• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
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    • 专利摘要:
    The raw cannabis plant material is mixed with ethanol and centrifuged to extract cannabinoids. Ethanol can be cooled before adding it to the raw cannabis plant material, and a non-polar solvent stage can be used to increase the extraction yield. The crude oil and ethanol resulting from the dissolved cannabinoids are separated from the raw cannabis plant material and filtered to remove particulate materials, waxes, lipids, dissolved fats and impurities. The ethanol is then evaporated from the resulting mixture of oil and ethanol, and the remaining oil is then washed with saline, decarboxylated and distilled to obtain the cannabinoids and other desirable volatile phytochemicals.
    公开号:BR112019026417B1
    申请号:R112019026417-5
    申请日:2018-09-07
    公开日:2020-12-01
    发明作者:Ryan Delmoral Ko；Brock Hughes；Krupal Devendra Pal；Alexzander Samuelsson
    申请人:Nextleaf Solutions Ltd；
    IPC主号:
    专利说明:

    Technical Field
    [001] This application concerns the extraction of cannabinoids from raw cannabis plant material. More specifically, it refers to the extraction of cannabinoids using an ethanol-based method that includes washing the extracted oil with saline. Background
    [002] In the legal adult markets, sales of extracts are growing ten times faster compared to sales of dry cannabis, and extracts represent more than 60% of revenue. With legalization, consumer preferences are shifting from dry cannabis to extracted cannabis products.
    [003] However, the aroma and flavors of cannabis can be undesirable in many products infused due to the excess of lipids, plant matter and impurities present in the extracts currently available.
    [004] US patent 9,155,767 to Hospodor et al. refers to the extraction of medicinal cannabis compounds in an eluate, separating a portion of medicinal cannabis compounds contained in an eluate portion at a first target level of extraction, to provide sufficient clean solvent to continue extraction operations. A high-efficiency concentrator process elutes from one or more tanks, creating a clean solvent when extraction objectives are achieved or when the clean solvent is exhausted. This manages the eluate concentration levels and limits the amount of medicinal cannabis compounds concentrated on the spot at any time.
    [005] US patent 7,700,368 to Flockhart et al. refers to the purification of cannabinoid oil from plant material. The high degree of purity for the final cannabinoid oil extract is achieved using a combination of chromatography techniques and different types of solvent to prepare the cannabinoid oil extract and remove any insoluble impurities from it.
    [006] This background information is provided to reveal information considered by the depositor to be of possible relevance to the present invention. No admission is necessarily intended, nor should it be interpreted, that any of the foregoing information constitutes state of the art against the present invention. Brief Description of the Invention
    [007] The present invention is directed to the extraction of cannabinoids from plant material. In particular, it relates to the mixing of dried and ground cannabis plants with ethanol in a centrifugal washing and drying apparatus (WSD), followed by filtration, ethanol evaporation, washing with saline, decarboxylation and distillation.
    [008] Here is disclosed a process for extracting cannabinoids from raw cannabis plant material, comprising the steps of: adding ethanol to the dry and ground cannabis plant material to form an initial mixture; centrifuge the initial mixture to separate a mixture of crude oil and ethanol from the initial mixture; treating the mixture of crude oil and ethanol with medium to remove unwanted components from it; evaporating the ethanol from the mixture of crude oil and treated ethanol to leave the oil; wash the oil with saline solution; decarboxylating the oil washed with saline to form decarboxylated oil; and distill the decarboxylated oil to obtain cannabinoids. Brief Description of Drawings
    [009] The following drawings illustrate embodiments of the invention, which should not be construed as restricting the scope of the invention in any way.
    [010] Figure 1 is a high level flow chart showing the main steps of a process for extracting cannabinoids according to an embodiment of the present invention.
    [011] Figure 2 is a flow chart showing more detailed steps of a process for extracting cannabinoids according to an embodiment of the present invention.
    [012] Figure 3 is a schematic diagram of the apparatus used for the extraction of cannabinoids according to an embodiment of the present invention.
    [013] Figure 4 is a high level flow chart showing the main steps of a process for extracting cannabinoids according to another embodiment of the present invention.
    [014] Figure 5 is a flow chart showing more detailed steps of a process for extracting cannabinoids according to a further embodiment of the present invention.
    [015] Figures 6A-B show a schematic diagram of the apparatus used for the extraction of cannabinoids according to a further embodiment of the present invention. description A. Glossary
    [016] Cannabidiol (CBD) is one of the active cannabinoids found in cannabis and is used for medicinal purposes.
    [017] Cannabinoid mimetics are phytochemicals that act on cannabinoid receptors in the body, but are not derived from the cannabis plant nor are they strictly classified as cannabinoids.
    [018] Cannabinoids are a group of chemicals that act on cannabinoid receptors in the body, many of which are found in the cannabis plant.
    [019] Crude oil is a term for the description of unfiltered condensed oil, that is, oil that is not winter and is not treated by charcoal, clay and silica. Crude oil contains cannabinoids.
    [020] Tetrahydrocannabinol (THC) is a psychotropic cannabinoid and is the main psychoactive ingredient in cannabis. THC also has medicinal uses. THCa is the non-psychoactive form of THC.
    [021] WSD separator (washing and drying by centrifugation) - a solvent-based extraction system / centrifuge drum used to extract botanical compounds from different plant species. The device provides a process in which the plant material is first washed or stirred in solvent and then dried by centrifugation to separate the solvent loaded with extract from the residual biomass. Shaking includes turning the drum back and forth, for example.
    [022] Rotovap - a rotary evaporator.
    [023] Preparation for winter use refers to cooling oil to precipitate and remove unwanted fats, waxes and lipids from plants through cooling and filtration. B. Overview
    [024] With reference to Figure 1, a flow chart of the basic steps of the process is shown. In step 10, a solvent, such as ethanol, is added to the dried cannabis plant material and ground under pressure. Ethanol can be at room temperature or cooled. As a result, cannabinoids found in plant material dissolve in ethanol. In step 12, the ethanol solution is drained from the plant material to form a mixture of crude oil and ethanol. The first two stages are considered the primary extraction stage.
    [025] In step 14, impurities are then removed by treating the mixture medium of crude oil and ethanol, which contains cannabinoids. In step 16, ethanol is removed or recovered from the mixture, by evaporation, for example. Steps 14 and 16 are considered the solvent recovery stage.
    [026] In step 18, the oil remaining after evaporation is decarboxylated to activate THC. Decarboxylation converts THCa to THC; the process activates THC by separating the acid component from THCa, the acid form of cannabinoid, converting it to THC, the neutral form, by heating to remove the carboxylic acid group and release carbon dioxide. The residue after decarboxylation is then, in step 20, distilled using a film cleaning apparatus to extract the cannabinoids. C. Exemplary Process
    [027] With reference to Figure 2, a detailed process for the extraction of cannabinoids is shown. This exemplary process refers to the extraction of cannabinoids from cannabis plant material.
    [028] Steps 100-123 refer to the primary extraction phase. Steps 124-138 refer to the treatment stage of the adsorbent medium. The rotovap stage 160 forms the solvent recovery phase. Step 165 refers to the decarboxylation stage and steps 170-180 refer to the distillation of cannabinoids.
    [029] In step 100, raw cannabis plant material is supplied. The raw cannabis plant material includes, for example, the flower, the leaves and the stems next to the leaves. Any part of the plant that contains cannabinoid resin glands can be included. Not all stems and leaves have these glands present. In other cases, the raw cannabis plant material includes only the flowers, or the raw cannabis plant material includes only the leaves and stems, that is, the parts of the plant that would normally be considered waste, in which valuable phytochemicals are found only in lower concentrations.
