METHOD OF EXTRACTING POLYHYDROXYLATED FATTY ALCOHOLS USING SUPERCRITICAL CO2

Abstract

A method of extracting Polyhydroxylated Fatty Alcohols is disclosed. The method may include: inserting crushed avocado seeds to one or more extraction chambers; flowing supercritical CO.sub.2 fluid through the crushed avocado seeds in one or more extraction chambers; and separating from the supercritical CO.sub.2 flown through the crushed avocado seeds the Polyhydroxylated Fatty Alcohols extracted and dissolved in the supercritical CO.sub.2. The supercritical CO.sub.2 fluid may be the only solvent used for dissolving and extracting the Polyhydroxylated Fatty Alcohols.

Claims

1. A method of extracting Polyhydroxylated Fatty Alcohols (PFA) comprising: inserting crushed avocado seeds to one or more extraction chambers; flowing supercritical CO.sub.2fluid, at a pressure range of 100 bar to 200 bar, through the crushed avocado seeds in the one or more extraction chambers; and separating from the supercritical CO.sub.2flown through the crushed avocado seeds the PFA extracted and dissolved in the supercritical CO.sub.2, wherein the supercritical CO.sub.2fluid being the only solvent used for dissolving and extracting the PFA from the seeds.

2. The method of claim 1, further comprising drying the crushed avocado seeds to a humidity level of at most 20 wt.% before the insertion of the crushed avocado seeds to the one or more extraction chambers

3. The method of claim 1, wherein the crushed avocado seeds have a particle size of at most 2 mm.

4. The method of claim 1, wherein the supercritical CO.sub.2 fluid has a temperature range of 30° C. to 80° C.

5. The method of claim 1 according to any one of the preceding claims, wherein flowing the supercritical CO.sub.2fluid comprises: obtaining liquidized CO.sub.2; increasing the pressure of the liquidized CO.sub.2 to reach a required supercritical pressure; heating the pressurized liquid CO.sub.2 to reach a required supercritical temperature; and inserting the supercritical CO.sub.2 fluid to the one or more extraction chambers.

6. The method of claim 1, wherein separating the PFA comprises: introducing the supercritical CO.sub.2 flown through the crushed avocado seeds into a separator having two or more separation stages.

7. The method of claim 1, wherein for every kilogram, of crushed avocado seeds at least 1 gram of the PFA is extracted and collected.

8. The method of claim 7, wherein a time of production of the at least 1 gram of the PFA from 1 kg of crushed avocado seeds is at most 5 hours.

9. The method of claim 1, further comprising: collecting the CO.sub.2separated from the PFA; and recycling the collected CO.sub.2.

10. A non-toxic PFA extract comprising less than 0.5 ppm cosolvent.

Description

BRIEF DESCRIPTION OF THE DRAWINGS

[0013] The subject matter regarded as the invention is particularly pointed out and distinctly claimed in the concluding portion of the specification. The invention, however, both as to organization and method of operation, together with objects, features, and advantages thereof, may best be understood by reference to the following detailed description when read with the accompanying drawings in which:

[0014] FIG. 1 is an illusration of an extraction system according to some embodiments of the invention; and

[0015] FIG. 2 is a flowchart of a method of extracting PFA using supercritical CO.sub.2 according to some embodiments of the invention.

[0016] It will be appreciated that for simplicity and clarity of illustration, elements shown in the figures have not necessarily been drawn to scale. For example, the dimensions of some of the elements may be exaggerated relative to other elements for clarity. Further, where considered appropriate, reference numerals may be repeated among the figures to indicate corresponding or analogous elements.

[0017] DETAILED DESCRIPTION OF EMBODIMENTS OF THE INVENTION

[0018] In the following detailed description, numerous specific details are set forth in order to provide a thorough understanding of the invention. However, it will be understood by those skilled in the art that the present invention may be practiced without these specific details. In other instances, well-known methods, procedures, and components, modules, units and/or circuits have not been described in detail so as not to obscure the invention. Some features or elements described with respect to one embodiment may be combined with features or elements described with respect to other embodiments. For the sake of clarity, discussion of same or similar features or elements may not be repeated.

