WO2022104360A1 - Lyophilisation de matière végétale aromatique - Google Patents

Lyophilisation de matière végétale aromatique Download PDF

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Publication number
WO2022104360A1
WO2022104360A1 PCT/US2021/072363 US2021072363W WO2022104360A1 WO 2022104360 A1 WO2022104360 A1 WO 2022104360A1 US 2021072363 W US2021072363 W US 2021072363W WO 2022104360 A1 WO2022104360 A1 WO 2022104360A1
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Prior art keywords
plant matter
vacuum chamber
mtorr
pressure
freeze drying
Prior art date
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PCT/US2021/072363
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English (en)
Inventor
Travis J ARNOVICK
Original Assignee
Arnovick Travis J
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Application filed by Arnovick Travis J filed Critical Arnovick Travis J
Priority to US18/252,530 priority Critical patent/US20240118026A1/en
Publication of WO2022104360A1 publication Critical patent/WO2022104360A1/fr

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Classifications

    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B5/00—Drying solid materials or objects by processes not involving the application of heat
    • F26B5/04—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum
    • F26B5/06—Drying solid materials or objects by processes not involving the application of heat by evaporation or sublimation of moisture under reduced pressure, e.g. in a vacuum the process involving freezing
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B1/00—Preliminary treatment of solid materials or objects to facilitate drying, e.g. mixing or backmixing the materials to be dried with predominantly dry solids
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
    • F26B21/06—Controlling, e.g. regulating, parameters of gas supply
    • F26B21/08—Humidity
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F26—DRYING
    • F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
    • F26B21/00—Arrangements or duct systems, e.g. in combination with pallet boxes, for supplying and controlling air or gases for drying solid materials or objects
    • F26B21/06—Controlling, e.g. regulating, parameters of gas supply
    • F26B21/10—Temperature; Pressure