    [030] In step 105, the raw cannabis plant material is dried, if not already supplied in dry form. The raw cannabis plant material is dried in a dry room with a dehumidifying air controller, or can be dried instantly in a vacuum oven at a pressure <2kPa. Ideally, the moisture content of the raw cannabis plant material after drying is 10% or less by weight. The temperature of the oven and the drying time depend on how much moisture the raw material has and how much raw material there is. The moisture content is measured using a moisture analyzer. In some embodiments, a hygrometer can be used. The lower the moisture content, the better, because less moisture will cause less dilution of ethanol than if the moisture level were higher. If the ethanol that is recovered is diluted with water, it will be less effective for repeated processes. However, in other embodiments, the moisture content can be as high as 15% while still allowing for an acceptable process. In other embodiments, other drying techniques can be used.
    [031] In step 110, the dry plant material is ground, for example, to an average size between 250-300 μm. However, in other embodiments, it is possible to grind the dry plant material to a size of thousands of microns, and it has been found that the process works with average particle sizes of up to 3000 to 5000 μm. If the plant material is ground to less than 250 μm, say, there will be problems with the unwanted packaging of the material in the material columns (240, Figure 3). Notably, the unwanted packaging is due to the packaging of the raw material in a buffer under applied pressure. If the particulate material is too fine, the raw material will form an apparently solid mass, making it difficult for ethanol to pass through it.
    [032] Note that, in other embodiments, the grinding step can occur before the drying step.
    [033] In step 112, ethanol is cooled to a temperature between -35 ° C and -50 ° C, in a tank surrounded by a pressurized liquid CO2 jacket, for example. In other embodiments, the ethanol is cooled using a heat exchanger or a jacket of solid CO2 or liquid nitrogen.
    [034] In step 115, the cooled ethanol is added to the material column on which the ground and dried vegetable material was placed. Typically, approximately 50 liters of ethanol are used for every 5 kg of plant material, although it is possible that other proportions can be used.
    [035] In some embodiments in which ethanol is cooled, the ideal temperature has been found to be -45 ° C. However, the ideal temperature can be different in other embodiments. The ideal choice is an agreement between keeping the time needed to cool down to a minimum, keeping the consumption of liquid nitrogen and / or liquid CO2 soda low and maximizing the miscibility of ethanol with the cannabinoids to be extracted. However, using the treatment and filtration process described here, fats and lipids can be economically removed from the mixture extracted from crude oil and ethanol. The use of cooled ethanol is more efficient for the process in general in relation to the post-filtration steps, however, it presents a little less efficiency in relation to the yield. Uncooled ethanol is more efficient in terms of extraction yield, but very inefficient for post-filtration steps. Uncooled ethanol extracts unwanted fats, waxes and lipids. In some embodiments, step 112 is optional and the extraction process takes place with ethanol cooled or at room temperature, that is, in the range of -60 ° C to +18 ° C.
    [036] In step 118, the mixture of ethanol and plant material is pressurized to a pressure in the range of 70 to 280 kPa (10 to 40 psi). The goal is to select a pressure that is low enough to prevent the formation of a plug of plant material within the column of materials. The actual pressure value is determined by the packaging of the material column. The tighter the raw cannabis plant material is packed in the column, the lower the upper pressure limit with which ethanol can be conducted through the column. While under pressure, the temperature of the mixture can vary up to ± 5 ° C, but should not be allowed to rise above -35 ° C. Note that, in some embodiments, pressure is applied to the mixture of ethanol and plant material by centrifugal action.
    [037] In step 120, the plant material is allowed to immerse in ethanol for a while, in order to allow cannabinoids to dissolve in it. Normally, the plant material immerses for up to 15 minutes, as long as the temperature is below -35 ° C. In other embodiments, the immersion time may be different. The pressure is maintained in the range of 70 to 280 kPa (10 to 40 psi) while the mixture of ethanol and plant material is immersed.
    [038] In step 122, ethanol, now with crude oil and cannabinoids dissolved, is drained from the volume of the plant material, to form a mixture of crude oil and ethanol. This mixture is the total fluid that comes directly from the extractor (material column) after extraction. The crude oil contains cannabinoids and other phyto-compounds and is dissolved in ethanol. The mixture also contains some unwanted residual plant materials and other undesirable components. The mixture of crude oil and ethanol is drained under a pressure in the range of 70 to 280 kPa (10 to 40 psi), that is, it is the same pressure as the pressure used to immerse the plant material. In other embodiments, a vacuum is used to drain the mixture of crude oil and ethanol instead of applying pressure.
    [039] In other embodiments, ethanol is pumped continuously through the raw cannabis plant material under pressure in the range of 70 to 280 kPa (10 to 40 psi), without the specific immersion step.
    [040] Optionally, in step 123, a centrifuge is used to separate the additional plant material from the mixture of crude oil and ethanol. The centrifuge can be used instead of step 122 of draining the material column or instead of pumping ethanol through the raw material under pressure. In this case, the contents of the material column are transferred directly to the centrifuge or to a mesh bag and then placed in the centrifuge.
    [041] In step 124, the mixture of crude oil and ethanol is heated to a temperature between 60 ° C and 78 ° C for treatment with charcoal. It is important not to exceed the upper temperature of this range, as the target elements in the crude oil will melt in a liquid state and cannot be filtered. In addition, ethanol will be boiling and cannabinoid degradation may occur. In other embodiments, it is possible to skip this step and perform the subsequent filtration steps at room temperature or even using the mixture of crude oil and ethanol in its previously cooled state, or at another refrigerated temperature, for example, as low as - 40 ° C.
    [042] In the following steps, the mixture of crude oil and ethanol is treated and filtered to remove more plant material that is inevitably retained in the mixture during the drainage step. Treatment and filtration remove fats, lipids, chlorophyll, waxes, heavy metals and other unwanted chemicals. There are usually 1 to 5 different medium treatments. Although filtration is almost always necessary, the necessary filtration steps are not necessarily as robust if the ethanol used in the primary extraction phase is cooled, compared to if the ethanol is not cooled.
    [043] In step 125, the mixture of crude oil and ethanol is treated with charcoal. Charcoal removes pigments, chlorophyll, heavy metals and particulate materials. Charcoal is used as the first treatment medium to remove as much pigment as possible. The charcoal, when in particulate form, is added first to the mixture of crude oil and ethanol heated, at room temperature or cooled, and then the mixture is stirred. The average size of the charcoal particles is in the range of 0.25 to 150 μm, although other sizes are possible in other embodiments.
    [044] The crude oil and ethanol mixture is then cooled or allowed to cool to a temperature between 10 and 50 ° C in step 127. Any charcoal that is in the crude oil and ethanol mixture is removed by filtering it using filter paper borosilicate glass, in step 128, particularly if it has been added to the mixture of crude oil and ethanol during the treatment process. The filtration of charcoal is carried out at a temperature between 10 and 50 ° C. Other filter media or materials, or a filter screen, can be used. For example, the solution is filtered through a 10 to 30 μm paper or mesh filter and then through a 0.25 to 1 μm paper or mesh filter. In other embodiments, a different number of paper or screen filters can be used and they can be of different sizes. In another example, a filter cartridge is used, with a pore size of 0.2 to 1 μm.
    [045] In step 129, the mixture of crude oil and ethanol is reheated to a temperature between 60 ° C and 78 ° C for further treatment. In other embodiments, it is possible to skip this step and perform the subsequent treatment and filtration steps at room temperature or even using the mixture of crude oil and ethanol in its previously cooled state or at another refrigerated temperature, for example, as low as -40 ° C.
    [046] In step 130, the mixture of crude oil and ethanol is treated with agulite clay, also known as fuller earth clay, paligorskite, atapulgite or bentonite. The clay mainly removes pigments. The clay, when in particulate form, is first added to the heated crude oil and ethanol mixture and then the mixture is stirred. The average size of the clay particles is in the range of 0.25 to 150 μm, although other sizes are possible in other embodiments.
