Abstract:
An extraction apparatus and a processes for preparing extracts of natural products, such as plant material, and for preparing purified extracts from crude extracts of natural products by extraction with a non-polar solvent hot gas.

Description:
CROSS-REFERENCE TO RELATED APPLICATION 
       [0001]    The present disclosure claims priority to U.S. Provisional Patent Application Ser. No. 62/134,621, filed Mar. 18, 2015, to TENNANT et al and titled: EXTRACTION APPARATUS AND METHOD, the contents of which are incorporated herein for all purposes. 
     
    
     FIELD 
       [0002]    The present disclosure relates to an extractor apparatus and a processes for preparing extracts of natural products, such as plant material, and for preparing purified extracts from crude extracts of natural products by extraction with a non-polar solvent hot gas. 
       BACKGROUND 
       [0003]    It has been known for some time to use an extraction apparatus to expose a plant and/or flower to a solvent for the purpose of extracting various constituent components from the plant or flower and to then remove the solvent from the extracted components. The extracted components may be used in any variety of foods, goods and compositions. While extraction apparatuses are generally known for use in extracting various constituent components of plant material, the disclosure of U.S. Pat. No. 7,622,140 published Nov. 24, 2009, to Whittle et al, and entitled Processes For Preparing A Cannabinoid-Rich Extract From  Cannabis  Plant Material, the entire contents of which are incorporated herein by reference for all purposes, discloses a particular process and an apparatus for the useful separation of certain plant constituents. Despite the many known types of extraction devices and apparatuses, there remains no device which is highly capable of a controlled, efficient and effective extraction in a thoroughly portable device. 
         [0004]    While there have been many attempts by others to address this long known need, including the known apparatuses and processes, there remains an unmet need for an extraction apparatus and process for more efficiently, effectively and safely separating plant constituent components. 
     
    
     
       BRIEF DESCRIPTION OF THE DRAWINGS 
         [0005]      FIG. 1  is a front perspective view of an extraction apparatus according to the present disclosure. 
           [0006]      FIG. 2  is an alternate back perspective view of the extraction apparatus of  FIG. 1 . 
           [0007]      FIG. 3  is a plan front view of the extraction apparatus of  FIG. 1 . 
           [0008]      FIG. 4  is a partial perspective view of a solvent tank of the extraction apparatus of  FIG. 1 . 
           [0009]      FIG. 5  is a partial perspective view of a material column of the extraction apparatus of  FIG. 1 . 
           [0010]      FIG. 6  is a partial perspective view of a cryogenic column and a lipid filtering column of the extraction apparatus of  FIG. 1 . 
           [0011]      FIG. 7  is a partial, expanded, perspective view of the bottom end of the cryogenic column and lipid filtering column of  FIG. 6 . 
           [0012]      FIG. 8  is a partial, perspective view of a collection chamber column of the extraction apparatus of  FIG. 1 . 
           [0013]      FIG. 9  is a partial, perspective view of an expansion filter column of the extraction apparatus of  FIG. 1 . 
           [0014]      FIG. 10  is a schematic flow diagram of the extraction apparatus of  FIG. 1 . 
       
    
    
     DETAILED DESCRIPTION 
       [0015]    Referring in general to all of the figures, and initially in particular to  FIGS. 1 through 3 , there is illustrated an extraction apparatus  10  according to the present disclosure and capable of operating according to a method for more efficiently, effectively and safely extracting constituent materials and components from an amount of raw, plant or flower material. The extraction apparatus  10  may have particular use in isolating, via short path distillation or extraction, specific components and combinations of components of the plant or flower material. 
         [0016]    The extraction apparatus  10  of the present disclosure may be capable of providing sufficient control of the extraction process to more specifically isolate particularly components and combinations of components of the plant or flower material being extracted, and may provide improved control and process for obtaining the components to a molecular level. In one specific application, the extraction apparatus  10  may be used to isolate specific cannabinoids or groups of cannabinoids, as well as isolating THC and other specific constituent components and combinations to obtain an extraction product. More particularly, the present disclosure provides an extraction apparatus  10  including various components making it specifically possible to extract a particular terpene profile from a plant or flower material in a portable extraction apparatus  10 . The portable extraction apparatus  10  may accomplish the above while using a far more efficient and effective process. The extraction apparatus  10  may be operated to perform an extraction process preferably using a non-polar solvent. The extraction apparatus  10  may use a light hydrocarbon solvent. The extraction apparatus  10  may provide for greater control and efficiency of the extraction process such that a user may have greater control to obtain particular flavor profiles as well as desired quality, flavors and combinations of cannabinoids. 