Definitions

  • the field of innovation is the processing of plant matter containing aromatic, flavoring and/or medicinal compounds such as linear, mono and cyclic terpenes and cannabinoids and more particularly using freezing processes and freeze drying to separate undesired material to better extract and preserve the state of desired chemical compounds and constituents.
  • Cannabis plants such as hemp, with less than 0.3% THC (tetrahydrocannabinol) by dry weight, are particularly rich in the cannabinoid compound CBD (cannabidiol) which has known therapeutic properties for the treatment of medical conditions.
  • THC tetrahydrocannabinol
  • CBD cannabinoid compound
  • Hemp and other Cannabis plants may also contain other cannabinoids such as THC-A (tetrahydrocannabinolic acid),), CBN (cannabinol), CBG (cannabigerol), CBC (cannabichromene), CBDA (cannabidiolic acid), CBL (cannabicyclol), CBV (cannabivarin), THCV (tetrahydrocannabivarin), THCP (tetrahydrocannabiphorol), CBDV (cannabidivarin), CBCV (cannabichromevarin), CBGV (cannabigerovarin), CBGM (cannabigerol monomethyl ether), CBE (cannabielsoin) and CBT (cannabicitran).
  • THC-A tetrahydrocannabinolic acid
  • CBN cannannabinol
  • CBG canannabigerol
  • CBC cannabichromene
  • CBDA canannabidiolic acid
  • CBL cannabi
  • Hemp and other Cannabis plants also contain varying amounts of linear and cyclic terpene and terpinoids that are based on number of isoprene units, such as myrcene, limonene, linalool, a-pinene, b- caryophyllene, terpinolene, eucalyptol, humulene, nerolidol, ocimene, a- bisabolol and the like.
  • the medicinal and recreational benefits derived from Cannabis consumption varies with different strains and is believed to be the result of the synergy between the various cannabinoids and the terpenes, which vary among strains.
  • Cannabis plants are traditionally dried after harvest. During the 14-30 days it takes the cannabis plant to dry, the enzymes that cause plant senescence deteriorate as they act on the chlorophyll The drying is preferably at least these 14-30 days to the chlorophyll is eliminated to remove the “green” or grassy taste when the product is consumed by smoking.
  • THC-A undergoes decarboxylation, converting it into the psychoactive compounds A9 THC, & CBN. It is believed these, and possibly other cannabinoids are responsible for making users feel drowsy or lethargic. Linear terpene compounds are also lost in conventional drying.
  • a first object is achieved by providing process for freeze drying of plant matter that comprises the steps of freezing the plant matter with a liquid freezing agent at atmospheric pressure to one of fragment undesired plant matter and dislodge desired plant matter such that desired plant matter remains on a sieving member, with the fragmented plant matter passing through the sieving member, removing the desired plant matter from the sieving member while frozen, providing one of a storage and a vacuum chamber that is prechilled to receive the desired frozen plant matter from the sieving member, introducing the desired plant matter to the pre-chilled vacuum chamber, reducing the pressure in the vacuum chamber for a predetermined amount of time to sublime frozen water in the plant matter under a pressure not lower than 500 mTorr and below at least 1500 mTorr, maintaining the plant matter at temperature below about 32 °F (0 °C) until the pressure in the vacuum chamber is reduced to below at least about below at least 1500 mTorr, raising the temperature of the plant matter in the vacuum chamber to 69 °F (2
  • FIG. 1 Another aspect of the innovations is characterized by any such process for freeze drying of plant matter in in which the vacuum chamber has a bleed valve that is operatively connected to the controller to be modulated between an at least partially open position and a closed position to maintain a pressure in the vacuum chamber not lower than 500 mTorr and below at least 1500 mTorr.
  • FIG. 1 Another aspect of the innovations is characterized by any such process for freeze drying of plant matter in which the plant matter is one of buds and flowers from a species of cannabis, hops and hemp.
  • Another aspect of the innovations is characterized by any such process for freeze drying of plant matter wherein the step of raising the temperature in the vacuum chamber to 69 °F (20.6 °C) is completed in 2 or more stages, in which at least one of the stages the temperature in the vacuum chamber is maintained below 32 °F (0 °C) for at least about 10 hours.
  • Another aspect of the innovations is characterized by any such process for freeze drying of plant matter wherein the step of raising the temperature in the vacuum chamber to 69 °F (20.6 °C) is completed in a plurality of stages in which the pressure is maintained below 900 mTorr in a first stage and above 900 mTorr in a second stage, in which the duration of the plurality of stages is at least about 18 hours.
  • Another aspect of the innovations is characterized by any such process for freeze drying of plant matter that further comprises a step of reacclimating the dehydrated plant matter after removal from the vacuum chamber by exposure to room temperature and atmospheric conditions until RH% at between about 5% and 10% and then sealing the dehydrated plant matter 10 in containers.
  • Another aspect of the innovations is characterized by any such process for freeze drying of plant matter in which the step of reducing the pressure in the vacuum refrigeration chamber for a pre-determined amount of time to sublime frozen water in the plant matter is under a pressure not lower than 500 mTorr and below at least about 1500 mTorr.
