INDUCED CAVITATION MIXING APPARATUS
20220023809 · 2022-01-27
Inventors
Cpc classification
B01F35/92
PERFORMING OPERATIONS; TRANSPORTING
B01F31/85
PERFORMING OPERATIONS; TRANSPORTING
International classification
Abstract
A cavitation mixing apparatus is provided for performing separations from solid material using subcritical liquid CO.sub.2. A cavitation inducing device inside a cavitation mixing vessel is held in place with a cavitation mixer mount comprising at least one fluid channel for equalizing gaseous pressure of CO.sub.2 around the cavitation inducing device. Also described is method of separating oils from a crude plant oil mixture by injecting crude plant oil into a pressurized mixing vessel comprising liquid carbon dioxide and mixing the crude oil with the liquid carbon dioxide under pressure using powered induced cavitation, the cavitation mixing vessel comprising an encapsulated cavitation inducing device.
Claims
1. A cavitation mixing apparatus comprising: a cavitation mixing vessel comprising a material inlet and a discharge outlet, the cavitation mixing vessel capable of containing pressurized liquid CO.sub.2; a cavitation inducing device mounted inside the cavitation mixing vessel; an electrical connection for connecting the cavitation inducing device to a power supply through the cavitation mixing vessel; and a cavitation mixer mount for mounting the cavitation inducing device inside the cavitation mixing vessel, the cavitation mixer mount comprising at least one fluid channel for equalizing pressure of CO.sub.2 around the cavitation mixer inside the cavitation mixing vessel.
2. The mixing apparatus of claim 1, wherein the cavitation inducing device is an ultrasonic mixer.
3. The mixing apparatus of claim 2, wherein the ultrasonic mixer produces an ultrasonic vibration at a frequency of at least 20 KHz.
4. The mixing apparatus of claim 2, wherein the ultrasonic mixer operates at a frequency of between 20 KHz to 1.0 MHz.
5. The mixing apparatus of claim 1, wherein the cavitation inducing device is a high shear cavitation mixer.
6. The mixing apparatus of claim 1, further comprising an injection tube to direct crude oil proximate the cavitation inducing device.
7. The mixing apparatus of claim 1, wherein the cavitation mixer mount comprises a plurality of fluid channels.
8. A cavitation dewaxing system comprising: a carbon dioxide reservoir for containing liquid carbon dioxide; a cavitation mixing vessel comprising an encapsulated cavitation inducing device; a separation vessel; and an evaporation vessel.
9. The system of claim 8, wherein the cavitation inducing device is an ultrasonic mixer.
10. The system of claim 8, wherein the cavitation inducing device is a high shear cavitation mixer.
11. The system of claim 8, further comprising a carbon dioxide condenser.
12. The system of claim 8, wherein the separation vessel comprises a filter.
13. The system of claim 8, which is a passive circulation system.
14. A method of separating oils from a crude plant oil mixture, the method comprising: injecting crude plant oil into a pressurized mixing vessel comprising liquid carbon dioxide; and mixing the crude oil with the liquid carbon dioxide under pressure using powered induced cavitation, the cavitation mixing vessel comprising an encapsulated cavitation inducing device.
15. The method of claim 14, where the induced cavitation is provided by an ultrasonic mixer.
16. The method of claim 14, where the induced cavitation is provided by a high shear mixer.
17. The method of claim 14, wherein the pressure of liquid carbon dioxide in the mixing vessel is 80 to 15,000 psi.
18. The method of claim 14, wherein the method is in a batch, semi-continuous, or continuous industrial process.
19. The method of claim 14, further comprising filtering the crude oil and liquid carbon dioxide mixture, and evaporating off the carbon dioxide to isolate a purified plant oil.
Description
BRIEF DESCRIPTION OF THE FIGURES
[0031] For a better understanding of the present invention, as well as other aspects and further features thereof, reference is made to the following description which is to be used in conjunction with the accompanying drawings, where:
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DETAILED DESCRIPTION OF THE INVENTION
[0051] Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
[0052] As used in the specification and claims, the singular forms “a”, “an” and “the” include plural references unless the context clearly dictates otherwise.
[0053] The term “comprising” as used herein will be understood to mean that the list following is non-exhaustive and may or may not include any other additional suitable items, for example one or more further feature(s), component(s) and/or element(s) as appropriate.
[0054] As used herein, the term “closed system” refers to an enclosed environment which limits material flow with the environment and where temperature and pressure are controlled. In a closed system, pressure is maintained in a controlled environment by limiting and controlling material and solvent influx and outflow and keeping the system largely closed from the external environment. In application, in systems that use CO.sub.2 as a solvent, this means maintaining the system above a pressure that enables stabilization of liquid CO.sub.2.