         [0017]    The extraction apparatus  10  may preferably include a plurality of sub-components mounted to a wheeled, mounting rack  11 . The mounting rack  11  may preferably include a lower base portion, a plurality of uprights coupled to and extending from the lower base portion and a plurality of cross members extending between and coupled with the uprights. A first upright may include an upper surface and a second upright may include a second upper surface, as best shown in  FIGS. 1 through 3 . The mounting rack  11  may preferably be comprised of any material, including, in one particular embodiment, a metal such as stainless steel. The mounting rack  11  may be comprised of any known or appropriate material for use with the extraction apparatus  10  and for carrying out the extraction methods. 
         [0018]    The extraction apparatus  10  may include the solvent tank  20 , the material column  30 , the cryogenic column  40 , the lipid filtering column  50 , the collection chamber column  60 , the expansion filter column  80 , the recovery pump  90 , the cryogenic chiller  100 , and the recirculating heat  110 , all of which are coupled using a plurality of hoses  15  and having a plurality of ¼″ shut off valves  16  and gauges  18 . The components of the extraction apparatus  10  may be set up to create an extraction process flow as best shown by the  FIG. 10  which is continually referenced during the present disclosure. 
         [0019]    The solvent tank  20  may be coupled to the material tank or column  30  by a hose  15  coupling the outlet of the solvent tank  20  to an inlet on the lid of the material column tank  30 , the bottom of the material column  30  may be coupled to the inlet in the top of the top of the cryogenic column  40 . The cryogenic column  40  and the lipid filtering column  50  are integrated such that material (i.e., solvent and dissolved plant constituent components) leaving the cryogenic column  40  passes to the lipid filtering column  50  for removing the coagulated material constituent components and to separate them from the solvent and the dissolved constituent components from the plant material. The bottom of the lipid filtering column  50  is coupled (by a hose  15 ) to the inlet of the collection chamber column  60  which is integrated with the collection bowl  70  so that the solvent and the dissolved extracted constituent components from the material flowing there through may be collected in the collection bowl  70 . The dissolved extracted constituent components and the hydrocarbon solvent may then move to one of the expansion filter column  80  and the hydrocarbon recovery pump  90 . The hydrocarbon solvent removed by the hydrocarbon recovery pump  90  is then conveyed back to the solvent tank  20  as explained in greater detail herein. 
         [0020]    Referring generally to  FIGS. 1 through 3 , and in particular to  FIG. 4 , the extraction apparatus  10  may include the solvent tank  20  generally having the construction and proportions as shown in the figures. The solvent tank  20  may include a lid or cover  21 . The solvent tank cover  21  may include a plurality of passages for coupling the solvent tank  20  to the other components of the extraction apparatus  10 . The solvent tank  20  may preferably have a generally cylindrical shape and be made from any known or appropriate material for use in producing an (human) edible product, including, in particular, a stainless steel such as 304SS. The solvent tank  20  may be coupled to the other components using a hose  15  including a shutoff valve  16  for isolating the solvent tank  20  from all other components of the extraction apparatus  10 . 
         [0021]    The solvent tank  20  cover may also include a passage for receiving a high pressure vent down  17  as best shown in  FIG. 10 . The high pressure vent down  17  may be adjusted to have a relief, pressure setting of approximately 150 psi such that if the pressure in the solvent tank  20  is above the relief pressure setting (i.e., 150 psi), then the high-pressure vent down  17  will open and reduce the pressure in the solvent tank  20  below the relief pressure setting. The cover of the solvent tank  20  may also include a passage for receiving a compound pressure gauge  18  as best shown in  FIG. 11 . The high-pressure vent down  17  and the pressure gauge  18  may be coupled to the cover  21  of the solvent tank  20  using an end cap as is generally understood. The end cap may be coupled to the opening in the cover  21  of the tank  20  and sealed using a 1 inch Viton gasket (not shown). The end cap includes a passage for coupling the high-pressure vent down  17  and the pressure gauge  18 . The cover of the solvent tank  20  may further include a male JIC to male NPT union i straight hydraulic hose adapter as best shown in  FIG. 14 . 
