System for staged continuous cooled filtration

Abstract
A series of vertically oriented filters of decreasing pore size is sealed from the atmosphere. Pressurized gas is used to force the liquid to be filtered through the filters. The filter stages are thermally insulated from ambient temperatures in order to maintain the liquid passing through at a reduced temperature. Each filter stage has a removable lid, which provides convenient access for replacing the filter cartridge, allowing it to be changed without disturbing the thermally insulated sidewalls of the filter stage.
Description
TECHNICAL FIELD

This application relates to filtering. More specifically, it relates to a multi-stage, chilled filter arranged in a closed-loop configuration.


BACKGROUND

Filtering is a necessary step in the process of essential element extraction. Traditionally, the vertically oriented in-line and T-form filter housings that exist require the main body of the housing to be lifted off the base in order to replace the filter cartridge inside.


In legal, adult-use markets, sales of cannabis extracts are growing ten times faster compared to the sales of dried cannabis, and extracts account for over 60% of revenue. With legalization, consumer preferences are shifting from dried cannabis to extracted cannabis products. However, the scent and flavors of cannabis can he undesirable in many infused products because of excess lipids, plant matter and impurities present in currently available extracts.


U.S. Pat. No. 9,155,767 to Hospodor et al, relates to the extraction of medicinal cannabis compounds into an eluate, by separating a portion of medicinal cannabis compounds contained within a portion of eluate at a first extraction target level, to provide enough clean solvent to continue extraction operations. A high efficiency concentrator processes eluate from one or more tanks, creating clean solvent when extraction targets are met or when clean solvent is exhausted. This manages eluate concentration levels and limits the quantity of concentrated medicinal cannabis compounds on site at any moment in time.


U.S. Pat. No. 9,655,937 to Jones discloses extraction devices, methods, and systems. Example devices have a solvent chamber, a plant material chamber, a collection chamber, and a solvent return that create a sealed, closed-cycle extraction and/or solvent purification process. Any extractable plant material can he used in the disclosed devices, methods, and systems although in some examples some form of the cannabis plant is used.


This background information is provided to reveal information believed by the applicant to be of possible relevance to the present invention. No admission is necessarily intended, nor should be construed, that any of the preceding information constitutes prior art against the present invention.


SUMMARY OF INVENTION

The present invention is directed to a system of chilled filters connected in a closed-loop configuration for use in the extraction of essential elements from plant material. When extracting essential elements, the plant material is washed and/or soaked in a solvent such as ethanol to result in a crude oil and ethanol mixture, for example. The system of chilled filters is used to filter the crude oil and solvent mixture to remove particulate matter, and may be used at different stages of the extraction process. In particular, the filter system may be used as part of a process for extracting cannabinoids from cannabis plants, for example for medicinal purposes.


Disclosed herein is a filtration system comprising a solvent vessel, a plurality of filter stages and the same plurality of transfer tubes. Each filter stage has a thermally insulated cylindrical side wall; a lid that is removable from said wall; a replaceable, elongated filter cartridge; a support configured to locate a base of said filter cartridge centrally in the filter stage; an inlet port in the lid located to introduce liquid into the filter cartridge; an inlet port configured for introducing pressurized gas outside of the filter cartridge; and a base with an outlet port that drains fluid from outside the filter cartridge. The solvent vessel has a thermally insulated side wall; an inlet port configured for introducing pressurized gas; and an outlet tube having a first end located at a bottom region of the solvent vessel and a second end located outside the solvent vessel. The transfer tubes are each removably connected at an outlet end thereof to one of the inlet ports in one of the lids of the filter stages; and at an inlet end thereof to either the second end of the outlet tube of the solvent vessel or the outlet port of another of said filter stages such that the solvent vessel and the filter stages are connected in series.





BRIEF DESCRIPTION OF DRAWINGS

The following drawings illustrate embodiments of the invention, which should not be construed as restricting the scope of the invention in any way.



FIG. 1 is a schematic diagram of the closed-loop, multi-stage, chilled filter system, according to an embodiment of the present invention.



FIG. 2 is a flowchart of a process undertaken using the system of FIG. 1.



FIG. 3 is a schematic diagram of an alternate embodiment of the closed-loop, multi-stage, chilled filter system of the present invention.