[0055] As used herein, the term “subcritical” refers to a physical state of a fluid wherein the fluid can exists as gas or vapour, liquid, or combination of both vapour and liquid. Subcritical fluids are fluids which are compressed below their critical temperatures, yet kept in the liquid state and used above their boiling points with the use of pressure. Subcritical fluid states vary along a range of temperatures and pressures and are unique to each fluid, which includes solvents, liquids, and the same with dissolved and/or emulsified materials therein. Subcritical conditions for CO.sub.2 are shown in
[0056] As used herein, the term “closed,” as it refers to a system or apparatus, refers to one or more connected vessels that are sealed to the environment. Such systems can optionally be pressurized and are sufficiently sealed such that they can retain an internal pressure, or can contain a solvent from evaporation or leak outside of the system. Closed systems are particularly useful for maintaining increased pressures with pressurized solvents.
[0057] As used herein, the term “induced cavitation” refers to cavitation applied to a fluid where the cavitation is created by a powered device. This is in contrast to passive cavitation which can be caused by structural features as a result of fluid flow, such as, for example, barriers or obstacles such as fins, filters, meshes, and the like.
[0058] Herein is described a cavitation mixing system and induced cavitation mixing apparatus capable of operating at subcritical solvent conditions in a pressure controlled environment. The present system and apparatus can be used for winterization and dewaxing of plant materials, as well as other industrial and chemical processes that benefit from cavitation mixing in a closed environment, particularly those which operate in subcritical solvent conditions in closed systems. By inputting cavitation energy into a closed, induced cavitation mixing vessel, solvent and solute mixtures can benefit from cavitation mixing in a pressurizable closed environment in batch, semi-continuous, or continuous industrial processes. The presently described induced cavitation mixer or mixing apparatus is operable at subcritical conditions and can be used in closed systems and pressure controlled environments.
[0059] Cavitation involves the phenomenon of vapor bubble formation in the solvent fluid experiencing reduced pressure, which is followed by violent bubble collapse. The phenomenon is named cavitation because cavities form when the fluid pressure has been reduced to the vapor pressure of its constituent(s), in this case liquid carbon dioxide. The vapor bubbles expand as they move and suddenly collapse. The violent collapse causes sudden, localized increases in temperature and pressure, as well as tiny but powerful micro jets which hold an enormous amount of kinetic energy and cause physical damage to circulating crude oil and wax particulate, breaking apart the particulate. Particulate disruption caused by the cavitation improves access of the solvent to desirable oils inside the wax particulate and increases the yield from extractive and separative processes.
[0060] The present apparatus and separation vessel with integrated induced cavitation mixing device are compatible with the high pressures required for subcritical fluid dewaxing and separation, as well as other processes that benefit from induced cavitation in closed system mixing in a pressure controlled environment. A commonly used subcritical solvent is liquid carbon dioxide, however it is understood that other solvents may be used, as well as combinations of solvents with and without CO.sub.2. Carbon dioxide will be referred to herein as an example solvent, however it is understood that the presently described devices, apparatus and methods can be used with any subcritical fluid, or any solvent or industrial mixing process done in a closed or pressure-controlled environment. The present apparatus can also be used in standard or atmospheric solvent conditions and under other temperatures and pressures where solvent is retained inside a closed vessel system or in a closed process.
[0061] The critical point of CO.sub.2 is easily accessible as it has a critical temperature of 31° C. and critical pressure 73.9 bar (72.9 atm). Above the critical point CO.sub.2 behaves as a supercritical fluid above its critical temperature (304.25 K, 31.10° C., 87.98° F.) and critical pressure (72.9 atm, 7.39 MPa, 1,071 psi, 73.9 bar). Subcritical solvents are of interest when extracting yields with increased volumes of terpenoids, flavonoids, and other such volatile plant materials at least because subcritical carbon dioxide runs at milder separation parameters than other solvents, targeting those volatile compounds. Through only modest changes in the temperature and pressure, the physical properties of CO.sub.2 can be manipulated. CO.sub.2 can be a stable liquid from about 80 psi and roughly −57° C. which would prove a very low pressure extraction with very low solubility, however the pressure of CO.sub.2 can be increased so long as the process stays below 31° C., which is the critical temperature limit.
[0062] The solvent power of subcritical fluids is dependent on the temperature utilized and temperature helps to increase solvency. In contrast, pressure is used to help retain the liquid state of the fluid. Subcritical separations at low temperature and low pressure take more time than superfluid separations, but they can be used effectively to retain the essential oils terpenes and other sensitive chemicals within the plant. Subcritical CO.sub.2 separation is often preferred because the milder conditions result in production of a lighter colored extract, fewer waxes, and resins, and retention of more volatile oils. Subcritical separation can also be used effectively to scrub the extractant matrix of any valuable compounds and achieve a full-spectrum extraction. In any closed system with controlled pressure, embedded mixing systems can improve extraction efficiency as well as product yield and purity by improving in situ mixing.