         [0022]    Once the solvent tank  20  is completely assembled and isolated from the rest of the extraction apparatus  10  by closing the shutoff valves  16 , a vacuum pump (not shown) may be coupled to the tank  20  and a negative pressure (or vacuum) of approximately −30 inches of Mercury (in-Hg) may be established in the solvent tank  20  to remove as much oxygen (O 2 ). The vacuum pump may then be removed and a hydrocarbon solvent fill tank (not shown) may then be coupled to the solvent tank  20 . 
         [0023]    Once the solvent fill tank is coupled to the solvent tank  20 , the valve  16  may be opened and liquid solvent filled in an internal chamber  23  of solvent tank  20  to approximately 80% of the volume of the internal chamber  23 . It should be understood that other percentages may be used as may be desirable for achieving a particular outcome of the extraction process. The solid tank  20  may include sight glasses for viewing the level of the liquid hydrocarbon solvent therein. While it is possible to fill the solvent tank  20  at any time after the vacuum is established and an appropriate temperature is achieved (as described below), it is commonly not done until the entire system is prepared. 
         [0024]    Referring generally  FIGS. 1 through 3 , and in particular to  FIG. 5 , the components and details of the material column  30  are shown in partial perspective view in greater detail. The material column  30  may be a generally elongate cylindrical shaped body  31  including an inner chamber  33  extending between a first or upper end and a second or lower end. The material column  30  may further include a material column reducer  34  coupled to the lower end of the material column body using a 4 inch high-pressure tri-clamp  35  as shown in  FIG. 5  and which may be sealed using a 4 inch Viton gasket  36 . The first or upper end of the material column  30  may include a material column end cap  37  coupled to the upper end of the material column body using a 4 inch high-pressure tri-clamp  35  and may be sealed using a 4 inch Viton gasket  36 . The upper material column end cap  37  may further include a pressure gauge  18  ( FIG. 2 ) and a coupling for coupling the other end of the hose  15  from the solvent tank  20 . 
         [0025]    The second or lower end of the material column  30  may include a material column end cap  38  coupled to the lower end of the material column reducer  34 . The extractor apparatus  10  may further include a hose  15  extending from a coupling on the lower end cap of the material column reducer  34  and having a second end connected to a coupling of the inlet of the cryogenic column  40  as shown in  FIG. 6 . 
         [0026]    The cryogenic column or tank  40  is a generally cylindrically shaped member also made from a metal material such as 304 stainless steel. The inlet to the cryogenic column  40  may be located on one side (although it may be located in other positions) and may include a ¼″ NPT coupling which may be coupled to a coiled ¼ inch tubing  42  located within a chamber or passage  41  in the cryogenic column  40 , as best shown in  FIG. 6 . The coiled tubing  42  generally extends the length of the cryogenic column  40  to the generally opposite end of the chamber  41  within the cryogenic column  40  including an endplate  44  closing one end of the chamber or passage  41  within the cryogenic column  40  and having the end of the tube  42  exiting and passing through the endplate in one alternate embodiment. In the present embodiment, the column  40  may include a jacket  45  including an inlet and an outlet  46  for passing cryogenically cooled material for reducing the temperature within the passage  41 . The cryogenic column  40  may further include a chiller inlet located on the wall of the cryogenic column  40  and including a coupling for connection to a cryogenic chiller hose coupled to the outlet of the cryogenic chiller  100 . The chiller inlet may be located near the top of the cryogenic column  40 . The cryogenic column  40  may further include a chiller outlet located on the wall of the cryogenic column  40  (which may be located near the bottom of the chamber) and including a coupling for connection to a cryogenic chiller hose coupled to the inlet of the cryogenic chiller  100 . Accordingly, the coiled tubing  42  within the chamber  41  may be contacted and cooled by the cryogenic cooler  100  material circulated through the chamber  41  of the cryogenic column  40 . The cryogenic cooler  100  circulating the material in the cryogenic dewaxing column  40  may preferably keep the temperature at approximately −40° F. and may preferably operate as low as −120° F. depending upon the performance criteria of the cryogenic cooler  100  and the required performance specifications of the particular extraction process. 