[0019] Although embodiments of the invention are not limited in this regard, discussions utilizing terms such as, for example, “processing”, “computing”, “calculating”, “determining”, “establishing”, “analyzing”, “checking”, or the like, may refer to operation(s) and/or process(es) of a computer, a computing platform, a computing system, or other electronic computing device, that manipulates and/or transforms data represented as physical (e.g., electronic) quantities within the computer's registers and/or memories into other data similarly represented as physical quantities within the computer's registers and/or memories or other information non-transitory storage medium that may store instructions to perform operations and/or processes. Although embodiments of the invention are not limited in this regard, the terms “plurality” and “a plurality” as used herein may include, for example, “multiple” or “two or more”. The terms “plurality” or “a plurality” may be used throughout the specification to describe two or more components, devices, elements, units, parameters, or the like. The term set when used herein may include one or more items. Unless explicitly stated, the method embodiments described herein are not constrained to a particular order or sequence. Additionally, some of the described method embodiments or elements thereof can occur or be performed simultaneously, at the same point in time, or concurrently.

[0020] Aspects of the invention may be directed to a method of extracting all molecules of PFA, both the polar and non-polar molecules, using supercritical CO.sub.2 without any additional cosolvent. Although, prior art extraction method of oils from seeds using supercritical CO.sub.2 requires the addition of 7-15wt.% of cosolvent, the applicant has surprisingly found that such an addition is not required when extracting PFA using supercritical CO.sub.2 from avocado seeds, while maintaining or even increasing the required production yield. Furthermore, although supercritical CO.sub.2 is known to be non-polar solvent, a method of extraction according to embodiments of the invention resulted in the extraction of both the polar and non-polar PFA molecules. Therefore, unlike the prior art methods, a method and an extract according to some embodiments of the invention may be completely non-toxic, or cosolvent free. A method according to embodiments of the invention may be executed by any known supercritical CO.sub.2 extraction system, for example, the system illustrated in FIG. 1.

[0021] Referring now to FIG. 1 which is an illusration of an extraction system 100 according to some embodiments of the invention. System 100 may include an extraction unit 110 and a separation unit 120. Extraction unit 110 may include: a CO.sub.2 reservoir 112 configured to hold CO.sub.2, a condenser 113 configured to condense and liquidize the CO.sub.2, a pump 114 (e.g., a dual piston pump) for increasing the extraction pressure of the CO.sub.2 and a heater 115 for heating the pressurized CO.sub.2 to supercritical conditions. Accordingly, the CO.sub.2 leaving heater 115 is a supercritical CO.sub.2 fluid. As used herein, supercritical CO.sub.2 fluid may refer to a CO.sub.2 fluid that may have a density of liquid CO.sub.2(e.g., 600-1600 kg/m.sup.3) and a dissolving power (solubility) of CO.sub.2 gas. In some embodiments, supercritical CO.sub.2 fluid may have a temperature range of 30° C. to 80° C. In some embodiments, supercritical CO.sub.2 fluid may have pressure range of 100 bar to 400 bar, for example, 100 bar to 200 bar.

[0022] In some embodiments, the supercritical CO.sub.2 fluid is introduced into one or more extraction chambers 116 included in extraction unit 110. One or more extraction chambers 116 may be preloaded with crushed seeds, for example, crushed avocado seeds. The supercritical CO.sub.2 fluid is flown through the crushed seeds in at least one of one or more extraction chambers 116. In some embodiments, PFA may be dissolved from the crushed seeds into the supercritical CO.sub.2 fluid to form a supercritical CO.sub.2 solution. In some embodiments, other materials may also be extracted from the crushed avocado seeds in the process, for example, tocopherols, carotenoids, unsaturated fatty acids, etc. It should be appreciated by those skilled in the art that a cosolvent reservoir is not required in systems according to embodiments of the present invention.

[0023] In some embodiments, the supercritical CO.sub.2 solution that includes the extracted PFA may be introduced into separation unit 120 to be separated. Separation unit 120 may include one or more separators 122 each being in fluid connection to one or more tanks 124. In some embodiments, separation unit 120 may further include one or more filters and one or more containers (not illustrated) for collecting the separated PFA. In some embodiments, separators 122 may each include a tank at which the supercritical CO.sub.2 solution may be depressurized using aback-pressure regulator and maintained in a desired temperature (e.g., 30-60° C.) until the CO.sub.2 may gradually be converted into gas. In some embodiments, in order to avoid pressure and temperature changes the processes may be carried out is several stages in two or more separators 122. The evaporated CO.sub.2 may be recycled and condensed back into a liquid CO.sub.2.