DESCRIPTION

A. Glossary


Cannabinoids are a group of chemicals that act on cannabinoid receptors in the body, numerous of which are found in the cannabis plant. Cannabidiol (CBD) is one of the active cannabinoids found in cannabis and is used for medicinal purposes. Tetrahydrocannabinol (THC) is a psychotropic cannabinoid and is the main psychoactive ingredient of cannabis. THC also has medicinal uses. THCa is the non-psychoactive form of THC.


Crude oil is a term for the description of condensed, non-filtered oil, i.e. oil that is non-winterized and not treated via charcoal, clay and silica. The crude oil contains the essential elements. Winterization refers to the removal of unwanted plant waxes and lipids.


B. Apparatus


Referring to FIG. 1, a closed-loop, multi-stage filter system 10 is shown, which includes a solvent vessel 12, a first filter stage 14, a second filter stage 16 and a third filter stage 18 all connected in series, and a collection vessel 19 for collecting filtered liquids from the system.


The solvent vessel 12 contains the crude oil and solvent mixture 20 that is to be filtered. The crude oil and solvent mixture 20 is the liquid that is drawn out of an extractor column, for example, i.e. after the plant material in the extractor column has been washed and/or soaked with the solvent. The crude oil contains essential elements and is dissolved in the solvent. The mixture also contains some unwanted residual plant matter and other undesirable components. Before the crude oil and solvent mixture 20 is placed in the solvent vessel 12, it may undergo one or more pre-filtering steps. For example, the crude oil and solvent mixture 20 may be pre-filtered with activated charcoal, clay and/or silica. The charcoal removes pigments, chlorophyll, heavy metals and particulates. The clay primarily removes pigments. The silica removes very fine plant matter and other particulates.


The stainless steel solvent vessel 12 has an outer wall 22, an inner wall 23 and a base 24. The outer wall 22 and inner wall 23 form a side wall or jacket that is filled with chilled, pressurized liquid CO2 in order to keep the contents of the solvent vessel 12 cool. Thermal insulation 26 is wrapped around the outer wall 22 of the filter stage 12. In other embodiments, the jacket could be evacuated to provide thermal insulation, and the thermal insulation is not necessary. The main requirement is that the inner wall 23 of the solvent vessel be thermally insulated from ambient temperatures of the surrounding atmosphere in order to keep the contents of the vessel cool. Optionally, the jacket includes the base 24 of the solvent vessel 12, and the base may be further thermally insulated.


A removable lid 28 seals to the top of the solvent vessel 12 so that the contents of the vessel can be pressurized via inlet port 30. Nitrogen gas under pressure is fed into the vessel 12 via inlet tube 32 and valve 34. As the solvent vessel 12 is pressurized, the crude oil and solvent mixture 20 within it is forced out of the vessel through exit tube 38, which forms an airtight seal around its outside with the lid 28. The exit tube has an inlet in the bottom region 39 of the solvent vessel 12 so that liquid in the solvent vessel can readily enter it.


The exit tube 38 is connected via an airtight connector 40 outside of the solvent vessel 12 to a transfer tube 42. The transfer tube 42 is connected in turn via an airtight connector 44 and 3-way valve 45 to the inlet port 46 of the first filtering stage 14. Optionally, the transfer tube 42 is thermally insulated. Additional solvent may be introduced via the inlet tube 47 connected to the 3-way valve 45.


The first filter stage 14 has an outer side wall 50 surrounded by a thermal insulator 51, an inner side wall 52 spaced apart from the outer side wall, a lid 54 that seals to the top of the filter stage and a base 56. The outer wall 50 and inner wall 52 form a side wall or jacket that is filled with chilled, pressurized liquid CO2 in order to keep the contents of the filter stage 14 cool. While different configurations of thermal insulation are possible, the main requirement is that the inner wall 52 of the filter stage 14 is thermally insulated from ambient temperatures in order to keep the contents of the stage cool. Optionally, the jacket includes the base 56 of the filter stage 14, and the base may be further thermally insulated. The first stage 14 is sealed against the atmosphere so that it can be pressurized. The first stage 14 is mounted on supports 58.