         [0027]    The bottom of the cryogenic column  40  may be coupled to one end of a lipid filtering column  50  using the appropriate clamp and gasket and the solvent and extracted material exiting the end of the tube at the bottom of the cryogenic column  40  may be transferred to the lipid filtering column  50 . The other end of the lipid filtering column  50  may be coupled to a filter stack spacer  51  having an under bore to fit inside the lipid filtering column and designed to hold a filter mesh as well as a paper lipid filter. In one particular embodiment, the paper lipid filter may be a Grade  41  quantitative, circle filter paper ashless, having a typical thickness of 220 μm, a basis weight of generally 85 g/m 2 , and airflow rate of generally 3.4 seconds/100 mL per square inch, and other related performance specifications and made from a high-quality cotton linters material. In one embodiment, the filter stack  51  of the lipid filtering column tank  50  may include a plurality of filter spacers and a plurality of filter mesh and/or a plurality of paper lipid filters as may be desirable for achieving a particular extracted material while using the extraction apparatus  10  to perform the extraction process. 
         [0028]    The filter stack  51  functions to trap the coagulated lipids (from the heat transfer of the cooling of the lipid filtering tank column  40 ) and to separate the coagulated lipids and other coagulated components of the constituent materials that are coagulated via cooling within the chamber  41  within the cooling jacket or chamber  45  of the lipid filtering column  50  and the solvent and the remaining dissolved plant material constituents and solvent (e.g., cannabinoids) may pass through the lipid column tank filter stack  51  and may be transferred from the lipid filtering column  50 . As noted, in one design, the lipid filtering column tank or column  50  may preferably include the cooling chamber  45  surrounding the solvent and dissolved constituent material passage  41  for providing a cooling effect thereto. 
         [0029]    In one alternate version of the extraction apparatus  10 , a lipid column reducer may be included. The lipid column reducer may be coupled to the bottom of the lipid filtering column  50  in a manner similar to the material column reducer  34 , and may further include an end cap including a coupling for coupling a hose  15  which conveys the dissolved cannabinoids and solvent to an inlet in the collection chamber lid  61  of the collection chamber column  60  as best shown in  FIG. 8 . 
         [0030]    As a point of reference, the extraction apparatus  10  of the present disclosure may include a plurality of valves  16  coupled to the hoses  15  and the respective components of the extraction apparatus  10  for isolating each component of the extraction apparatus  10  for operating the method of extraction according to the present disclosure including the use of the hydrocarbon solvent for extracting the constituent materials from the plant material and for operating the closed-loop method of extraction. 
         [0031]    Referring in particular now to  FIG. 8 , the collection chamber column  60  may include an inner chamber  62  for receiving the material from the lipid column  50 . The collection chamber lid  61  may preferably be located at, and coupled to, the top end of the chamber  62  of the column  60 . The extraction apparatus  10  may further include a collection chamber bowl  70  coupled to the bottom end of the chamber column  60 . The collection chamber lid  61  and the collection chamber bowl  70  may each preferably be coupled to the collection chamber column  60  using a clamp  64  including a seal  65 . The collection chamber lid  61  of the collection chamber column  60  may include an outlet coupled to a hose  15  and the other end of the hose  15  may be coupled to the inlet of the expansion filter column  80  ( FIG. 2 ). Notably, the extracted material components from the plant material from column  30  is in a generally liquid form and may be deposited in the collection chamber bowl  70  along with the liquid hydrocarbon solvent. 
         [0032]    The collection chamber bowl  70  may include a heater jacket  76  separate from a heater jacket  67  of the collection chamber  60  for heating the extracted material and the solvent (e.g., liquid hydrocarbon) and causing the solvent to transition from a liquid to a gas while the material collects in the bowl  70 . The heater jackets  67  and  76  may be heated using any known or appropriate heater and may include a recirculating heater  110  coupled to the heater jackets of the collection chamber y and the collection chamber bowl  70  (as well as the expansion/filter column  80  ( FIG. 2 ) as described herein) and may have an operating range of between approximately 30° F. and 400° F. Once all of the hydrocarbon solvent is in the collection chamber bowl  70 , the connection between the collection chamber column  60  and the material column  30  may be closed and the connection between the collection chamber y and the expansion/filter column  80  may be opened. 