    [047] The crude oil and ethanol mixture is then cooled or allowed to cool to a temperature between 10 and 50 ° C in step 132. Any clay that is in the crude oil and ethanol mixture is removed by filtering it in step 133, using borosilicate glass filter paper, particularly if it has been added to the mixture of crude oil and ethanol during the treatment process. Other filter media or materials, or a filter screen, can be used. For example, the solution is filtered through a 10 to 30 μm paper or mesh filter and then through a 0.25 to 1 μm paper or mesh filter. In other embodiments, a different number of paper or screen filters can be used and they can be of different sizes. In another example, a filter cartridge is used, with a pore size of 0.2 to 1 μm.
    [048] In step 134, the mixture of crude oil and ethanol is reheated to a temperature between 60 ° C and 78 ° C for further filtration. In other embodiments, it is possible to skip this step and perform the subsequent treatment and filtration steps at room temperature or even using the mixture of crude oil and ethanol in its previously cooled state, or at another refrigerated temperature, for example, as low -40 ° C.
    [049] In step 135, the mixture of crude oil and ethanol is then treated with silica. Silica removes very fine plant matter and other particulate materials. The silica, when in particulate form, is first added to the heated crude oil and ethanol mixture and then the mixture is stirred. The average size of the silica particles is in the range of 0.25 to 150 μm, although other sizes are possible in other embodiments. The removal of very fine solid particulate materials helps prepare for winter use of the oil to occur more quickly. In addition, it allows product visibility, which, in turn, allows you to review the integrity of the filtration process.
    [050] The crude oil and ethanol mixture is then cooled or allowed to cool to a temperature between 10 and 50 ° C in step 137. Any silica present in the crude oil and ethanol mixture is removed by filtering it in step 138, using paper borosilicate glass filter, especially if it has been added to the mixture of crude oil and ethanol during the treatment process. Other filter media or materials, or a filter screen, can be used. For example, the solution is filtered through a 10 to 30 μm paper or mesh filter and then through a 0.25 to 1 μm paper or mesh filter. In other embodiments, a different number of paper or screen filters can be used and they can be of different sizes. In another example, a filter cartridge is used, with a pore size of 0.2 to 1 μm.
    [051] In step 160, the resulting oil and ethanol mixture is then processed with a rotary evaporator to remove and recover any ethanol that remains in it. The rotary evaporator temperature is 43 to 49 ° C and is operated at a pressure of 83 to 101 kPa (25 to 30 inHg, 635 to 760 mmHg). Other evaporators can be used in other embodiments. The ethanol that is recovered can be used to extract cannabinoids from another batch of dry and ground raw cannabis plant material.
    [052] After removing the remaining ethanol using the rotary evaporator, decarboxylation is carried out on the resulting oil in step 165. The oil is heated to 120-140 ° C to evaporate residual solvents and convert THCa to THC, releasing CO2 in the process. If the temperature is below this range, there will potentially be some residual ethanol. Most of the CO2 that is produced from decarboxylation is removed to ensure consistent vacuum levels later in the process. If the temperature is above this range, product degradation will occur. The oil is heated gradually while stirring so as not to overheat parts of it. In the decarboxylation step, residual ethanol is not recovered. The decarboxylation process usually takes several hours. Note that in an embodiment described below, the decarboxylation step is not performed on a rotary evaporator, but on a clean film under vacuum, to decrease the required contact temperatures and prevent oxidation.
    [053] In step 170 and referring to Figure 3, the decarboxylated oil is passed through a 370 short path distillation film cleaning device. As we are using a clean film distillation process versus a conventional short path static device , it is important to separate the pre-distillation from waxes, fats and lipids.If this is not done, the waxes, fats and lipids will be cleaned in the cleaning film, causing some of these elements to distill into the final product.
    [054] The decarboxylated oil is first passed through the short path distillation film cleaner to remove some volatile terpenes. The temperature of the feed tank 365 for film cleaning is set in the range of 100 to 115 ° C and is more generally set in the range of 107 to 110 ° C. The temperatures of pump 366 and feed line 367 for cleaning film are set to the same value as the feed tank. The temperature of the waste discharge arm 390 and its associated pump, not shown, is also set in the range of 100 to 115 ° C and is also more generally set in the range of 107 to 110 ° C. The temperature of the target heater, which controls the temperature of the inner wall 372, is adjusted within a range of 155 to 162 ° C, usually 159.5 ° C. Condensing coil 376 is set at a temperature of 58 ° C, as well as the distillate or target discharge arm 380 and its associated pump (not shown). Another temperature control unit maintains the temperature of a cold trap between vacuum port 396 and the vacuum pump from -22 to -30 ° C, although even lower temperatures are possible. The film cleaning process is carried out at a pressure of 0.3 to 0.8 mbar or less.
    [055] In step 175, the residual oil, after removing volatile terpenes, is again passed through the short-path distillation film cleaner to remove some non-volatile terpenes. All temperatures are the same, except the temperature of the inner wall, which is normally set to a higher temperature and is in the range of 159 to 162 ° C. The pressure is the same, from 0.3 to 0.8 mbar or less.
    [056] In step 180, the additional residual oil is again passed through the short path distillation film cleaner to remove the cannabinoids as a whole. The temperature of the feed tank 365 for film cleaning is set in the range of 100 to 115 ° C and is more generally set in the range of 107 to 110 ° C. The temperatures of pump 366 and feed line 367 for cleaning film are set to the same value as the feed tank. The temperature of the waste discharge arm 390 and its associated pump, not shown, is also set in the range of 100 to 115 ° C and is also more generally set in the range of 107 to 110 ° C. The temperature of the target heater, which controls the temperature of the inner wall 372, is adjusted within a range of 168.5 to 170 ° C. Condensing coil 376 is set at a temperature of 74 ° C, as well as the distillate or target discharge arm 380 and its associated pump (not shown). The temperature of the cold trap between the vacuum port 396 and the vacuum pump is -22 to -30 ° C, although even lower temperatures are possible. The film cleaning process is carried out at a pressure of 0.03 to 0.08 mbar or less.
    [057] The result of the distillate discharge arm is a tasteless, odorless oil that contains up to 99% pure cannabinoids. Often, however, the additional residual oil will require another pass through the clean film apparatus in order to achieve purities of 90% or more.
    [058] Using this process, a certain weight of dry cannabis can be transformed into approximately 10 to 15% of crude oil, which produces approximately 4 to 10% of pure cannabinoids. D. Device
    [059] With reference to Figure 3, an example of the device is shown schematically. The raw cannabis plant material is supplied in a loading hopper 202, for example, and is released in batches in container 204. The raw cannabis plant material is vacuum dried 210. Then the dry plant material is placed in a grinder 220. After the grinding step, the ground vegetable material is placed in one or more columns of material 240. Each column has a lid 241 that is removable so that the ground vegetable material can be placed in it. Each column supports 1.5 to 4.5 kg (3 to 10 lb) of plant material, depending on its size. Other capacities are also possible. In an example device, there are four columns of material 240. The column of material can be surrounded by an insulating wall or vacuum liner 242, which can be evacuated through port 244. Alternatively, an insulating liner can be wrapped around the material column. Insulating wall 242 or jacket helps keep the content 246 cool in the process using cooled ethanol as the solvent. When using cooled ethanol, the material column is kept cool by the use of pressurized liquid CO2 in the jacket. Ethanol 250 is cooled in a cryogenic tank 260, the internal temperature of which is kept low by a jacket 262 filled with liquid CO2 pressurized through port 264. In other embodiments, other refrigerants can be used or a refrigerator or heat exchanger can be used. to be used.
    [060] Pressurized nitrogen gas is fed into port 272, forcing the cooled ethanol 250 through the insulated tube 274 in the 240 material column. The nitrogen pressure is used to maintain the pressure of the 246 mixture of ethanol and raw cannabis plant material. and / or to pump ethanol through raw cannabis plant material. After the raw cannabis plant material is immersed in ethanol, ethanol, now with dissolved cannabinoids, is drained from the material column 240 as a mixture of crude oil and ethanol, through outlet tube 276 into container 280. The volume of the raw cannabis plant material remains in the 240 material column. The mixture of crude oil and ethanol can alternately be pumped out of the material column under nitrogen pressure.
