Counter current reprocessing regime for the continuous refining of edible oils and fats

Abstract

A system for purifying edible oils includes a train of fiber reactors arranged in series and where the oil and water run counter current from reactor to reactor. The edible oils may be first neutralized with an alkali solution and then washed with water to thereby remove impurities such as free fatty acids, mono- and diacylglycerols, phospholipids, glycolipids, trace metals, soap and unsaponifiable matter. The system allows for continuous, high-yield production of improved quality edible oils through the implementation of surge vessels and the reprocessing of emulsions from the interface. In addition, the system also describes the implementation of acid splitting to reprocess the aqueous waste stream prior to implementing a water purification schema.

Description

Patent Application Attorney Docket No. 58566.45WO01COUNTER CURRENT REPROCESSING REGIME FOR THE CONTINUOUS REFINING OF EDIBLE DIES AND FATS SCOTT KOHL, DAVID SHARP, MARIO RIVERA, JONATHAN CAMPBELL & WILLIAM LANIERCROSS-REFERENCE TO RELATED APPLICATIONS

[0001] The present application claims priority to U.S. Provisional Application No. 63 / 760,026 filed February 18, 2025, and entitled “COUNTER CURRENT REPROCESSING REGIME FOR THE CONTINUOUS REFINING OF EDIBLE OILS AND FATS,” which is hereby incorporated by reference in its entirety.TECHNICAL FIELD OF THE DISCLOSURE

[0002] The present disclosure generally relates to the chemical refining of edible oils and fats (e.g., crude cocoa butter). More specifically, the present disclosure relates to design and operational modes of a high throughput fiber reactor for industrial scale chemical refining in continuous flow using a counter current configuration, surge tanks for better operation control, the reprocessing of emulsions back through the reactor towers, and the recovery of in-process water through an acid splitting process.BACKGROUND

[0003] Chemical and physical processes for the refining of edible oils and fats have emerged to address challenges in the poor quality and shelf life of oils that were produced through solvent extractions. Such processes typically include a combination of degumming, neutralization, and dewaxing steps which often terminate in a final bleaching or deodorization step to ensure optimal taste, aroma, appearance, and stability of the edible oil product. The optimal process flow depends on several factors such as the type of oil, the corresponding impurity profile, and the markets the final oil product aims to supply.

[0004] In the confectionary industry, Theobroma oil (i.e., cocoa butter) is an essential ingredient which contributes to the gloss, texture, and crystallization behavior of chocolate. Crude cocoa butter is predominantly composed of triacylglycerides (also referred to herein as tri acylglycerols or TAGs) (>95 wt%) but typically has a sour flavor and odor due to minor contaminants such as free fatty acids (FFAs), mono- and diacylglycerols (DAGs), phospholipids, glycolipids, trace metals and unsaponifiable matter. To comply with the EU directive 2000 / 36 / EC (2000), which limits the FFAs and unsaponifiable matter concentrations to <1.75 wt% and <0.5 wt%, crude cocoaPatent Application Attorney Docket No. 58566.45WO01butter must undergo refining if it is to meet the mandated specifications. Although steam refining is typically successful in removing most quality-compromising contaminants, the process is energy intensive, requires temperatures in excess of 200°C, and results in poor crystallization behavior and a less desirable bland taste in the final purified butter. Consequently, a mild and cost-effective chemical refining process that removes FFAs and other undesirable contaminants is necessary to obtain good quality cocoa butter amenable to a mild sequential (e.g., a lower temperature of 160 °C) steam stripping deodorization step that preserves the residual aroma desired in the final product.