A support 60, which is positioned in the bottom of the filter stage 14, has a locating feature such as a beveled edge 62. The locating feature 62 serves to position the lower portion or base 61 of a replaceable cylindrical filter cartridge 64 centrally in the filter stage 14. In other embodiments, different shapes of the support are possible. In this embodiment, the filter cartridge is a polypropylene filter with a pore size in the range of 10-15 μm. Other filter sizes may be used in other embodiments. At the top of the filter stage 14 there is a guide ring 66, which serves to direct the filter cartridge 64 along the axis of the filter stage and maintain an upper portion 63 of the filter cartridge aligned axially within the filter stage. In other embodiments the shape of the guide ring 66 is different.


The support 60 has through holes 65 to permit the passage of filtered liquid from a volume 67 of the filter stage above the support to a volume 69 below it, which is adjacent to and in fluid communication with the outlet port 70. The guide 66 has through holes 71 to permit the passage of filtered liquid from a volume 73 above the guide to the volume 67 below the guide. Supports 60 and guides 66 may have slots or gaps with other shapes to provide fluid communication between the volumes 73, 67, 69 of the solvent vessel. The top of the filter cartridge 64 is sealed to the underside of the lid 54 with an O-ring 68.


The crude oil and solvent mixture 20 enters the filter stage 14 through inlet port 46, which directs the mixture into the inner region 75 of the filter cartridge 64. The mixture is then filtered as it passes out through the side walls and base of the filter cartridge 64. The filtered mixture collects in the bottom of the filter stage 14 and passes out of it through exit port 70 in the base 56 of the filter stage,


When required, the cartridge 64 is replaced by disconnecting transfer tube 42 from the lid 54, removing the lid from the filter stage 14, lifting out the cartridge, and then placing a new cartridge in its place. By removing only the lid 54 from the filter stage 14, the side walls 50, 52 can remain in place, together with the thermal insulation 51. This makes it convenient to change the filter cartridge 64, particularly if the filter stage is large. In some embodiments, the side walls 50 can be 1 m tall or more. As well as making the filter cartridge more convenient to change, taller filtration stages can be used within the same headroom compared to stages that require the outer walls to be lifted to change the filter cartridge.


A connector 78 connects a second transfer tube 79 to the outlet port 70 of the filter stage 14. A second port 80 in the lid 54 of the filter stage 14 allows for nitrogen to be supplied directly to the filter stage through tube 82 and valve 84. This is useful in case a blockage occurs upstream in the system 10.


The transfer tube 74 is connected via an airtight connector to the inlet port of the second filtering stage 16. The second filter stage 16 is similar to the first filtering stage 14, except that the filter cartridge 90 has a smaller pore size, which in this embodiment is in the range 3-10 μm. Other filter sizes may be used in other embodiments.


The outlet port at the bottom of the second filter stage 16 is connected via a third transfer tube to an inlet port in the top of the lid of the third filtering stage 18. The third filter stage 18 is similar to the first and second filter stages 14, 16, except that the filter cartridge 92 has an even smaller pore size, which in this embodiment is 1 μm. Other filter sizes may be used in the third filter stage 18 in other embodiments, including filter sizes that are smaller than 1 μm.


The outlet port at the bottom of the third filter stage 18 is connected via a connector and collection pipe 94 to the collection vessel 19, in which the filtered crude oil and solvent mixture 96 is collected. The collection vessel 19 is covered or sealed from the atmosphere with a pressure relief valve 98, although, optionally, it may be uncovered.


A benefit of having the solvent vessel 12 and the three filter stages 14, 16, 18 sealed from the atmosphere is that it reduces the amount of condensation of water into the chilled solvent. This would otherwise dilute the solvent and reduce its effectiveness.


C. Exemplary Process


In use, the crude oil and solvent mixture is chilled either before placing it in the solvent vessel 12 or while it is in the solvent vessel. After this, nitrogen is fed into the solvent vessel 12 at a pressure in the range of about 70-210 kPa (10-30 psi). When the filter system 10 is used for the extraction of essential elements from cannabis and the solvent used is ethanol, the crude oil and solvent mixture is maintained at a temperature between −40° C. and −20° C. in the solvent vessel 12, and remains below −10° C. as it passes through the three filter stages 14, 16, 18.