  • Another aspect of the innovations is characterized by any such process for freeze drying of plant matter in which the step of reducing the pressure in the vacuum refrigeration chamber for a pre-determined amount of time to sublime frozen water in plant matter is under a pressure not lower than 720 and not more than about 760 mTorr.
  • Another aspect of the innovations is a process for freeze drying of plant matter that comprises the steps providing frozen plant matter from one of the species of cannabis, hemp and hops, providing a vacuum chamber that is prechilled to receive the frozen plant matter, introducing the frozen plant matter to the pre-chilled vacuum chamber, reducing the pressure in the vacuum refrigeration chamber for a pre-determined amount of time to sublime frozen water in the frozen plant matter under a pressure not lower than 500 mTorr and below at least 1500 mTorr to maintain a temperature below about 32 °F (0 °C) for a time sufficient to reduce the %RH of the frozen plant matter to about 5% or less, raising the temperature in the vacuum chamber to 69 °F (20.6 °C), removing dehydrated plant matter from the vacuum chamber.
  • Another aspect of the innovations is such a process for freeze drying of plant matter in which the frozen plant matter is from the species Cannabis and the removed dehydrated plant matter comprises essentially THC-A and is essentially free of delta 9 THC.
  • Another aspect of the innovations is any such process for freeze drying of plant matter wherein the step of raising the temperature in the vacuum chamber to 69 °F (20.6 °C) is completed in 2 or more stages, in which in at least one stage the temperature in the vacuum chamber is maintained below 32 °F (0 °C) for at least 10 hours.
  • Another aspect of the innovations is any such process for freeze drying of plant matter wherein the step of raising the temperature in the vacuum chamber to 69 °F (20.6 °C) is completed in a plurality of stages in which the pressure is maintained below about 900 mTorr in a first stage and above 900 mTorr in a second stage, in which the plurality of stages have a total duration of at least about 18 hours.
  • Another aspect of the innovations is any such process for freeze drying of plant matter in which the vacuum chamber that prechilled to -25 °F (-88 °C) or less before said step of introducing the frozen plant matter to the pre-chilled vacuum chamber.
  • Another aspect of the innovations is any such process for freeze drying of plant matter in which the step of reducing the pressure in the vacuum refrigeration chamber for a pre-determined amount of time to sublime the frozen water in the plant matter is under a pressure not lower than 500 mTorr and below at least about 1500 mTorr.
  • Another aspect of the innovations is any such process for freeze drying of plant matter in which the step of reducing the pressure in the vacuum refrigeration chamber for a pre-determined amount of time to sublime the frozen water in the plant matter is under a pressure not lower than 720 and not more than about 760 mTorr.
  • an apparatus for freeze drying that comprises a vacuum chamber, a refrigerant system configured in thermal communication with the vacuum chamber for reducing the temperature thereof, a heating system configured to raise the temperature within selected portion of the vacuum chamber to raise the temperature of one or more trays for containing plant matter, a vacuum pump in fluid communication with the vacuum chamber, a pressure sensor configured to measure the vacuum within one of the vacuum chamber and between the vacuum chamber and the vacuum pump, a relative humidity sensor configured for making proximal contact for matter to be freeze dried within the vacuum chamber, a first temperature sensor for configured for making proximal contact with plant matter to be freeze dried within the vacuum chamber, a second first temperature sensor for configured for being in thermal communication with an interior portion of the vacuum chamber that is remote from the plant matter to be freeze dried within the vacuum chamber, a controller that is operative to energize and de-energize the vacuum pump, heating systems and refrigerant system in response to signals received from the pressure sensor, relative humidity sensor, first and second temperature sensors.
  • FIG. 1 Another aspect of the innovations is such an apparatus for freeze drying further comprising a bleed valve that is operatively connected to the controller that is programmed to modulate the valve between an at least partially open and closed position to maintain a vacuum chamber pressure not lower than 500 mTorr and below at least 1500 mTorr when the refrigerant system and heating system are energized.
  • a bleed valve that is operatively connected to the controller that is programmed to modulate the valve between an at least partially open and closed position to maintain a vacuum chamber pressure not lower than 500 mTorr and below at least 1500 mTorr when the refrigerant system and heating system are energized.
  • Another aspect of the innovations is such an apparatus for freeze drying in which the controller is programmed to raise the temperature of plant matter in the vacuum chamber by energizing the heating system in 2 or more stages, in which at least one stage the temperature of the plant matter is maintained below 32 °F (0 °C) for at least 10 hours.
  • Another aspect of the innovations is such an apparatus for freeze drying in which the controller is programmed to maintain the pressure in the vacuum chamber for one of a pre-determined amount of time and until the RH% of the plant matter is below at about 10% during which frozen water in plant matter is sublimed at vacuum chamber pressure not lower than about 720 mTorr and not more than about 760 mTorr.
  • FIG. 1 is a schematic diagram of an apparatus for carrying out various aspects of the innovative processes.