    [061] Optionally, a 290 centrifuge is used to separate the volume of plant material from the mixture. If the centrifuge 290 is used, the contents of the material column are emptied into the centrifuge, which then separates the volume of plant material from the mixture of crude oil and ethanol. The centrifuge 290 can be used instead of draining the material column, or instead of pumping ethanol through the raw material under pressure, or it can be used as well as the draining and / or pumping steps.
    [062] The mixture of crude oil and ethanol is then treated with various media and fed through several different filters sequentially. In this embodiment, the first treatment unit is charcoal 310. Below the charcoal, there is a filter 311 of 10 to 30 μm and a 312 filter from 0.25 to 1 μm to filter the charcoal. Then there is a clay treatment unit 314, below which there is a 315 filter from 10 to 30 μm and a filter 316 from 0.25 to 1 μm to filter the clay. The following is a silica treatment 318, below which there is a filter 319 of 10 to 30 μm and a filter 320 of 0.25 to 1 μm to filter the silica. Each of the filters can be replaced independently. After filtration, the resulting oil and ethanol mixture leaves the final filter through outlet tube 324 and is collected in container 328.
    [063] The filtered oil and ethanol mixture is then passed to a rotary evaporator 340. The oil and ethanol mixture 342 is kept at an elevated temperature in flask 346, which is heated in a temperature bath 348. Flask 350 collects ethanol 352, which is evaporated from the oil and ethanol 342 mixture.
    [064] After the recovery of 352 ethanol from oil 342, the oil is decarboxylated in container 360, which is heated by heater 362. During the decarboxylation process, oil 363 is stirred by a magnetic stirrer 364.After decarboxylation , the oil 363 is transferred to a feed chamber 365. At the bottom of the feed chamber 365, a pump 366 pumps the oil through a feed line 367 and a check valve 368 to a trajectory film cleaner short 370. Pump rates are typically 1000 to 1500 ml / hr and depend on the CO2 emission, if any, the percentage of THCa converted to THC and the vacuum pressure of the short path film cleaner. In the short path film cleaner 370, the oil is cleaned in a thin film around the heated inner wall 372 of the film cleaner 370 by a blade 374. The inner wall 372 is heated through a maintenance jacket temperature. A cooler condensing coil 376 condenses the target fraction, which leaves film cleaner 370 as a distillate through target discharge tube 380 and is collected in container 382. Residual liquids fall down the inner wall 372 of the film cleaner 370 and exit through residual arm 390 to be collected in container 392. Film cleaning takes place under reduced pressure provided by a vacuum pump connected to port 396 through a cold trap. E. Additional Exemplary Process
    [065] With reference to Figure 4, a flow chart is shown that summarizes the basic steps of an alternative process.
    [066] In step 402, after adding ethanol to a WSD separator containing the raw cannabis plant material, the plant material is washed with ethanol in the WSD. The raw cannabis plant material is then “dried” using the centrifugation cycle function of the WSD separator. Then, in step 404, the resulting mixture of crude oil and ethanol is treated with different media and filtered. During step 404, the impurities contained in the mixture of crude oil and ethanol are removed. In step 406, the ethanol from the resulting oil and ethanol mixture is evaporated and recovered. After that, in step 408, the oil is washed with a saline solution and then the non-polar solvent is added before the saline wash is removed in step 410. Steps 406 and 410 are considered to be the recovery stages of solvent.
    [067] In step 412, the oil remaining after evaporation of the non-polar solvent is decarboxylated to activate the THC and evaporate any remaining solvent. The residue after decarboxylation is then, in step 414, distilled using a 592 film cleaner to extract the cannabinoids.
    [068] With reference to Figure 5, details of the alternative process for the extraction of cannabinoids are shown. Steps 420-432 refer to the primary extraction phase. Steps 434-452 refer to the treatment and filtration stage of the medium. The ethanol removal and recovery stage 454 and the non-polar solvent removal stage 464 form the solvent recovery stages. Steps 456-463 are the saline wash stage. Step 466 refers to the decarboxylation stage and step 468 refers to the distillation of cannabinoids.
    [069] In step 420, raw cannabis plant material is supplied. In step 422, the raw cannabis plant material is dried, if not already supplied in dry form. Ideally, the moisture content of the raw cannabis plant material after drying is 10% or less by weight. In other embodiments, the moisture content can be as high as 15% while still allowing for an acceptable process. other embodiments, other drying techniques can be used.
    [070] In step 424, the dry plant material is ground, for example, to an average size between 250 and 300 μm. However, in other embodiments, it is possible to grind the dry plant material to a size of thousands of microns, and it has been found that the process works with average particle sizes of up to 3000 to 9000 μm. Note that, in other embodiments, the milling step can take place before the drying step. The ground and dried vegetable material is then placed in a closed, porous bag.
    [071] In step 426, ethanol is cooled (if necessary) to a temperature between -60 ° C and +18 ° C, in a tank surrounded by a pressurized liquid CO2 jacket, for example. In some embodiments, ethanol is used at room temperature, that is, 18 ° C. However, cooled ethanol, when used for extraction, reduces impurities such as fats, lipids and pigments in crude cannabis oil.
    [072] In step 428, the cooled ethanol is added to the WSD separator in which the bag of ground and dried vegetable material was placed. Typically, approximately 40 to 50 liters of cooled ethanol are used for every 5-6 kg of plant material (ie 6.6 to 10 liters per kg), although it is possible that other proportions may be used. In step 430, the mixture of ethanol and plant material is passed through the washing and centrifugation modes of the WSD separator. Ethanol is continuously fed into the drum as it is turned. Depending on the embodiment, the drum is rotated for 8 to 15 minutes. Ethanol, in some embodiments, is pressurized between 1 to 15 psi (7 to 100 kPa) as it is fed into the drum. Due to the centrifugal force, the crude oil is extracted (that is, dissolved in ethanol). The extent of drying, that is, the removal of liquid from plant material, depends on the speed of the centrifugation cycle. The WSD separator has a centrifugal drum for washing and extraction and a centrifuge cycle mode to separate the solvent. In step 432, the ethanol, now with dissolved extracts (ie, a mixture of crude oil and ethanol), is drained out of the centrifuge drum during the centrifuge cycle mode. The mixture of crude oil and ethanol is drained as a result of the centrifugal force due to the rotation action of the drum. The solid plant material remains inside the mesh bag.
    [073] In some embodiments where ethanol is cooled, the ideal temperature has been found to be -45 ° C. However, the ideal temperature can be different in other embodiments.
    [074] In the following steps, the mixture of crude oil and ethanol is treated with different media and filtered to remove chlorophyll, pigments, plant material and any other impurities that are inevitably retained in the mixture after the 432 drainage step. 1 to 5 different means of treatment.
    [075] In step 434, the mixture of crude oil and ethanol is treated with charcoal (charcoal scrubbing). The mixture of crude oil and ethanol is at a temperature between -10 ° C and +85 ° C for the charcoal scrub. Charcoal, when in particulate form, is first added to the crude oil and ethanol mixture and then the mixture is stirred. The average size of the charcoal particles is in the range of 0.25 to 150 μm, although other sizes are possible in other embodiments.
    [076] Any charcoal that is in the mixture of crude oil and ethanol is removed by filtering it using lenticular depth filtration devices and / or column housing filters with insertion cartridges, in step 436. The depth filtration systems lenticular filters generally use lenticular filters that are capable of retaining and collecting charcoal particles. A filter cartridge with a pore size of 0.2 to 1 μm is used. The filtration of charcoal is carried out at a temperature between -10 ° C and 50 ° C.
    [077] In another embodiment, lenticular filtration alone for the treatment of charcoal is used to simultaneously handle the charcoal treatment and the filtration process.