[0005] The financial incentive for a chemical solution is growing considering recent trends indicating a steady annual increase of the volume of cocoa butter with >1.75 wt% concentration of FFAs due to improper handling of cocoa beans, unpredictable crop history, and / or wet postharvest conditions. At higher concentrations, free fatty acids negatively impact the butter’s crystallization behavior and decrease its stability against oxidation. The effect of other organic contaminants, such as phospholipids, on the crystallization behavior of cocoa butter is more complex and has been reported to be species dependent. Generally, phospholipid concentrations comprise a range of 0.26-0.94 wt% of cocoa butter mass. The structural characterization of these compounds has identified a wide compositional array including diphosphatidylglycerol (DPG), phosphatidylglycerol (PG), phosphatidylethanolamine (PE), phosphatidylcholine (PC), phosphatidylinositol (PI), lysophosphatidylethanolamine (LPE), lysophosphatidylcholine (LPC) and phosphatidic acid (PA).

[0006] Due to the different packing configurations the triglycerides (predominantly POP, SOS, and POS) in cocoa butter can adopt, cocoa butter is a polymorphous fat which has unique physical properties such as multiple-melting points and variable crystallization kinetics. As a result, the bulk phase behavior of cocoa butter in standard chemical refining processes using aqueous solutions can be quite unpredictable and particularly sensitive to batch dependent fluctuations in contaminants. For example, in the FFA neutralization process using aqueous alkali, phospholipids present in the butter can behave as aggressive surfactants and form lipophilic mixed aggregates with the generated FFA salts. Although the concentration of phospholipids in crude cocoa butter is low relative to other edible oils, their presence presents a significant challenge during chemical extractions due to their low Critical Micelle Concentration (CMC). At the critical phospholipid concentration, typically in the micromolar and nanomolar range for C18 and C16 lipid chains, thePatent Application Attorney Docket No. 58566.45WO01amphiphilic phospholipids self-assemble into aggregates with variable morphologies, in turn complicating the separation of the aqueous effluent from the purified triglycerides. This results in inefficient low-yielding extractions due to the formation of kinetically stable emulsions further exasperated by stabilization mechanisms characteristic of cocoa butter’s triglyceride profile.BRIEF DESCRIPTION OF THE DRAWINGS

[0007] Various embodiments of the present disclosure will be understood more fully from the detailed description given below and from the accompanying drawing. Embodiments are described in detail hereinafter with reference to the accompanying figure, in which:

[0008] FIG. 1 is a schematic diagram showing an edible oil chemical purification system according to an embodiment of the present disclosure.

[0009] FIG. 2 is a schematic diagram showing an edible oil chemical purification system according to an embodiment of the present disclosure.

[0010] FIG. 3 is a schematic diagram showing an edible oil chemical purification system according to an embodiment of the present disclosure.

[0011] FIG. 4 is a schematic diagram showing an edible oil chemical purification system according to an embodiment of the present disclosure.

[0012] FIG. 5 is a schematic diagram showing an edible oil chemical purification system according to an embodiment of the present disclosure.DETAILED DESCRIPTION

[0013] The following disclosure provides many different embodiments or examples. Specific examples of components and arrangements are described below to simplify the present disclosure. These are, of course, merely examples and are not intended to be limiting. In addition, the present disclosure may repeat reference numerals and / or letters in the various examples. This repetition is for the purpose of simplicity and clarity and does not in itself dictate a relationship between the various embodiments and / or configurations discussed.

[0014] The present disclosure relates to the chemical refining of edible oils and fats (e.g., crude cocoa butter). Various modes of reactor operations include: counter current flow; partial counter current flow; buffering of perturbations in flow with surge tanks when present; the option to reprocess emulsions back into the workflow should intractable emulsions emerge; and the implementation of acid splitting chemistry as part of a water treatment recycling strategy.Patent Application Attorney Docket No. 58566.45WO01Collectively, these system modifications provide for a more robust operational system than previously disclosed. This methodology enables the conversion of crude mixtures of triglycerides into higher quality oils and fats amenable to the milder sequential refining steps necessary to meet market requirements at minimal cost through the implementation of a more robust operational system.

[0015] The aggregate morphologies and phase separation of natural cocoa butter and aqueous alkali mixtures are highly dependent on factors such as temperature, pH, concentration, salinity, and flow conditions. The intractable formation of stabilized cocoa butter emulsions during chemical refining is exasperated via the Pickering stabilization mechanism of polymorphic crystals of saturated fatty acids and results in unpredictable morphologies and spontaneous aggregation due to minor changes in pH and different caustic concentrations. The present disclosure presents improved system operations that help to destabilize interfacial barriers through reprocessing the emulsion.