  • FIG. 2 is a schematic diagram of another embodiment of an apparatus for carrying out various aspects of the innovative processes.
  • FIG. 3 is a flow chart of one embodiment of the innovative processes.
  • FIG. 4 is a flow chart of another embodiment of the innovative processes.
  • FIG. 5A and 5B are timing diagram showing temperatures and pressure stages in one implementation of the freeze-drying process.
  • FIG. 6 is a timing diagram showing temperatures and pressure stages in another implementation of the freeze-drying process.
  • FIG. 7 is a timing diagram showing temperatures and pressure stages in another implementation of the freeze-drying process.
  • a process 1000 for freeze drying of plant matter comprises the steps of freezing the plant matter with a liquid freezing agent at atmospheric pressure, removing a desired portion of the frozen plant matter to a vacuum refrigeration chamber 121, reducing the pressure in the vacuum refrigeration chamber for a pre-determined amount of time to sublime frozen water in the plant matter under a pressure not lower than 500 mTorr, and not higher than 1500 mTorr, while raising the temperature in the vacuum chamber before gradually venting when excess water is removed to provide a stable dehydrated plant product.
  • the liquid freezing agent is preferably inert, such as liquid nitrogen, liquid carbon dioxide (CO2) or any other inert or noble gas.
  • benefits of the innovative apparatus and process are preserving a greater amount of the native cannabinoids and terpenes including THC, CBD, CBN, CBG & CBC among others, than any other drying method.
  • Another benefit is that the freeze-dried plant matter is stable and additional processes may then be deployed to separate linear or mono-terpenes from polycyclic plant terpenes and terpenoids, such as cannabinoids, or distinct species of cannabinoids from each other.
  • Cannabis plants are hung up after harvest to dry in air 14-30 days. During this drying process the plant enzymes that cause plant senescence deteriorate as they slowly degrade the chlorophyll. The full removal of chlorophyll is necessary to remove the “green” or grassy taste when the product is consumed by smoking. However, as moisture is removed slowly, the drying plants can still be attacked by fungus or molds.
  • the basic principle of freeze-drying cannabis, hemp or other plants is the removal of water from plant matter 10 as water vapor through sublimation of frozen ice crystals or otherwise bound water molecules. With the biomass or plant matter 10 solidly frozen during the process, and under a deep vacuum, shrinkage is eliminated, and near perfect preservation of the bud and flower shape and appearance can be achieved. This process is also known as lyophilization.
  • the innovative apparatus 100 and process 1000 can be used to separate, and freeze dry a wide range and type of materials.
  • Many plant and herb species have the highest concentrations of terpene and cyclic terpene compounds with aromatic and medicinal properties in the flowering portions of the plant, and in particular in glandular or secreting trichomes.
  • the flowers typically form at the tips of growing plant shoots.
  • the flowers, flower buds and leaves have hair like outgrowths that are referred to as trichomes.
  • These trichomes being glandular secrete plant resins as a small bulb or head at the end of a stalk like hair.
  • the various embodiments of the process 1000 are particularly useful for processing hemp and cannabis plants that contain both linear terpenes and cyclic terpenes in the form of cannabinoids and is likely beneficial in processing other plants with a high concentration of trichomes in the flowers or buds, such as hop plants, in which the flowers and buds contain important flavoring compounds for beer brewing.
  • the various embodiments of the process 1000 are also useful in removing water from plant matter 10 that is primarily the trichomes that contain the highest concentration of terpene and cyclic terpene compounds, which depending on the plant species, such as by mechanical agitation with or without ciyo-processing.
  • Another object of the innovations is to rapidly process the buds and flowers in a manner that produces a shelf stable product of high quality, preserving color, flavor and aroma, as well as the desired chemical species.
  • the tips of growing plants that are beginning the flowering process may have multiple flower buds or flower interspersed with fine leaves. These fine leaves are known as bracts and bracteoles.
  • the flower region may contain multiple buds, also known as calyxes, as well as pistils, seeds, bracts and bracteoles.
  • the bracts and bracteoles in Cannabis are referred to as sugar leaves.
  • a preferred way to process cannabis, hemp, hops and other plants to remove plant matter, such as sugar leaves, that does not contain significant trichome content is to rapidly freeze freshly harvested plants, using an inert freezing agent like liquid CO2 or liquid nitrogen, as in the patented Cryo-TrimTM process which is disclosed in commonly owned US Patent No. 10,507,223B2 and 10,512,938B2, which are incorporated herein by reference, which is may deploy an apparatus referred to herein as a rotary separation apparatus 110.
  • the innovative apparatus 100 is the rotary separation apparatus 110 used in conjunction with the freeze-drying system 120.
  • the freeze-drying system 120 of FIG. 1 and 2 deploys a vacuum chamber 121 for receiving the product of the rotary separation apparatus 110.
  • the temperature in the vacuum chamber 12 l is reduced by a refrigerant system 122.
  • the refrigerant system 122 and the vacuum pump 123 are energized by a controller 124 that is preferably responsive to one or more of the pressure sensors 125, one or more temperature sensors 126 and preferably a relative humidity (RH) sensor 127 in the vacuum chamber 121 that is in proximal contact with the plant matter 10 during the drying process.