    [078] In step 438, the mixture of crude oil and ethanol is reheated to a temperature between 60 ° C and 78 ° C for further treatment. In other embodiments, it is possible to skip this step and perform the subsequent treatment and filtration steps at room temperature or even using the mixture of crude oil and ethanol in its previously cooled state, or at another refrigerated temperature, for example, as low -40 ° C.
    [079] In step 440, the mixture of crude oil and ethanol is treated with a bentonite clay. The clay, when in particulate form, is first added to the heated mixture of crude oil and ethanol and then the mixture is stirred. The average size of the clay particles is in the range of 0.25 to 150 μm, although other sizes are possible in other embodiments.
    [080] The mixture of crude oil and ethanol is then allowed to cool to a temperature between 10 and 50 ° C in step 442. Any clay that is in the mixture of crude oil and ethanol is removed by filtering it in step 444, using Lenticular depth filtration and / or column housing filters with insertion cartridges. A filter cartridge with a pore size of 0.2 to 1 μm is used.
    [081] In step 446, the mixture of crude oil and ethanol is reheated to a temperature between 60 ° C and 78 ° C for further treatment. In other embodiments, it is possible to skip this step and perform the subsequent treatment and filtration steps at room temperature or even using the mixture of crude oil and ethanol in its previously cooled state, or at another refrigerated temperature, for example, as low -40 ° C.
    [082] In step 448, the mixture of crude oil and ethanol is then treated with magnesium oxide. Magnesium oxide, in particulate form, is first added to the heated crude oil and ethanol mixture and then the mixture is stirred. The average size of the magnesium oxide particles is in the range of 0.25 to 150 μm, although other sizes are possible in other embodiments.
    [083] The crude oil and ethanol mixture is then allowed to cool to a temperature between 10 and 50 ° C in step 450. Any magnesium oxide that is in the crude oil and ethanol mixture is removed by filtering it in step 452, using Lenticular depth filtration apparatus and / or column housing filters with insertion cartridges.
    [084] In one embodiment, filtration of charcoal (step 436), clay (step 444) and MgO (step 452) are all performed as a single step after treatment with MgO.
    [085] In an additional embodiment, a silica gel is used as a treatment of the medium, after treatment with clay and before treatment with MgO.
    [086] In step 454, the resulting oil and ethanol mixture is then processed with a rotary evaporator to remove and recover ethanol from the mixture. The rotary evaporator temperature is 43 to 49 ° C and is operated at a pressure of 83 to 101 kPa (25 to 30 inHg, 635 to 760 mmHg). Other evaporators or evaporation techniques can be used in other embodiments, for example, downward film evaporators, upward film evaporators or instant and spray dryers can be used. The ethanol that is recovered can be used to extract cannabinoids from an additional batch of dry and ground raw cannabis plant material. Normally, 75% of the used ethanol is recovered.
    [087] The oil, now without ethanol, is then mixed with hexane, heptane or pentane (non-polar solvents) with a 1: 1 ratio of hexane, heptane or pentane to oil, in step 456, to result in a mixture of oil and solvent. Note that other reasons are also possible. The role of non-polar solvents here is to further extract the oil for the next processing steps, due to its ability to solubilize cannabinoids. Non-polar solvents, such as hexane, heptane or pentane, dissolve fats and oils and leave behind proteins, carbohydrates and other insoluble impurities in these solvents and other non-polar solvents. This type of solvent is also used in the oil extraction field for its ability to be removed due to its low boiling point. In addition, non-polar solvents exhibit the property of being insoluble in water, which helps to some extent to separate water and other water-soluble solvents from the non-polar one.
    [088] Next, the saline solution is added to the oil and solvent mixture in step 458. The oil and solvent mixture is then washed with saline solution (60% to 100% saturated with salt) to remove water-soluble compounds in the step 460, and remove impurities and any traces of the treatment medium that may have remained in the oil. The saline solution helps to break the emulsions and to dry the oil by extracting the water that may have dissolved in the mixture and also extracts ethanol from the non-polar phase and crude oil in the saline solution. Then, the saline solution is separated from the oil in step 462.
    [089] The saline solution is prepared with distilled water and kosher salt, that is, sodium chloride without iodine. After washing with saline solution, the saline solution, with water-soluble compounds, is separated from the oil and non-polar solvent by means of a centrifuge or a gravity-fed separating funnel. Unless solvents of 99.9999% purity are used, there is always a water content that extracts soluble (ie, sugars) from the raw cannabis plant material in the primary extraction stage. These water-soluble compounds need to be removed by washing with liquid-to-liquid extraction saline.
    [090] As an example, 500 ml of hexane, pentane or heptane are added to 500 ml of oil and then homogenized using an overhead stirrer. Then, 1000 ml of distilled water saturated with kosher sodium chloride at 60-100% saturation are added to the mixture of oil and solvent (that is, the ratio of non-polar solvent to oil and saline is 1: 1: 2) and stirred for 5 to 30 min with an overhead stirrer.
    [091] After removing the saline from the oil, the remaining traces of water, if any, are then removed from the oil with a treatment with magnesium sulfate, in step 463, in which powdered MgO4 is spun in the oil and then filtered , for example by gravity filtration.
    [092] In step 464, the oil and solvent mixture is then processed with a rotary evaporator to remove and recover the non-polar solvent. The rotary evaporator temperature is 43 to 49 ° C and is operated at a pressure of 83 to 101 kPa (25 to 30 inHg, 635 to 760 mmHg). The non-polar solvent, such as hexane, heptane and / or pentane, which is recovered, can be used for future saline wash applications. About 75% of the non-polar solvent is recovered for later use.
    [093] After removing the non-polar solvent using the rotary evaporator, decarboxylation is performed on the resulting oil in step 466. Decarboxylation is performed to convert THCa to THC, releasing CO2 in the process. In the process, residual solvents that may be present are evaporated.
    [094] In one embodiment, oil is first passed through a 592 short path distillation film cleaning apparatus to convert THCa to THC. The temperature of the 584 feed tank (Figure 6B) for cleaning the film is set in the range of 100 to 115 ° C. The temperatures of the pump 586 and the feed line 588 for the film cleaning apparatus 592 are set to the same value as the feed tank 584. The temperature of the waste discharge arm 604 and its associated pump, not shown, is also set in the range 100 to 115 ° C and is also more generally set in the range 107 to 110 ° C. The temperature of the target heater, which controls the temperature of the inner wall 594, is adjusted within a range of 140 to 175 ° C, usually 170 ° C.
    [095] The temperature of the inner wall is controlled by adjusting the temperature of a 595 bath. A pump circulates fluid that is heated to the bath temperature through a jacket around the outside of the wall. As such, the temperature of the inner wall is expected to be slightly below the temperature of the bath, depending, for example, on the temperature and the rate at which the oil is cleaned on the inner wall 594. Other temperatures of the film cleaner are defined in a similar way. These other temperatures are also expected to be slightly different from the bath configuration, but not to a significant degree. The condensing coil 598 is set at a temperature of 0 ° C to -20 ° C, as well as the distillate or target discharge arm 600 and its associated pump (not shown).
    [096] Liquid nitrogen is used to maintain cryogenic temperatures in a cold trap between vacuum port 608 and the vacuum pump (not shown) from -180 ° C to -196 ° C. The use of these temperatures allows the maintenance of a deep vacuum. The film cleaning process is carried out at a pressure of 150 to 200 mbar. Decarboxylated oil is collected through the distillate arm.
    [097] Although the temperature of the film cleaner is higher than the minimum 90 ° C required for converting THCa under vacuum and in the range where product degradation can occur, the residence time at these high temperatures in the film is low or sufficient for insignificant amounts of product degradation to occur. In addition, the temperature settings do not actually represent the contact temperature, as the settings are defined in the circulating bath fluid and do not represent the oil temperature that is in contact with the glass surface area of the evaporator. The glass acts as an insulator between the heat transfer fluid and the oil. The temperature difference between the bath heat transfer fluid and the heated oil should be in the range of 1 to 5 ° C.