[0016] Once removed from cocoa butter; the free fatty acids, phospholipids and other aqueous partitioned biological constituents of Theobroma oil typically create a significant wastewater treatment burden. The addition of acid to the water waste stream allows for the recovery of alkali solubilized compounds by converting the once saponifiable matter back into a water insoluble constituent. Once reprotonated, the removal of these compounds from the wastewater can now be more easily accomplished through physical methods, thus reducing the burden placed on an acid less single stage water treatment process. Furthermore, the recovery of cocoa butter derived fatty acids creates a secondary offtake biproduct that can be used in other consumer goods.

[0017] According to embodiments of the present disclosure, a plurality of fiber reactors may be used to optimize reactor designs specific to particular feedstocks in which diffusion rates and mass transfer between oleaginous and aqueous solutions are specifically tailored to the application. The microchannel fiber reactor may be fabricated via the uniform vertical suspension of micron-sized stainless-steel fiber enclosed in a cylindrical reactor shell (see, e.g., U.S. Patent Nos. 7,618,544 and 11,198,107, each of which is hereby incorporated by reference in its entirety).

[0018] Referring to FIG. 1, a system 100 for refining an edible fat or oil (“edible oil”) includes an oil supply 101 containing the edible oil to be processed. The edible oil may include a mixture of triglycerides, FFA, phospholipids, and other minor contaminants. In some embodiments, the edible oil may include about 0.5 to about 8 wt%, about 1 to about 5 wt%, or about 2 to about 4 wt% ofPatent Application Attorney Docket No. 58566.45WO01FFA. However, it should be noted that the system described herein has been shown to remove greater than 90 wt% FFAs in non-cocoa butter feedstocks including greater than 15 wt% starting FFAs.

[0019] In some embodiments, the oil supply 101 may include an agitation mechanism 101a, such as a stirrer. Yet, it is critical to ensure that air entrainment is kept to a minimum and in some instances, a degassing system 103 could be placed in the workflow via line 102 to minimize air being carried into the reactor train through line 104. This strategy also has merit for the degassing of water in degasser 155 as the carrying capacity of oxygen for water is reduced at higher operation temperatures. In some embodiments, the oil supply 101 may be maintained at or above a melting point of the edible oil (e.g., at least 60 °C, at least 70 °C, or at least 80 °C). In some embodiments, the entire system 100 may be maintained at or above a melting point of the edible oil. The edible oil is transported from the oil supply 101 to a first reactor 110, which may be a fiber reactor engineered for a particular feedstock.

[0020] A concentrated aqueous reactant solution or extraction solution (“reactant solution”) is simultaneously supplied to the first reactor 110 via line 106 from a reactant supply 105 and combined with in-process water from line 126a in a full counter current operation or from lines 136b and / or 146b when run in partial counter current operation. In some partial counter current operations, fresh water may be supplied to the first reactor 110 from aqueous tank 150 via line 115b, as in system 400 of FIG. 4 or system 500 of FIG. 5. The reactant solution may include an aqueous reactant such as a solution including NaOH, KOH, and the like and / or may include an extractant, such as water. In some embodiments, the amount of base in the reactant solution is from 0.2 to 2.0, from 0.5 to 1.2, about 0.5, about 1.0, or about 1.2 molar equivalents, based on the amount of FFA in the edible oil. The edible oil reacts with reactant solution in the first reactor 110-which controllably contact the reactants within concentration, temperature, and flow under continuous operations-to form reaction products. The structured vertical suspension and packing of the fibers within the reactor serve the function of providing an inert scaffold comprising thousands of fibers between which the acid-base reaction occurs with high efficiency, enabling very precise dosing of reactant (e.g., NaOH) and rapid formation of products (e.g., lipid salts). Inside the reactor tower, the FFAs of the edible oil undergo a rapid acid base reaction with the NaOH in which free fatty acid sodium salts and water are formed and migrate into the aqueous phase.Patent Application Attorney Docket No. 58566.45WO01