[0024] It should be understood by one skilled in the art that the invention is not limited to system 100 disclosed herein and illustrated in FIG. 1, which is given as an example only.

[0025] Reference is made to FIG. 2 which is a flowchart of a method of extracting PFA according to some embodiments of the invention. In step 210, crushed avocado seeds may be introduced to one or more extraction chambers (e.g., one or more chambers 116). In some embodiments, the avocado seeds may be crushed using any known method, for example, grinding, milling, etc. In some embodiments, the crushed avocado seeds may have a particle size (e.g., average diameter) of at most, 2 mm, 1 mm, 500 μm, 150 μm or less. In some embodiments, the smaller the particle size the higher is the specific surface area exposed to the supercritical CO.sub.2 fluid, therefore the higher is the extraction rate of the PFA from each particle. Therefore, the smaller the particle size the higher is the yield of the extraction process.

[0026] Undried raw avocado seeds may be crushed at room temperature. In some embodiments, the crushed seeds may be dried such that the crushed seeds may have a humidity level of at most 20 wt.%, for example, at most 18 wt.%, at most 15 wt.% at most 12 wt.% or lower. PFA are insoluble in water therefore the presence of water is an impediment to the diffusion of the PFA into the supercritical CO.sub.2 fluid. Furthremore, it is easier to recycle the CO.sub.2 if it does not contain water.

[0027] In some embodiments, the crushed seeds may be incubated for at least 24 hours, for example, about 48 hours, at a temperature range of 15-45 ° C.

[0028] In step 220, supercritical CO.sub.2 fluid may be flown through the crushed avocado seeds in at least one of the one or more extraction chambers (e.g., chambers 116). The supercritical CO.sub.2 fluid may be obtained by pressurizing and heating CO.sub.2 into supercritical conditions as disclosed hereinabove with respect to FIG. 1. Some embodiments of the invention may include: obtaining liquidized CO.sub.2, increasing the pressure of the liquidized CO.sub.2 to reach a required supercritical pressure and heating the pressurized liquid CO.sub.2 to reach a required supercritical temperature; and inserting the supercritical CO.sub.2 fluid to at least one extraction chambers.

[0029] In some embodiments, the supercritical CO.sub.2fluid may have a density of liquid CO.sub.2and a dissolving power (solubility) of the PFA in the supercritical CO.sub.2gas. In some embodiments, the supercritical CO.sub.2fluid may have a temperature range of 30° C. to 80° C. In some embodiments, the supercritical CO.sub.2fluid has pressure range of 100 bar to 400 bar, for example, 200 bar.

[0030] In some embodiments, as the supercritical CO.sub.2fluid is flowing and wetting the crushed avocado seeds, PFA may be extracted from the surface area of the crushed avocado seed particles. The PFA may be dissolved into the supercritical CO.sub.2fluid. In some embodiments, the PFA dissolved into the supercritical CO.sub.2fluid may include both polar and non-polar PFA molecules.

[0031] In step 230, PFA extracted and dissolved in the supercritical CO.sub.2may be separated from the supercritical CO.sub.2flown through the crushed avocado seeds. In some embodiments, PFA from within the avocado seed cells may diffuse from the cells and dissolve in the supercritical CO.sub.2. In some embodiments, the supercritical CO.sub.2fluid may be the only solvent used for dissolving and extracting the PFA.

[0032] In some embodiments, the extracted PFA may be non-toxic and/or cosolvent free extracted PFA including both polar and non-polar PFA molecules. As used herein, the term non-toxic refers to cosolvent amounts which are lower than the required standard (e.g., lower than 20 ppm) or the lowest detection limit, for example, lower than 0.5 ppm, lower than 0.1 ppm or lower than 0.06 ppm measured, for example, using Headspace Gas Chromatograph (HSGC). In some embodiments, the lowest detection limit may depend form the type of product material (oil, paste, solid, solution, etc.), the type of the toxic cosolvent and the like.