    [098] Decarboxylation is performed under vacuum to decrease the temperature required to convert THCa to THC. It can be done on the 592 film cleaner effectively as a decarboxylation step, or done in a heated reactor (eg 504), for example. The oil itself must reach temperatures of at least 105 ° C at atmospheric pressure. If a vacuum reactor is used, the oil only needs to be heated to at least 90 ° C. The same temperature (> 90 ° C) can also be used when the 592 film cleaner is used. The film cleaner decarboxylation process allows for a much shorter heat residence time, so that oil degradation is less when compared to decarboxylation in a reactor.
    [099] In other embodiments, decarboxylation is carried out by heating the oil to 90-110 ° C under vacuum in an oven. If the temperature is below this range, then there is potentially some residual solvent. Most of the CO2 that is produced from decarboxylation is removed to ensure consistent vacuum levels later in the process. If the temperature is above this range, then product degradation will occur. This method of decarboxylation process usually takes several hours.
    [0100] There are other ways in which the decarboxylation process can be carried out. For example, cannabis resin is heated in vegetable biomass in greenhouses similar to the vacuum greenhouses used to dry the cannabis plant, before adding ethanol for primary extraction. The process is simply to heat the biomass to> 90 ° C for a period of time subject to the amount of biomass being heated.
    [0101] The decarboxylated oil is passed through the 592 short path distillation film cleaner once more, this time to remove some volatile terpenes. The temperature of the feed tank 584 for the film cleaner 592 is set in the range of 100 to 115 ° C and, more generally, is set in the range of 107 to 110 ° C. The temperatures of the pump 586 and the feed line 588 for the film cleaner 592 are set to the same value as the feed tank 584. The temperature of the waste discharge arm 604 and its associated pump, not shown, is also set in the range of 100 to 115 ° C and is also more generally adjusted in the range of 107 to 110 ° C. The temperature of the target heater, which controls the temperature of the inner wall 594, is adjusted within a range of 140 to 145 ° C, usually 145 ° C. The condensing coil 598 is set at a temperature of 0 to -20 ° C, as well as the distillate or target discharge arm 600 and its associated pump (not shown), through which the terpenes are removed. Liquid nitrogen is used to maintain cryogenic cold trap temperatures between vacuum port 608 and vacuum pump from -180 to -196 ° C. This film cleaning process is carried out at a pressure of 0.001 to 0.01 mbar.
    [0102] The residual oil from the previous film cleaning step is again passed through the short path distillation film cleaning apparatus 592 to remove some non-volatile terpenes. Especially volatile terpenes are removed in the previous step and mainly non-volatile terpenes are removed in this step, as there is no sharp cut between volatile and non-volatile terpenes. The temperature of the feed tank 584 for cleaning film is set in the range of 100 to 115 ° C and, more generally, is set in the range of 107 to 110 ° C. The temperatures of the pump 586 and the feed line 588 for the film cleaner 592 are set to the same value as the feed tank 584. The temperature of the waste discharge arm 604 and its associated pump, not shown, is also set in the range of 100 to 115 ° C and is also more generally adjusted in the range of 107 to 110 ° C. The temperature of the target heater, which controls the temperature of the inner wall 594, is adjusted within a range of 145 to 159 ° C, usually 155 ° C. The condensing coil 598 is set at a temperature of 20 to 60 ° C, as is the distillate or target discharge arm 600 and its associated pump (not shown), through which the terpenes are removed. Liquid nitrogen is used to maintain cryogenic cold trap temperatures between vacuum port 608 and vacuum pump from -180 to -196 ° C. The use of cryogenic temperatures allows the maintenance of a deeper vacuum. This film cleaning process is carried out at a pressure of 0.001 to 0.01 mbar.
    [0103] The residual oil from the previous film cleaning step is again passed through the short path distillation film cleaning apparatus 592 to remove the cannabinoids as a whole. The temperature of the feed tank 584 for cleaning film is set in the range of 100 to 115 ° C and, more generally, is set in the range of 107 to 110 ° C. The temperatures of the pump 586 and the feed line 588 for the film cleaner 592 are set to the same value as the feed tank 584. The temperature of the waste discharge arm 604 and its associated pump, not shown, is also set in the range of 100 to 115 ° C and is also more generally adjusted in the range of 107 to 110 ° C. The temperature of the target heater, which controls the temperature of the inner wall 594, is adjusted within a range of 140 to 165 ° C. The condensing coil 598 is set at a temperature of 68 to 73 ° C, as is the distillate or target discharge arm 600 and its associated pump (not shown), through which the cannabinoids are removed. Liquid nitrogen is used to maintain cryogenic cold trap temperatures between vacuum port 608 and vacuum pump from -180 to -196 ° C. The film cleaning process is carried out at a pressure of 0.0008 to 0.003 mbar. This passage requires the use of a diffusion pump to help reach deeper voids. It is installed in the 592 film cleaner, but is not used for decarboxylation and terpene fraction passages.
    [0104] The result of the distillate discharge arm 600 is a tasteless and odorless oil containing up to 99% pure cannabinoids. Often, however, the resulting oil will require another pass through the clean film apparatus 592 in order to achieve purities of 90% or more. F. Additional device
    [0105] With reference to Figures 6A-B, an example of the apparatus for the additional exemplary process is shown schematically.
    [0106] The raw cannabis plant material is supplied in a 500 hopper, for example, and is released in batches in container 502. The raw cannabis plant material is vacuum dried 504. Then the plant material dry is placed in a 506 grinder.
    [0107] After the grinding step, in one embodiment, the ground vegetable material is placed in a bag in one or more WSD 508 separator units.
    [0108] After the raw cannabis plant material has been processed into ethanol, ethanol, now with dissolved cannabinoids, is drained out of the WSD 508 separator as a mixture of crude oil and ethanol, through the 510 outlet tube into the container 512. An example of an extraction vessel holds 5 to 5.5 kg of biomass in a single biomass cavity. Other capabilities are also possible. The container is surrounded by an insulating jacket.
    [0109] The mixture of crude oil and ethanol is then fed into a charcoal treatment unit 514 and after processing is then fed into a 516 lenticular depth filtration apparatus through an inlet tube 518.The oil mixture crude and ethanol is filtered through one or more 520 lenticular depth filtration cartridges. The 520 lenticular depth filtration cartridges retain the particles present in the crude oil and ethanol mixture within their structure. The mixture of crude oil and ethanol is further transported to the central column 522 of the lenticular depth filtration apparatus 516 and collected through an outlet tube 524 in a container with a treatment medium of bentonite clay 526.
    [0110] After processing with charcoal, the mixture of crude oil and ethanol is drained from the bentonite clay and then fed through the inlet tube 528 to another lenticular depth filtration apparatus 530. The mixture of crude oil and ethanol is then filtered through one or more lenticular depth filtration cartridges 532. The mixture of crude oil and ethanol is further transported to a central column 534 of the lenticular depth filtration apparatus 530 and collected through an outlet tube 536 into a container with a 538 magnesium oxide treatment medium.
    [0111] The crude oil and ethanol mixture is drained from magnesium oxide and then fed through a 540 inlet tube to another 542 lenticular depth filtration apparatus. The crude oil and ethanol mixture is then filtered through one or more lenticular depth filtration cartridges 544. The mixture of crude oil and ethanol is further transported to a central column 546 of the lenticular depth filtration apparatus 542 and then through an outlet tube 550 to a container 552.
    [0112] Each of the filter cartridges can be replaced independently. Additional treatment media and filter groups are used for additional treatment media in other embodiments.
    [0113] The resulting oil and ethanol mixture is then passed to a rotary evaporator 554. The oil and ethanol mixture 556 is maintained at an elevated temperature in flask 558, which is heated in a bath of temperature 560. Flask 562 collects ethanol 564, which is evaporated from the mixture of oil and ethanol 556.