Referring to FIG. 2, the first step of the process is to chill the crude oil and ethanol mixture in step 200 to a temperature between −40° C. and −20° C. In step 204, the crude oil and ethanol mixture is filtered through a 10-15 μm filter in the first filtering stage 14. In step 208, the crude oil and ethanol mixture is then filtered through a 3-10 μm filter in the second filtering stage 16. In step 212, the crude oil and ethanol mixture is finally filtered through a ≤1 μm filter in the third filtering stage 18.


D. Variations


While the best presently contemplated mode of carrying out the subject matter disclosed and claimed herein has been described, other modes are also possible.


The outlet tube 38 of the solvent vessel 12 may lead downwards from the base 24 of the solvent vessel, in the same way that the outlet ports 70 are located on the filter stages 14, 16, 18.


Referring to FIG. 3, an alternate filter stage 300 is shown. Multiple such filter stages can be connected in series as above. The filter stage 300 includes a removable base 302 with jacketed sidewall 304 and surrounding insulation 306, mounted on legs 308 or other equivalent rack or support. An inlet pipe 310 from the previous stage or from the solvent vessel feeds fluid to be filtered into the stage, via the connector 312 and inlet port 314. The fluid to be filtered is fed into the volume 320 to the outside of the filter cartridge 325. As the fluid is filtered, it passes through the cartridge 325 to the volume 330 on the inside of the cartridge, and then leaves the filter stage via outlet port 340 in the removable base 302. Outlet pipe 342 transfers the filtered fluid to the next stage or to the collection vessel 19. The cartridge 325 is aligned with a guide 344 on the removable base 302 and with a spacer 346 at the upper end of the cartridge. A further inlet port 350 is used to introduce nitrogen gas if needed and/or solvent. Other valve and/or inlets may be included in the filter stage 300, e.g. for evacuating the jacket, filling it with chilled liquid CO2, removing fluids from the stage and/or for introducing fluids into the stage.


The legs 308 or other equivalent support holds the body or main sidewall 304 of the filter stage 300 off the floor by a distance that is sufficient to detach the inlet and outlet pipes 310, 342 from the removable base 302, lower the base and remove/replace the cartridge 325 without having to move the sidewall 304 H1. This is possible when distance H1 is greater than distance H2. Distance H1 is the height of the legs off the floor 360 and distance H2 is the height of the cartridge 325 plus the height of the removable base 302 with its permanent fixtures (i.e. inlet port 314 and outlet port 340). It is important not to have to disturb the jacketed sidewall 304 so that the insulation 306 does not need to be moved.


In some embodiments, the apparatus is portable so that it can be taken to the different sites of various plant growers, to be used on an as-needed basis.


Different filter media may be used in this apparatus, such as clay, charcoal and silica.


In other embodiments within the purview of the present invention, other plant materials besides cannabis may be processed. For example, lavender and hemp may be processed, as well as other plants that produce phytochemicals of interest, which include cannabinoids, terpenes, and flavonoids.


Temperatures that have been given to the nearest degree include all temperatures within a range of ±0.5° C. of the given value.


In general, unless otherwise indicated, singular elements may be in the plural and vice versa with no loss of generality.


Throughout the description, specific details have been set forth in order to provide a more thorough understanding of the invention. However, the invention may be practiced without these particulars. In other instances, well known elements have not been shown or described in detail and repetitions of steps and features have been omitted to avoid unnecessarily obscuring the invention. For example, various ports, valves, tubes and other thermal insulation are not shown for clarity. Accordingly, the specification and drawings are to be regarded in an illustrative, rather than a restrictive, sense.


It will be clear to one having skill in the art that further variations to the specific details disclosed herein can be made, resulting in other embodiments that are within the scope of the invention disclosed. All parameters, dimensions, proportions, relative proportions, materials, and configurations described herein are examples only and may be changed depending on the specific embodiment. Accordingly, the scope of the invention is to be construed in accordance with the substance defined by the following claims.