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[0064] The CO.sub.2 solvent is supplied to the cavitation dewaxing assembly from fluid reservoir 102 to cavitation mixing vessel 104, optionally with the use of a fluid pump. The assembly can also be set up as a passive circulation system using only fluid flow through temperature control, and the optional addition of a pump can be used with either liquid (cooling and pumping) or vapor recovery (compressing and cooling), and could be added in different positions on the process flow. The fluid reservoir 102 holds the fluid solvent at a temperature and pressure to maintain the subcritical fluid properties of the solvent. Preferably the subcritical fluid is saturated liquid CO.sub.2. The CO.sub.2 reservoir can be further chilled via a refrigerated jacket to maintain CO.sub.2 in a liquid phase. The assembly can further comprise a working fluid accumulator which can also be used to store liquid/gas subcritical working fluid. Working fluid is the general term of circulating fluid which is being used as a solvent in the extraction or separation process. In the present system the preferred working fluid is CO.sub.2, optionally mixed with a co-solvent which stay in a liquid phase through the process. Some optional co-solvents include ethanol, methanol, hexane, heptane, propane, butane, and combinations thereof. Co-solvents may be used in ratios from 0 parts to 100:1 (co-solvent:input material) with a total solvent ratio from 1:1 to 100:1 (solvent solution:oils). Multiple injection nozzles may also be provided in the system for one or more additional oils and/or co-solvent injection into the system. The flow rate of CO.sub.2 through the system and control of the flow rate can be passive by controlling the rate of evaporation, or active by pumping such as by controlling the flow of liquid inlet, or both. A high pressure multi-phase pump can also handle subcritical fluid solvents by enabling both the compression of gasses and/or the pumping of a fluid. Any pump known to the skilled person useful in subcritical fluid systems may be used, such as, for example, a liquid pump optionally in combination with one or more suitable compressor. An optional cross flow heat exchanger can also be used to control the temperature of CO.sub.2 as required. From the fluid reservoir 102, CO.sub.2 is provided to cavitation mixing vessel 104 where temperature and pressure conditions are adjusted to the desired conditions to maintain a balance of liquid and gas CO.sub.2 in the vessel. Following emulsification the solution travels into the separation/filter vessel 106 where the density of CO.sub.2 can be controlled by adjusting the temperature to promote density separation of compounds. For example in isobaric condition of 500 psi CO.sub.2 has a density from 1.08 g/ml @−30C to 0.94 g/ml @−2C, as shown in
[0065] The separation/filter vessel 106 is preferably located below the cavitation mixing vessel 104 such that the separation/filter vessel 106 can be gravity-assisted to fill completely with the mixed CO.sub.2/extract mixture from the cavitation mixing vessel 104. The separation/filter vessel 106 can also be cooled by a refrigerated jacket. In the assembly shown, the oil/extract mixture is gravity fed into the top of the separation/filter vessel 106 in such a way as to cause as little agitation inside the separation vessel as possible. The separation/filter vessel 106 will begin to accumulate the solidified fats and waxes near the top as the oils and waxes separate from the CO.sub.2 mixture due to low temperatures. A separation vessel inlet tube 126 on the inlet of separation/filter vessel 106 allows incoming CO.sub.2/extract mixture from the cavitation mixing vessel 104 to pass through any oil layer in the separation/filter vessel 106 without excessive agitation. A filter element 130 at the bottom of the separation/filter vessel 106, optionally sintered and/or made from stainless steel, can prevent fats and waxes from exiting the vessel while allowing the remaining CO.sub.2 mixture with desired compounds for collection (minus the fats and waxes) through. An evaporation vessel inlet tube 124 on the evaporation vessel 108 is preferably located at the same height as the separation vessel inlet. A high purity gas filter can also be integrated into the system assembly as a variety of locations as needed. In particular, a coalescing high purity gas filter can be used to scrub any leftover compounds and water vapor from the gas stream. Other optional components which can be integrated into the assembly can include one or more of a condensing heat exchanger, an air cooled process chiller to cool accumulator and/or condenser, an air compressor, and a hot water circulating system for the heat exchanger.