    [0114] Hexane, heptane or pentane are then added to the mixture of oil and ethanol with a mixing ratio of 1: 1, to form a mixture of oil and solvent, which is stirred with an overhead stirrer 566. Saline is added to the oil / solvent solution and homogenized using a 568 overhead stirrer. The water (as a saline solution) is then separated from the saline / oil / solvent mixture by means of a 570 mechanical centrifuge.
    [0115] The oil and solvent mixture is then passed to a rotary evaporator 572. The oil and solvent mixture 574 is maintained at an elevated temperature in flask 576, which is heated in a temperature bath 578. Flask 580 collects the solvent 582, which is evaporated from the mixture of oil and solvent 574.
    [0116] After the recovery of solvents 582 from oil 574, the oil is decarboxylated. In one embodiment, oil 574 is transferred to a feed chamber 584 of a film cleaning apparatus 592. At the bottom of feed chamber 584, a pump 586 pumps oil through a feed line 588 and a valve holding capacity 590 for the short path film cleaner 592. Pump rates are typically 1000 to 1500 ml / hr and depend on the CO2 emission, if any, the percentage of THCa converted to THC and the vacuum pressure of the short path film cleaner 592. In short path film cleaner 592, the oil is cleaned in a thin film around the heated inner wall 594 of the film cleaner 592 by a blade 596. The wall internal 594 is heated through a temperature maintenance jacket. A cooler condensing coil 598 condenses the target fraction, which leaves the film cleaner 592 as a distillate through the target discharge tube 600 and is collected in container 602. Residual liquids fall down the inner wall 594 of the film cleaner 592 and exit through the residual arm 604 to be collected in the container 606. The film cleaning takes place under reduced pressure provided by a vacuum pump connected to port 608 through a cold trap.
    [0117] Using the system of the present invention, it is possible to convert approximately 40 to 44 kg (88 to 97 lb) of raw cannabis plant material into pure or almost pure distilled oil over a period of 16 hours. The apparatus and process can also be used for the extraction, refinement and distillation of residual plant material from processes that fail to extract all the valuable extracts. The apparatus and the process can be extended, depending on the amount of raw cannabis plant material to be treated. G. Variations
    [0118] Although the best way currently contemplated to carry out the object matter revealed and claimed here has been described, other ways are also possible.
    [0119] In some embodiments, a fractional distillation apparatus with a rotation axis is used instead of the short path film cleaning apparatus for one or more of the film cleaning steps.
    [0120] In some embodiments, ethanol is not cooled in step 112, which is omitted, and ethanol added to the raw decanabis plant material at a temperature of 15 to 30 ° C in step 115. In these embodiments, steps 127, 132 and 137 are omitted, as the ethanol is not cooled before stages128, 133 and 138 of paper filter. Filtration is particularly important if ethanol is used at room temperature. It has been found that 10% more extracts are obtained using ethanol at room temperature compared to using cooled ethanol, but that the filtration stage is significantly more expensive. This is also subjective to the type of plant material used, but it is known that uncooled ethanol has a greater miscibility, which makes ethanol less discriminatory, thus extracting more unwanted materials.
    [0121] Optionally, once cannabinoids are extracted in step 180 or 468, they can be passed additionally through the film cleaning apparatus 592 to separate them in THC and CBD. In other embodiments, fractional distillation with axis of rotation is used instead of film cleaning to separate THC and CBD.
    [0122] In other embodiments within the scope of the present invention, plant materials other than cannabis can be processed. For example, hemp can be processed to result in a 95% pure CBD oil. The present invention has wide application in relation to other plants that produce phytochemicals of interest, such as for the extraction of lavender mimetic cannabinoids. Phytochemicals of interest include cannabinoids, terpenes and flavonoids.
    [0123] In some embodiments, the device is portable so that it can be taken to the different locations of various plant producers, to be used as needed.
    [0124] In some embodiments, one or more additional medium treatment steps using an atapulgite clay, a bentonite clay and / or silica filtration medium, are added to the described medium treatment configurations.
    [0125] The 570 mechanical centrifuge, used to separate the oil and solvent mixture from the saline solution, can be replaced by a gravity-fed separating funnel.
    [0126] As an alternative to the 468 film cleaning step, a fractional distillation or axis rotation distillation procedure can be used to remove four fractions, for example, as opposed to the single fraction of the film cleaning process.
    [0127] Ethanol with 99% purity or more can be used for the extraction process.
    [0128] In some embodiments, to eliminate the washing step with saline solution, anhydrous ethanol (<0.005% water) is used instead of the most common formula of ethanol which is approximately 95% pure with 5% water. This reduces the need for more robust post-extraction filtration. However, measures must be taken to avoid instantaneous water contamination when anhydrous ethanol is exposed to air.
    [0129] In some embodiments, treatment of the medium is omitted if a lower quality of cannabis oil is desired.
    [0130] The temperatures that have been given to the nearest degree include all temperatures within ± 0.5 ° C of the given value. The temperatures that have been given to the nearest 0.1 ° C include all temperatures within ± 0.05 ° C of the given value.
    [0131] Other pore sizes of filter cartridges are used in other embodiments.
    [0132] In other embodiments, the vacuum pressure of the rotary evaporator in the non-polar solvent recovery step 464 is different from the range given above.
    [0133] In some embodiments, it is not necessary to completely remove the ethanol from the oil recovery step in ethanol 454. It has been found that the residual ethanol in the oil will be absorbed in the aqueous phase of saline during the solution washing step saline 460. Therefore, there is no need for absolute removal of ethanol from crude oil.
    [0134] In some embodiments, non-polar solvents other than hexane, heptane and pentane are used.
    [0135] In general, unless otherwise specified, singular elements may be plural and vice versa without loss of generality.
    [0136] Throughout the description, specific details have been established to provide a more complete understanding of the invention. However, the invention can be practiced without these details. In other cases, well-known elements have not been shown or described in detail and the repetitions of steps and characteristics have been omitted to avoid unnecessarily confusing the invention. For example, various pumps, valves, liners and lines are not shown for clarity. Therefore, the specification and drawings should be considered in an illustrative rather than a restrictive sense.
    [0137] It will be clear to a person skilled in the art that additional variations to the specific details disclosed herein can be made, resulting in other embodiments that are within the scope of the disclosed invention. The steps in the flowchart can be performed in a different order, other steps can be added, or one or more steps can be removed without changing the main outcome of the process. All parameters, dimensions, materials and configurations described here are examples only and can be changed depending on the specific embodiment. Therefore, the scope of the invention must be interpreted according to the matter defined by the following claims.
    权利要求:
    Claims (28)
    [0001]
    1. PROCESS TO EXTRACT CANNABINOIDS from raw cannabis plant material characterized by comprising the steps of: adding ethanol to the dry and ground cannabis plant material to form an initial mixture; centrifuge the initial mixture to separate a mixture of crude oil and ethanol from the initial mixture; treating the mixture of crude oil and ethanol with charcoal particles, bentonite clay particles and magnesium oxide particles to remove unwanted components from it; evaporating the ethanol from the mixture of crude oil and treated ethanol to leave the oil; wash the oil with saline solution; heating the washed oil with saline to convert THCa (tetrahydrocannabinolic acid) to the oil washed with saline solution in THC (tetrahydrocannabinol), resulting in decarboxylated oil; and distill the decarboxylated oil to obtain cannabinoids.
    [0002]
    2. PROCESS, according to claim 1, characterized by further comprising the steps of: adding a non-polar solvent to the oil before washing the oil with saline solution; and evaporate the non-polar solvent after washing the oil with saline.
    [0003]
    3. PROCESS, according to claim 2, characterized by the nonpolar solvent solvent comprising hexane, heptane or pentane.
    [0004]
    4. PROCESS, according to claim 2, characterized by further comprising, after washing the oil with saline solution and before evaporating the non-polar solvent, drying the oil with magnesium sulfate.
