80 C 110 C 110 C 80 C 80 C 60 C
30 C
Extruded Hashish Product (Single Screw Extruder) ¨ Operating condition (II)
Kief pre-treated in oven for 35min at 120 C
Kief feed to extruder: 157.1 gr Water added: 13.6 gr
Speed of extrusion: 45 rpm Pressure: 60-120 psi
Extruder Barrel Temp.: 60 C Melt Temp.: 55 C
Pressed Hashish Product ¨ Operating conditions (Ill)
Mass of kief: 45 gr Mass of water added: 1.35 gr
= Mould size: 3.0 in x 5.0 in1st pressing stage: 9400 lb of press load (25
C for 5min)
= Heating at 70 C for 30min (water bath)
= 2nd pressing stage (after a heating step): 9400 lb of press load (25 C
for 5min)
[0198] The resulting products in terms of appearance are shown in FIG. 7. It
was visually
observed that the pressed hashish product (operating condition III) had a
light color with darker
patches scattered over the surface (i.e., heterogeneous appearance likely due
to heterogeneous
distribution of cannabis plant matter). Although the hashish product obtained
from the single-
screw extruder (operating condition II) had a relatively more consistent and
brown color, it lacked
shininess. In contrast, the hashish product obtained from the twin-screw
extruder (operating
condition I) had both a consistent black color and a shiny surface.
[0199] High potency kief can make shiny hash more easily than low potency hash
as it is easier
bring out the resin to the surface. Hash that has been post-processed to
impart better surface
uniformity, such as when rolling into a ball, will also make any hash shinier.
When enough resin
coats the surface of the kief-turned-hash and the hash also meets the criteria
of a smooth surface,
it will have gloss. Higher potency can be obtained when making hash from
trichomes isolated with
water and ice methods (i.e., "bubble hash"), which have less impurities and
higher potency. Dry
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sift kief, in contrast, necessitates a lot of mechanical and/or thermal energy
to get that shine /
gloss. The present inventors have demonstrated that with the process described
herein, which
preferably uses a twin-screw extruder, there is sufficient energy input when
mixing any type of
kief, such as low potency, dry sift kief, etc., to facilitate resin oozing out
from the trichomes and
imparting better characteristics to the hashish product.
[0200] Other examples of implementations will become apparent to the reader in
view of the
teachings of the present description and as such, will not be further
described here.
[0201] Note that titles or subtitles may be used throughout the present
disclosure for
convenience of a reader, but in no way, these should limit the scope of the
invention. Moreover,
certain theories may be proposed and disclosed herein; however, in no way
they, whether they
are right or wrong, should limit the scope of the invention so long as the
invention is practiced
according to the present disclosure without regard for any particular theory
or scheme of action.
[0202] All references cited throughout the specification are hereby
incorporated by reference in
their entirety for all purposes.
[0203] Reference throughout the specification to "some embodiments", and so
forth, means that
a particular element (e.g., feature, structure, and/or characteristic)
described in connection with
the invention is included in at least one embodiment described herein, and may
or may not be
present in other embodiments. In addition, it is to be understood that the
described inventive
features may be combined in any suitable manner in the various embodiments.
[0204] It will be understood by those of skill in the art that throughout the
present specification,
the term "a" used before a term encompasses embodiments containing one or more
to what the
term refers. It will also be understood by those of skill in the art that
throughout the present
specification, the term "comprising", which is synonymous with "including,"
"containing," or
"characterized by," is inclusive or open-ended and does not exclude
additional, un-recited
elements or method steps.
[0205] Unless otherwise defined, all technical and scientific terms used
herein have the same
meaning as commonly understood by one of ordinary skill in the art to which
this invention
pertains. In the case of conflict, the present document, including definitions
will control.
[0206] As used in the present disclosure, the terms "around", "about" or
"approximately" shall
generally mean within the error margin generally accepted in the art, such as
for example +/- 20%,
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+1- 15%, +1- 10%, or +1- 5%. Hence, numerical quantities given herein
generally include such error
margin such that the terms "around", "about" or "approximately" can be
inferred if not expressly
stated.
[0207] As used throughout the present disclosure, the terms "concentration"
and "content" are
used interchangeably and refer to the weight or mass fraction of a
constituent, i.e., the weight or
mass of a constituent divided by the total mass of all constituents, and is
expressed in wt.%,
unless stated otherwise.
[0208] Although various embodiments of the disclosure have been described and
illustrated, it
will be apparent to those skilled in the art considering the present
description that numerous
modifications and variations can be made. The scope of the invention is
defined more particularly
in the appended claims.
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