         [0033]    The recirculating heater  110  may be initiated (before during or after) to warm the contents of the collection bowl  70  which will cause the hydrocarbon solvent to boil or re-distill and transition into a hydrocarbon gas and/or vapor while the extraction material and components will remain in a liquid state in the collection chamber bowl  70 . In one particular embodiment, the recirculating heater  110  may be a GSC high temperature thermostatic circulating oil bath device  110  available from Shanghai, Kankun Instrument Equipment Company, Limited. 
         [0034]    The expansion/filter column  80  ( FIG. 9  in particular) may include end caps  81  including an appropriate coupling for coupling the hoses  15  to the expansion/filter column  80 . The expansion/filter column  80  may include a jacketed chamber  82  including an inner chamber  82  for receiving the gaseous/vaporous hydrocarbon solvent from the collection chamber  60  as it is boiled off from the collection chamber bowl  70  and a jacket chamber  83  including an inlet and an outlet  84  for circulating the heated fluid there through and further insuring the solvent is sufficiently heated to be completely in a gaseous form prior to being conveyed from the outlet  85  of the expansion/filter column  80  and to the inlet of a hydrocarbon recovery pump  90 . 
         [0035]    The expansion/filter column  80  may further include a molecular sieve desiccant filter (such as a 3A 8×12 desiccant) media  87  located and filling at least a portion of the inner chamber of the column  80  for insuring all water and/or condensation (and thus any potential source of oxygen) is completely removed from the solvent returning to the solvent tank  20 . The desiccant filter media  87  may have a generally crystalline composition and may be particularly useful for absorbing and removing all water and condensation from the gaseous vapor solvent before it exits the expansion/filter column  80 . 
         [0036]    The expansion/filter column  80  may include a lower end cap  81  including an outlet  85  coupled to a hose  15  and the other end of the hose  15  may be coupled to the inlet of the hydrocarbon recovery pump  90 . The hydrocarbon recovery pump  90  draws the gaseous solvent from the expansion/filter column  80  and returns the hydrocarbon solvent to the solvent tank  20  where the hydrocarbon solvent may re-condense under pressure and lowered temperature and the hydrocarbon solvent is again in a liquid state and the entire process may be repeated with the same material in the material column  30  or with new material. The present extraction apparatus  10  allows for the same solvent to be reused or it may be removed as a liquid and new solvent may be added. 
         [0037]    The extraction apparatus  10  may be operated in a passive mode without the use of the hydrocarbon recovery pump  90  and by directly coupling the outlet of the expansion/filter column  80  to the inlet of the solvent tank  20 . The warming effect of the recirculating heat  110  may be sufficient to vaporize the hydrocarbon solvent and return it to the solvent tank  20  but will necessarily take a far greater amount of time without the use of the hydrocarbon recovery pump  90 . 
         [0038]    Based upon limited examples, the passive mode operation will take greater than approximately 7 hours for approximately 18 pounds of liquid solvent to be vaporized and re-condensed in the solvent tank  20 . Similarly, based upon limited examples, the use of the hydrocarbon recovery pump  90  reduces the recovery time to approximately 90 to 120 minutes for approximately 18 pounds of liquid solvent to be vaporized and re-condensed in the solvent tank  20 . Because the desired constituents of the material may be used for human consumption, it may be desired to use a food grade hydrocarbon recovery pump  90 . 
         [0039]    Once the desired extracted components of the plant material are extracted and deposited in the collection bowl  70  with the solvent (after the unwanted lipids and other coagulated constituents are removed in the lipid filtering column  40 ) and after the solvent is removed/boiled off and returned to the solvent tank  20 , the collection bowl  70  may either be easily removed from the collection chamber  60  and the desired extracted constituent materials and components may be stored and/or used as desired or the extracted components of the plant material may be removed from the bowl  70  using a connected outlet. 
         [0040]    While a particular embodiment of the present invention has been shown and described, it may be to be understood that the present invention may be not limited to the embodiments described above, but encompasses any and all embodiments within the scope of the following claims.