    [0005]
    5. PROCESS, according to claim 2, characterized by the fact that: - saline solution is 60-100% saturated with kosher sodium chloride; the saline wash step comprises stirring the non-polar solvent, oil and saline for 5 to 30 minutes; and the saline solution is removed by a gravity-fed centrifuge or separation funnel.
    [0006]
    6. PROCESS, according to claim 5, characterized by the fact that the ratio of non-polar solvent to oil to saline is 1: 1: 2 by volume.
    [0007]
    7. PROCESS, according to claim 2, characterized by the fact that the heating step comprises the passage of the oil washed with saline solution through a short-film cleaning device.
    [0008]
    8. PROCESS, according to claim 7, characterized by the fact that the film cleaning apparatus has: a supply temperature of 100 to 115 ° C; a temperature of the waste discharge arm of 100 to 115 ° C; an inner wall surrounded by a jacket with a circulating fluid at a temperature of 160 to 175 ° C; and a temperature of the condensing coil from 0 ° C to -20 ° C.
    [0009]
    9. PROCESS, according to claim 2, characterized in that the heating step comprises heating the oil washed with saline solution to 90-110 ° C in a vacuum oven.
    [0010]
    10. PROCESS, according to claim 1, characterized by further comprising the steps of: drying the raw cannabis plant material; and grinding the raw cannabis plant material to result in the dry and ground plant material.
    [0011]
    11. PROCESS, according to claim 10, characterized by the fact that the raw cannabis plant material is: dry to a moisture content <5%; and ground to an average particle size <9000μm.
    [0012]
    12. PROCESS, according to claim 1, characterized by the fact that the centrifugation step occurs in a washing and drying separator by centrifugation and has a duration of 8 to 15 minutes.
    [0013]
    13. PROCESS, according to claim 1, characterized by the fact that: ethanol is at a temperature between -60 ° C and 18 ° C when it is added to the dry and ground cannabis plant material; and ethanol is added to the dried and ground cannabis plant material in a ratio of 6.6-10 liters of ethanol to 1 kg of ground plant material.
    [0014]
    14. PROCESS, according to claim 1, characterized by the fact that the treatment of the mixture of crude oil and ethanol comprises the steps of: adding the charcoal particles to the mixture of crude oil and ethanol, stirring the charcoal particles and mixing crude oil and ethanol and filtering the charcoal particles; then add the bentonite clay particles to the crude oil and ethanol mixture, stir the bentonite clay particles and the crude oil and ethanol mixture and filter the bentonite clay particles; and then adding the magnesium oxide particles to the crude oil and ethanol mixture, stirring the magnesium oxide particles and the crude oil and ethanol mixture and filtering out the magnesium oxide particles.
    [0015]
    15. PROCESS, according to claim 14, characterized by the fact that: filtering the charcoal particles comprises filtering the charcoal particles and the mixture of crude oil and ethanol with a lenticular depth filtration apparatus; filtering the bentonite clay particles comprises filtering the bentonite clay and the mixture of crude oil and ethanol with a lenticular depth filtration apparatus; and filtering the magnesium oxide particles comprises filtering the magnesium oxide particles and the mixture of crude oil and ethanol with a lenticular depth filtration apparatus.
    [0016]
    16. PROCESS, according to claim 15, characterized by the fact that: the mixture of crude oil and ethanol is at a temperature between -10 ° C and +85 ° C when the charcoal particles are added; the charcoal particles are filtered at a temperature between -10 ° C and 50 ° C; and the bentonite clay particles and the magnesium oxide particles are filtered at a temperature between 10 ° C and 50 ° C.
    [0017]
    17. PROCESS, according to claim 1, characterized by the fact that the unwanted components are one or more among pigments, chlorophyll, fats, waxes, lipids, heavy metals and particulate materials.
    [0018]
    18. PROCESS, according to claim 1, characterized by the fact that the distillation step comprises: subjecting the decarboxylated oil to a first film cleaning to remove volatile terpenes and leaving a first residue; subjecting the first residue to a second film cleaning to remove non-volatile terpenes and leaving a second residue; and subjecting the second residue to a third film cleaning to obtain cannabinoids.
    [0019]
    19. PROCESS, according to claim 18, characterized by the fact that: the first and the second film cleaning are carried out at a pressure of 0.001 to 0.01 mbar; and the third film cleaning is carried out at a pressure of 0.0008 to 0.003 mbar.
    [0020]
    20. PROCESS according to claim 18, characterized in that it further comprises subjecting cannabinoids to an additional film cleaning process to separate cannabinoids into cannabidiol and tetrahydrocannabinol.
    [0021]
    21. PROCESS, according to claim 18, characterized by the fact that: -the first film cleaning is carried out with: a feeding temperature of 100 to 115 ° C; a waste discharge arm temperature of 100 to 115 an inner wall surrounded by a jacket with a circulating fluid at a temperature of 140 to 145 ° C; and a temperature of the condensing coil from 0 ° C to -20 ° C; -the second film cleaning is carried out with: a feed temperature of 100 to 115 ° C; a temperature of the waste discharge arm from 100 to 115 an inner wall surrounded by a jacket with a circulating fluid at a temperature of 145 to 159 ° C; and a condensing coil temperature of 20 to 60 ° C; and -the third film cleaning is carried out with: a feed temperature of 100 to 115 ° C; a temperature of the waste discharge arm of 100 to 115 ° C; an inner wall surrounded by a jacket with a circulating fluid at a temperature of 140 to 165 ° C; and a condensing coil temperature of 68 to 73 ° C.
    [0022]
    22.PROCESS, according to claim 1, characterized by the fact that the raw cannabis plant material is the cannabis flower.
    [0023]
    23. PROCESS, according to claim 1, characterized by the fact that the raw cannabis plant material is cannabis leaves and stems.
    [0024]
    24. PROCESS, according to claim 1, characterized by the fact that the distillation step is performed using a distillation apparatus with a rotation axis.
    [0025]
    25.PROCESS, according to claim 1, characterized by the fact that the addition and centrifugation steps are performed simultaneously.
    [0026]
    26. PROCESS, according to claim 1, characterized in that it also comprises leaving residual ethanol in the oil after the evaporation step, in which the saline washing step removes the residual ethanol from the oil.
    [0027]
    27.PROCESS, according to claim 1, characterized by the fact that the terpenes are obtained in the distillation stage.
    [0028]
    28. PROCESS, according to claim 18, characterized in that it further comprises subjecting cannabinoids to a fractional distillation process with a rotation axis to separate cannabinoids into cannabidiol and tetrahydrocannabinol.
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    同族专利:
    公开号 | 公开日
    AU2019250112A1|2019-10-31|
    US10406453B2|2019-09-10|
    CO2019014964A2|2020-01-17|
    IL269422A|2020-05-31|
    PE20200397A1|2020-02-26|
    EP3645027A4|2021-05-19|
    ZA201906293B|2020-09-30|
    US20190099696A1|2019-04-04|
    BR112019026417A2|2020-07-21|
    AU2018340881B2|2019-12-05|
    IL269422D0|2019-11-28|
    IL269306A|2020-05-31|
    IL269173A|2020-05-31|
    MA49527A|2021-05-19|
    CA3063960C|2020-03-10|
    MX2019012109A|2020-02-12|
    CO2020007209A2|2020-06-19|
    EP3645027A1|2020-05-06|
    IL269173D0|2019-11-28|
    AU2019250112B2|2019-12-05|
    CL2019003462A1|2020-03-06|
    WO2019060986A1|2019-04-04|
    AU2018340881A1|2019-10-17|
    CA3063960A1|2019-04-04|
    IL269306D0|2019-11-28|
    NZ757625A|2019-12-20|
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    法律状态:
    2020-11-17| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|
    2020-12-01| B16A| Patent or certificate of addition of invention granted|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 07/09/2018, OBSERVADAS AS CONDICOES LEGAIS. |
    优先权:
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