  • RH relative humidity
  • the vacuum chamber 121 preferably includes internal and or external insulation between the portions cooled directly or indirectly by the refrigeration system 112, such as outside a jacket circulating refrigerant fluid or inside or outside of a glass or transparent door on the vacuum chamber 121.
  • the vacuum chamber also has at least one vent port to admit air when the process is completed and may include a drainage port or line to remove water from the melting ice that build up inside the chamber interior walls that are in thermal communication with the circulating refrigerant.
  • a drain line may not be required.
  • the controller 124 is optionally a microprocessor, programmable logic controller or similar computing device that can be configured to be operative in response to a program in which the controller 124 receives signals from the pressure sensor 125, temperature sensor 126P, temperature sensor 126S and RH sensor 127 and either proportionally or discretely energizes and deenergizes the refrigeration system 122, at least one vacuum pump(s) 123 and a heater system 122b to provide the conditions of pressure and temperature indicated in FIG. 5 A to FIG. 7, and as otherwise described herein, as well as the optional bleed valve 129.
  • the pressure sensor 125 may be in direct fluid communication with the vacuum chamber 121 or a conduit forming the fluid communication between the vacuum pump(s) 123 and the vacuum chamber 121.
  • the heating elements of the heating system 122b are ideally dispersed to be proximal to the shelves 131 or shelf brackets 131 to gradually warm the trays 132, rather than heat the vacuum chamber 121 interior walls which are cooled by a circulating refrigerant from the refrigeration system 122.
  • the controller program may provide proportional control via a proportional-integral-derivative (PID) control scheme, a proportional-derivative (PD) control scheme, and the like.
  • PID proportional-integral-derivative
  • PD proportional-derivative
  • a non-limiting example of a device having a sensor to measure the RH% of the plant matter 10 directly during the process is the Elitech GSP-6 Temperature and Humidity Data Logger Recorder, which is available from Elitech Corp, of 1551 McCarthy Boulevard, Suite 112, Milpitas, CA.
  • the controller 124 may also include a memory module, user interface and output module or datalogger to record the actual process conditions and is energized by an external power source. Thus, the controller 124 is operative to switch and modulate power from an external source to the refrigeration system 122, vacuum pump(s) 123 and chamber heater system 122b.
  • the controller 124 may deploy a bus architecture in which the signal from the pressure sensor 125, temperature sensor 126P, temperature sensor 126S and RH sensor 127 are sent to the controller bus 124b and the same or another controller bus or subcomponent modulates the energy to the refrigeration system 122, vacuum pump(s) 123 and chamber heater system 122b.
  • FIG. 2 a more preferred apparatus 1000 is illustrated in FIG. 2.
  • the controller 124 is operative to modulate the condition of a bleed valve 129 to the vacuum chamber 121, which using the output of pressure sensor 125 is deployed to keep the pressure within pre-determined control limits in the process 1000, as illustrated by a flow chart in FIG. 3, at step 1040.
  • the plant matter is frozen in step 1010 before a physical separation in step 1020, which removes by size and/or density filtration undesired leave and other plant matter, such as sugar leaves, that fragments in the rotary separation apparatus 110.
  • the physical separation in step 1020 optionally uses the aforementioned rotary separation apparatus 110, but may use equivalents thereto, including those described in the US Patent No’s 10,507,223B2 and 10,512,938B2.
  • the desired plant matter 10 usually the flower and buds that are rich in trichome containing aromatic compounds, are then removed while still below about 32 °F (0 °C)(so the water content is still frozen) placed in the pre-chilled vacuum chamber 121 that is preferably at about -25 °F (-88 °C) (step 1030).
  • the frozen plant matter 10 can be obtained in the process illustrated in FIG. 4 in step 1025, and then placed in the pre-chilled vacuum chamber 121 that is preferably at about -25 °F (-88 °C) (step 1030).
  • the vacuum pump 123 is energized by the controller 124 to reduce the pressure in the vacuum chamber 121 to within control limits of greater than about 500 mTorr (milliTorr) to less than about 1500 mTorr. More preferably, when presented with equipment limitations, these limits are between about 720 mTorr to 760 mTorr in step 1040.
  • FIG. 1 illustrates a configuration in which a first temperature sensor 126P has a probe imbedded in the plant matter 10.
  • a second temperature sensor 126S uses a probe that measures the vacuum chamber temperature with a probe in thermal communication with a portion of the vacuum chamber distal from the plant matter 10, such as a shelf 131 in the vacuum chamber 121 or the chamber interior wall.
  • Plant matter 10 is also disposed on at least one shelf 131, but the probe of thermal sensor 1261 S is placed on a portion of such a shelf 131 remote from the plant matter 10. It should be understood that if the plant matter 10 is not immediately placed in such a pre-chilled vacuum chamber 121 after it is frozen in a prior process step, such as for separation of trichomes or removal of sugar leaves from buds and flowers, the plant matter 10 is preferably stored in freezers below about 0 0 F ( -17.8 °C) before the start of the dehydration in the pre-chilled vacuum chamber 121.