Claims
  • 1. A filtration system comprising a solvent vessel, a plurality of filter stages and the same plurality of transfer tubes wherein: each filter stage has: a thermally insulated cylindrical side wall;a lid that is removable from said wall;a replaceable, elongated filter cartridge;a support having a surface that positions a base of said filter cartridge centrally in the filter stage;an inlet port in the lid located to introduce liquid into the filter cartridge;an inlet port located to introduce pressurized gas into the filter stage outside of the filter cartridge; anda base with an outlet port that drains fluid from outside the filter cartridge; the solvent vessel has:a thermally insulated side wall;an inlet port for introducing pressurized gas; andan outlet tube having a first end located at a bottom region of the solvent vessel and a second end located outside the solvent vessel;and the transfer tubes are each removably connected: at an outlet end thereof to one of the inlet ports in one of the lids of he filter stages; andat an inlet end thereof to either the second end of the outlet tube of the solvent vessel or the outlet port of another of said filter stages such that the solvent vessel and the filter stages are connected in series.
  • 2. The filtration system of claim 1 further comprising a guide positioned to locate an upper portion of the filter cartridge centrally in the filter stage.
  • 3. The filtration system of claim 1 further comprising a seal between each filter cartridge and the lid of the corresponding filter stage.
  • 4. The filtration system of claim 1, wherein each support defines a fluid communication path from a volume above the support to a volume adjacent the outlet port.
  • 5. The filtration system of claim 1, wherein each guide defines a fluid communication path from a volume above the guide to a volume below the guide.
  • 6. The filtration system of claim 1, wherein there are three filter stages and: a first of the filter stages is connected to the solvent vessel and its filter cartridge has a pore size of 10-15 μm;a second of the filter stages is connected to the first filter stage and its filter cartridge has a pore size of 3-10 μm; andthe third of the filter stages is connected to the second filter stage and its filter cartridge has a pore size of ≤1 μm.
  • 7. The filtration system of claim 1, wherein each filter cartridge is made from polypropylene.
  • 8. The filtration system of claim 1, wherein the solvent vessel has chilled liquid carbon dioxide in its side wall.
  • 9. The filtration system of claim 8, wherein the side wall of the solvent vessel is at a temperature between −20° C. and −40° C.
  • 10. The filtration system of claim 1, wherein each filter stage has chilled liquid carbon dioxide in its side wall.
  • 11. The filtration system of 10, wherein the side walls of the filter stages are at a temperature of ≤−10° C.
  • 12. The filtration system of claim 1, wherein the pressurized gas is nitrogen that is pressurized to 70-210 kPa.
  • 13. The filtration system of claim 1, wherein the filtration system is sealed from an external atmosphere everywhere except at the outlet port of the filter stage that is at an end of the series.
  • 14. The filtration system of claim 13, wherein the outlet port of the filter stage that is at an end of the series discharges into a collection vessel.
  • 15. The filtration system of claim 14, wherein the outlet port of the filter stage that is at the end of the series discharges via a collection tube into the collection vessel.
  • 16. The filtration system of claim 1, wherein: the outlet port of the filter stage that is at the end of the series discharges via a collection tube into a collection vessel; andthe collection vessel is sealed from an external atmosphere via a pressure relief valve.