[0033] In some embodiments, for every kg of crushed avocado seeds at least 1-gram, for example, at least 1.4-gram, 1.5-gram, 2-gram, 3-gram or more. of the PFA may be extracted and collected. In some embodiments, a time of production of at least 1 gram of the PFA from 1 kg of crushed avocado seeds may be at most 5 hours.

Experimental results

[0034] Three batches of 2-4.5 kg of crushed avocado seeds were inserted into extraction chambers, such as chambers 116. Each batch was exposed to 8 kg of flowing supercritical CO.sub.2 fluid having pressure of: 100, 350 and 450 bar at 45° C. No additional cosolvent was used in the process. The flowing rate of the supercritical CO.sub.2 fluid was 21-25 kg/hour. Table 1 summarized the results of obtained PFA.

TABLE-US-00001 TABLE 1 Batch No. 1 2 3 Avocado species Reed Hass Pinkerton Weight of crushed 2.02 4.5 3.2 seeds [Kg] Moisture content 8-12% 8-12% 8-12% Total production time 4 h 4 h 4 h 35 min Total quantity of PFA 26.0 gr 65.1 gr 53.0 gr extraction ** Total Production Yield 1.3% 1.4% 1.7% (%, dry weight) ** PFA extraction may include PFA (e.g., 10-40 wt. %) and other additives, such as, tocopherols, carotenoids and unsaturated fatty acids. The PFA included both polar and non-polar PFA molecules.

[0035] As known in the art the typical production yield of solvents (e.g., ethyl acetate, hexane, etc.) based extraction process is 0.6-0.8%. As clearly shown in Table 1 above, a process according to embodiments of the invention may result in a higher production yield without the use of any cosolvent.

[0036] Using the same raw material as in the previous experiments, additional five batches of 10-15 kg and 2 batches of 87-92 kg of crushed avocado seeds were inserted into extraction chambers, such as chambers 116. Small scale batches were exposed to 115-430 kg of flowing supercritical CO.sub.2fluid and Large-scale batches were exposed to 1,350 kg of flowing supercritical CO.sub.2fluid, having pressure of: 100, 120, 160 and optionally also 280 bar at 45° C. No additional cosolvent was used in the process. The flowing rate of the supercritical CO.sub.2 fluid was 30-67 kg/hour for small scale batches and 430 kg/hour for large-scale batches. Table 2 summarized the results of obtained PFA.

TABLE-US-00002 TABLE 2 Batch No. 1 2 3 4 5 6 7 Avocado species Reed Reed Reed Reed Reed Reed Hass Weight of crushed 15.0 .sup.   13.5 .sup.   13.5 .sup.   13.5 .sup.   10.0 .sup.   87.7 .sup.   91.5  seeds [Kg] Extraction Pressure 100 bar 280 bar* 100 bar 120 bar 160 bar 120 bar 160 bar 120 bar 160 bar 160 bar (bar) Total quantity of 320 g 295 g*** 227 g 310 g 142 g 2.09 kg 2.12 PFA extraction ** Total Production 2.1% 2.2% 1.7% 2.3% 1.4% 2.4%  2.3% Yield (%, dry weight) *A larger number of undesirable compounds were extracted at this stage using pressure of 280 bar ** PFA extraction may include PFA (e.g., 10-40 wt. %) and other additives, such as, sterols, tocopherols, carotenoids and unsaturated fatty acids. The PFA included both polar and non-polar PFA molecules. ***The highest percent of PFA in the extract obtained at the higher pressure.

[0037] As shows in table 2, as pressure increases the yield increases and the selectivity decreases, accordingly, more compounds are extracted which lead to a change in the appearance and odor of the whole extract. Batches that were extracted above 200 bar appear as dark green extract with an unpleasant odor and larger number of undesirable compounds (such as pigments). Higher pressure during extraction enable producing in higher yields.

[0038] Therefore, process according to embodiments of the invention is toxin-free (e.g., non-toxic) and may provide a high quality PFA, free of any possible residual toxic solvents.

[0039] While certain features of the invention have been illustrated and described herein, many modifications, substitutions, changes, and equivalents may occur to those skilled in the art. It is, therefore, to be understood that the appended claims are intended to cover all such modifications and changes as fall within the true spirit of the invention.

[0040] Various embodiments have been presented. Each of these embodiments may of course include features from other embodiments presented, and embodiments not specifically described may include various features described herein.