[0066] The system assembly can also optionally have an electronic control system having circuitry, hardware, and software for controlling and reporting one or more of: inputting batch parameters; separation tracking; monitoring and recording system parameters at defined intervals; printing batch records with associated pressures and temperatures; controlling separation parameters based on user input to adjust pressure, temperature, flow, or other process parameters; initiating cleaning cycles; detecting system failures; initiating emergency shutdown procedures; and connecting to one or more networks for monitoring and reporting. The electronic control system can comprise one or more microcontrollers connected wired or wirelessly to one or more sensors, the one or more sensors for detecting, for example, pressure, temperature, fluid flow, and other fluid properties such as colour, viscosity, turbidity, and other properties. The assembly can further comprise one or more shunts or valves which can direct small amounts of process fluid to sensor or analytical devices to test, monitor, and control aspects of the separation/extraction, optionally providing feedback information to the system to change one or more physical parameters of the process. In one example, the operation of the cavitation mixer in the separation/filter vessel 106 can be adjusted to increase or decrease speed or frequency to provide optimal cavitation for the material being processed. Other physical parameters that can be controlled using the control system include but are not limited to pressure, temperature, fluid flow rates. In addition, the separation system can further comprise one or more electric heaters, electric motor controls, emergency stop circuitry, or automatic closure of an accumulator tank, and automatic switching of process valves, all of which can be optionally monitored and controlled by the control system. An in situ measurement device can also be used for determining the completion and real time separation rate of the extracted material, in one example, of dissolved plant extracts and cannabinoids. The system or assembly itself can be integrated directly into a CO.sub.2 extraction process, where the input material is the extraction collection material.
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[0072] Cavitation mixer 202 shown comprises a piezoelectric transducer 204 connected to an electrical power source to generate an ultrasonic vibration, which is transferred to an optional sonotrode booster 208 connected to sonication horn 206 with horn end 210. Piezoelectric transducer 204 is joined to the horn 210 optionally through a vibration transmitting block or sonotrode booster 208, which is used to amplify the vibration amplitude generated by the transducer 204, as the vibration amplitude of the transducer itself is sometimes not sufficient for mixing in many industrial processes. The optional sonotrode booster 208 can thereby provide an acoustic gain to the ultrasonic vibrations. The sonication horn 206 can have a variety of shapes and sizes, and can be conical, straight, or barbell shaped as desired. The horn end 210 configuration can be variable in size, cross-sectional shape, and surface area and can be pointed, flat, rounded, and have a variety of cross-sectional areas and shapes. The booster, horn, or both can also clad or plated with a reflective material that reflects ultrasonic vibrations or lessens loss of ultrasonic energy being transmitted to the horn.
[0073] The cavitation mixing vessel 200 accepts a metered amount of raw plant oils and waxes, also referred to as crude oil, through material inlet 222 with optional extended injection tube 244 and uses a cavitation mixer attachment to combine the extract with incoming clean CO.sub.2 fed through solvent inlet 212 from the CO.sub.2 reservoir. Homogeneous discharge outlet 214 just below the fluid interface 230 directs CO.sub.2 solvent mixed with cavitation-treated and solubilized or emulsified oils and waxes out of the cavitation mixing vessel 200. The cavitation mixing vessel 200 is cooled through a refrigerated jacket and cooling jacket 224 with cooling jacket port 226 to maintain the liquid phase of CO.sub.2 inside the vessel and to extract the heat input from the cavitation mixing vessel 200. The raw oil in the plant extract benefits from thorough mixing provided by cavitation to separate the fats and waxes from the desired compounds. The mixing time and amount in a continuous feed process can be controlled by the injection rate of the raw extract into the cavitation mixing vessel 200 and the injection rate of clean solvent through solvent inlet 212. The end surface of the induced cavitation device or cavitation mixer 202 is preferably positioned in a location within the effective zone of cavitation below the fluid interface 230 as initiated by the mixing device relative to the injection tube 244 such that crude oil is directed in the immediate vicinity of the horn end 210 of cavitation mixer 202. The liquid flow path inside the vessel is such that the entering liquid and crude oil strikes the end of the horn at a direction normal to the horn end 210, then flows across the surface of the horn before leaving the cavitation mixing vessel 200. The cavitation mixing vessel 200 has a high pressure electrical pass through fitting 216 for supplying power to the induced cavitation mixer 202, and adjacent pressure safety valve 218 and pressure sensor 220. The ultrasonic energy generated by the sonotrode can have a frequency in the range of, for example, 20 KHz to 1.0 MHz, or preferably from 20 KHz to 70 KHz. The frequency of the current is chosen to be the resonant frequency of the tool, so the entire sonotrode acts as a half-wavelength resonator, vibrating lengthwise with standing waves at its resonant frequency. The amplitude of sonotrode vibration is generally small, ranging from about 13 to 130 micrometres.
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[0082] All publications, patents and patent applications mentioned in this specification are indicative of the level of skill of those skilled in the art to which this invention pertains and are herein incorporated by reference. The invention being thus described, it will be obvious that the same may be varied in many ways. Such variations are not to be regarded as a departure from the scope of the invention, and all such modifications as would be obvious to one skilled in the art are intended to be included within the scope of the following claims.