  • 17. The filtration system of claim 1, wherein the transfer tubes are thermally insulated.
  • 18. The filtration system of claim 1, wherein the bases of the filter stages and a base of the solvent vessel are thermally insulated from an external atmosphere.
  • 19. The filtration system of claim 1, wherein the side walls of one or both of the filter stages and the solvent vessel are evacuated.
  • 20. The filtration system of claim 1, wherein the bases of the filter stages and a base of the solvent vessel are double walled and are either evacuated or filled with liquid carbon dioxide.
  • 21. The filtration system of claim 1, wherein each filter stage comprises a further inlet located to introduce solvent into the filter cartridge.
US Referenced Citations (89)
Number Name Date Kind
526695 Emery Oct 1894 A
2082847 Petty Jun 1937 A
2121208 Milligan Jun 1938 A
2168306 Schutte Aug 1939 A
2190589 Clayton Feb 1940 A
2234916 Jones Mar 1941 A
2309633 Du Pont Feb 1943 A
2325320 Holuba Jul 1943 A
2325635 Schutte Jul 1943 A
2380078 Schutte Jul 1945 A
2534210 Schutte Dec 1950 A
2552525 Wenzelberger May 1951 A
2614110 Davis Oct 1952 A
3067067 Etheridge Dec 1962 A
3072490 Sargeant Jan 1963 A
3254070 Roelen May 1966 A
3270437 Lara Sep 1966 A
3555074 DuBois Jan 1971 A
3817923 Ivanov Jun 1974 A
3968741 Hunt Jul 1976 A
4171265 Battigelli Oct 1979 A
4279824 McKinney Jul 1981 A
4784768 Mathieu Nov 1988 A
5043100 Chang Aug 1991 A
5207929 Sung May 1993 A
5324867 Asaoka Jun 1994 A
5371304 Asaoka Dec 1994 A
5382711 Asaoka Jan 1995 A
5382712 Asaoka Jan 1995 A
5403563 Crosbie Apr 1995 A
5672280 Demopoulos Sep 1997 A
6095153 Kessler Aug 2000 A
6103516 Reverso Aug 2000 A
7622140 Whittle Nov 2009 B2
8197691 Kale Jun 2012 B2
8343553 Hospodor Jan 2013 B2
8497389 Pottathil Jul 2013 B2
9034395 Whittle May 2015 B2
9155767 Hospodor et al. Oct 2015 B2
9199960 Ferri Dec 2015 B2
9242189 Buese et al. Jan 2016 B2
9327210 Jones May 2016 B1
9358259 Hospodor Jun 2016 B2
9655937 Jones May 2017 B2
9669328 Jones Jun 2017 B2
9789147 Jones Oct 2017 B2
9844740 Jones Dec 2017 B2
9873623 Hawks Jan 2018 B2
9987567 Ko Jun 2018 B1
10159908 Thomas Dec 2018 B2
10189762 Oroskar Jan 2019 B1
10195159 Whittle Feb 2019 B2
10238745 Finley Mar 2019 B2
10245525 Ko Apr 2019 B1
20080167486 Parnas Jul 2008 A1
20100016615 Nakaya Jan 2010 A1
20100119606 Whittle May 2010 A1
20110040138 Wilson Feb 2011 A1
20110078918 Koura Apr 2011 A1
20110097626 Waki Apr 2011 A1
20110133120 McGhee Jun 2011 A1
20110245523 Pottathil Oct 2011 A1
20120263804 Hospodor Oct 2012 A1
20150105569 Emo Apr 2015 A1
20150375153 Johnson Dec 2015 A1
20160030860 McGhee Feb 2016 A1
20160091226 Buese Mar 2016 A1
20160136541 Jones May 2016 A1
20160213722 Jones Jul 2016 A1
20160250564 Thomas Sep 2016 A1
20160279535 Jones Sep 2016 A1
20170002292 Cumings Jan 2017 A1
20170003264 Adams Jan 2017 A1
20170043276 Tennant Feb 2017 A1
20170166601 Myerson Jun 2017 A1
20170252385 Jones Sep 2017 A1
20170274298 Jones Sep 2017 A1
20170312327 Jones Nov 2017 A1
20170326472 McGhee Nov 2017 A1
20180008906 Kogon Jan 2018 A1
20180099017 Jones Apr 2018 A1
20180265803 Cumings Sep 2018 A1
20190010421 Emo Jan 2019 A1
20190046998 Stephens Feb 2019 A1
20190099695 Ko Apr 2019 A1
20190099696 Ko Apr 2019 A1
20190111368 Crippen Apr 2019 A1
20190143246 Ko May 2019 A1
20190192992 Ko Jun 2019 A1
Non-Patent Literature Citations (2)
Entry
Patent Cooperation Treaty International Search Report dated Feb. 7, 2019 issued for the co-pending application assigned International Application No. PCT/CA2018/051416 with an International Filing Date of Nov. 8, 2018.
Patent Cooperation Treaty Written Opinon dated Feb. 7, 2019 issued for the co-pending application assigned International Application No. PCT/CA2018/051416 with an International Filing Date of Nov. 8, 2018.
Related Publications (1)
Number Date Country
20190192992 A1 Jun 2019 US
Continuations (1)
Number Date Country
Parent 15809980 Nov 2017 US
Child 16291705 US