  • FIG. 5 A to 7 illustrate alternative implementations of the vacuum chamber
  • step 1070 the freeze-dried plant matter 10 removed from the vacuum chamber 121 is not so dry as to be unacceptably fragile or friable from under drying in which the plant structure collapses and re-absorbs excessive moisture that can produce spoilage. It has been discovered that when the product at step 1070 have more than 0% RH up to about 5% RH it is most suitable for the acclimation step 1080.
  • the final acclimation step 1080 before packaging is to reacclimatize the freeze-dried product to a stable state. It should be noted that as a preferred aspect of the apparatus 100 and/or process 1000 may deploy the Cryo-TrimTM process or an equivalent, the cell walls in the flower and buds are already disrupted by the growth of ice crystals in freshly harvested plants. This allows the biomass or plant matter 10 to absorb more moisture from the air, unless kept cold until introduced into the chilled vacuum chamber 121 of the freeze dryer 120.
  • the temperature is increased in steps while the pressure in the vacuum chamber 121 is maintained at between about 720-760 mTorr. During about the first 12 hours the temperature is at or below the freezing point of water ( 32 °F (0 °C) or zero degrees C) so that ice crystal are sublimed before the temperature is raised upward either gradually (dashed line in FIG.
  • the plant matter 10 in the vacuum chamber 121 then reaches a conditions when it has a RH% of 0 to 5%.
  • This RH% is usually reached when the chamber temperature, as measured by the temperature sensor 126S with the associated probe thereof in thermal communication or contact with internal components like shelves 131, is the same as the temperature sensor 126P with the probe thereof contacting the plant matter 10 to be dehydrated.
  • an RH meter can be contacting the plant matter 10 to be dehydrated as an additional means to monitor the progress of de-hydration process. It is also preferable to also use an RH meter to test the dehydrated plant matter 10 before packaging.
  • the pressure is raised in stage from generally not less than about 500 mTorr, but more preferably greater than about 720 mTorr, while the product is rapidly brought to about 69 °F (20.6 °C)when this initial pressure is reached.
  • the plant product temperature as measure by a probe of thermal sensor 126S remains at a temperature well below the freezing point of water until the ice crystal are sublimed.
  • the pressure can be raised to about 1300-1400 mTorr for the remaining 6 to 10 hours, for a total elapsed time of 18 to 24 hours.
  • the vacuum chamber 121 may be fully vented to atmosphere to remove the dried plant product 10, which then has an RH% is then usually greater than 0 up to about 5%.
  • Suitable freeze dryers can be obtained from Harvest Right, 95 North Foxboro Drive, Ste. 100, North Salt Lake, UT 84054. Alternative configurations of freeze dryers may be used, but preferably deploy in the vacuums system an oil free scroll pump.
  • the pressure is initially brought to and maintained at about 1,200 mTorr with an initial rise of the chamber temperature from about -25 °F (-88 °C)to about 105 °F, which is preferably as fast at the freeze drying system 120 will permits without overshoot in temperature and/or pressure and then maintaining at this temperature for about 6 hours. Then the temperature of the vacuum chamber 121 is gradually reduced to about 69 °F (20.6 °C)over the next 6 hours, for a total 12 hours.
  • the thermal sensor 126P with the probe thereof in contact or thermal communication with the frozen plant matter 10 remains at a temperature well below the freezing point of water until the ice crystals are sublimed. During the remaining hours the residual moisture that is absorbed in the plant matter 10 and not in the form of ice crystals is gradually removed.
  • the vacuum chamber 121 may then be fully vented to atmosphere to remove the product, as the RH% is then usually greater than 0 up to about 5%.
  • steps 1040, 1050 and 1060 as illustrated in FIG. 6 and FIG. 7 is more suitable for commercial freeze-drying equipment in which one or more vacuum pumps 123 and refrigeration system 122 are of adequate capacity and sufficiently stable to readily for the controller 124 to maintain a pressure within the chamber of between about 500 to 1500 mTorr, but more preferably 720 to 760 mTorr.
  • the implementation of FIG. 5A and 5B may be used with less capable equipment if provided with the bleed valve 129 or its equivalent to maintain the vacuum level at the more preferred range of 720 to 760 mTorr as the temperature is gradually raised in steps or the equivalent, such as a gradual rise or increase.
  • FIG. 5A and 5B may be used with less capable equipment if provided with the bleed valve 129 or its equivalent to maintain the vacuum level at the more preferred range of 720 to 760 mTorr as the temperature is gradually raised in steps or the equivalent, such as a gradual rise or increase.
  • the controller 124 is operative to open the bleed valve 129 to admit outside air in the vacuum chamber 121 at low rates to maintain the pressure about a lower limit and close the bleed valve 129 when the pressure is reaching or about to overshoot an upper control limit.
  • This additional control required by the bleed valve 129 may be required because the rate of sublimation of frozen water, which raises the vacuum chamber pressure may be uneven or chaotic because of the nature of the plant matter and how it packs down on the shelves 131 in the freeze-drying process 1000.
  • the sublimation rates may also be uneven or chaotic because of capacity and control of the refrigerant system 122 or heating system 122b.

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  • General Engineering & Computer Science (AREA)
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Abstract

L'invention concerne un procédé de lyophilisation de matière végétale aromatique qui déploie un agent de congélation inerte pour fracturer une matière végétale indésirable en fragments plus petits destinés à une séparation physique à partir de bourgeons et de fleurs de plantes, qui sont riches en trichomes aromatiques. Les bourgeons et les fleurs congelés sont retirés des éléments de tamisage utilisés pour une séparation physique et maintenus à l'état congelé jusqu'à ce qu'ils soient introduits dans une chambre sous vide pré-refroidie d'un système de lyophilisation. L'appareil de lyophilisation est conçu et déployé dans un procédé qui maintient la pression au-dessus de 500 mTorr mais en-dessous de 1500 mTorr pour réduire la teneur en humidité des plantes pour fournir un produit stable.
PCT/US2021/072363 2020-11-11 2021-11-11 Lyophilisation de matière végétale aromatique WO2022104360A1 (fr)

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US18/252,530 US20240118026A1 (en) 2020-11-11 2021-11-11 Freeze Drying Aromatic Plant Matter

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US202063113346P 2020-11-13 2020-11-13
US63/113,346 2020-11-13

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7919294B2 (en) * 2001-03-12 2011-04-05 Biotools Biotechnological & Medical Laboratories, S.A. Process for preparing stabilized reaction mixtures which are partially dried, comprising at least one enzyme, reaction mixtures and kits containing said mixtures
KR101594045B1 (ko) * 2009-07-20 2016-02-15 해팅턴 비즈니스 에스, 엘. 식물 시클라멘 에우로파에움 엘.의 동결-건조 분리된 추출물을 수득하는 방법 및 치료제로서의 이의 용도
US20190083558A1 (en) * 2016-07-06 2019-03-21 The Original Resinator Llc Rotary Separation Apparatus and Process
US20190285341A1 (en) * 2018-03-14 2019-09-19 Sp Industries, Inc. Means and methods for selective shelf temperature control
WO2020123000A2 (fr) * 2018-09-12 2020-06-18 University Of Florida Research Foundation, Inc. Injecteur de carburant pour fonctionnement de moteur à réaction hypersonique

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7919294B2 (en) * 2001-03-12 2011-04-05 Biotools Biotechnological & Medical Laboratories, S.A. Process for preparing stabilized reaction mixtures which are partially dried, comprising at least one enzyme, reaction mixtures and kits containing said mixtures
KR101594045B1 (ko) * 2009-07-20 2016-02-15 해팅턴 비즈니스 에스, 엘. 식물 시클라멘 에우로파에움 엘.의 동결-건조 분리된 추출물을 수득하는 방법 및 치료제로서의 이의 용도
US20190083558A1 (en) * 2016-07-06 2019-03-21 The Original Resinator Llc Rotary Separation Apparatus and Process
US20190285341A1 (en) * 2018-03-14 2019-09-19 Sp Industries, Inc. Means and methods for selective shelf temperature control
WO2020123000A2 (fr) * 2018-09-12 2020-06-18 University Of Florida Research Foundation, Inc. Injecteur de carburant pour fonctionnement de moteur à réaction hypersonique

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