[0021] The reaction products are collected in a first separator 110c of the first reactor 110, wherein the reaction products include a first raffinate including the edible oil having a first impurity removed therefrom and a first aqueous waste stream including the reactant solution and the first impurity. The first impurity may include, e.g., FFA and may be a combination of impurities. The aqueous reactant solution (in some embodiments having a high pH) readily separates from the oleaginous triglycerides of the edible oil (e.g., cocoa butter) by natural phase separation after exiting the fiber reactor wherein the higher density aqueous phase concentrates in the bottom of a first separator 110c. In instances where an emulsion or rag layer begins to accumulate at the interface between the raffinate and aqueous waste stream, the interfacial boundary can be selectively removed from the separator and reprocessed through the first reactor 110 via line 109 or processed in the second reactor 120 via line 109’ (optionally, via the surge tank 111). Similar procedures may be used for an emulsion or rag layer present in the second separator 120c (via line 129 or 129’, optionally using surge tank 121), the third separator 130c (via line 139 or 139’, optionally using surge tank 131), and / or the fourth separator 140c (via line 149). In some embodiments, removal of the rag layer may be achieved implementing either an adjustable dip tub inside the separator or by placing a port hole in the separator’s site glass.

[0022] Independent of this optional recirculatory mode of operation, the first aqueous waste stream is removed from the first separator 110a via line 116a or 116b depending on whether the mode of operation being implemented is either full or partial counter current flow. In practice, lines 116a and 116b could be the same pipe but instead have been kept separate in the flow diagram of FIG.1 for ease of contrasting different modes of operation as viewed across the entire reactor train. Examples of the different modes of operation are depicted in isolation in FIGS. 2-4. Upon exiting the first separator 110c the aqueous waste stream collects into an effluent tank 160, which may include an acid dosing system capable of reconstituting the progenitor FFAs through reprotonation of the lipid salts. Following reprotonation, the FFAs can more readily be separated from the water through a surface skimmer and / or centrifugation and utilized in the production of other consumer product goods. In practice, the removal of the FFAs from the wastewater stream effectively minimizes the overall load placed upon a downstream water treatment skid (e.g., membrane or reverse osmosis system) creating a more efficient staged water treatment strategy allowing for the recycling of the water back into the system via line 161. In some embodiments, the water from effluent tank 160 may be disposed of or reused in another process rather than being recycled to thePatent Application Attorney Docket No. 58566.45WO01aqueous tank 150.

[0023] The lower density neutralized edible oil raffinate (first raffinate) may be continuously collected from the top of the first separator 110c via line 107 and directed to a surge tank 111 (129 and 139 for separators 120c and 130c respectively) to help mitigate oscillations in flow rate and stabilize reactor dependent chemistries often experienced in continuous processes at industrial scales. In-process butter will progress from the optional intermittent surge tank 111 via line 108 to a second reactor 120.

[0024] Although a fresh aqueous solution could be simultaneously supplied from aqueous tank 150 via lines 115b, 125b, 135b, 145b and / or 145a into reactors 110, 120, 130 and 140, respectively, embodiments of the present disclosure provide the implementation of counter current flow strategies as a means to both minimize yield lose and reduce the overall water usage of the system. In the system 100, oil flows in the system 100 from left to right while water flows from right to left.

[0025] In the first of two strategies, as shown in FIG. 2, a full counter current strategy is utilized in which fresh water enters the fourth reactor 140 via line 145a and is used to wash the third raffinate as fed via line 138. Following collection in the fourth separator 140c, the water is reused to wash the second raffinate introduced by line 128 in the third reactor 130 using in process water introduced via line 146a which then collects into the third separator 130c. This process continues where the in-process water is then introduced via line 136a to treat the first raffinate transported into the second reactor 120 via line 108. As its final use, the in-process water collected in the second separator 120c is piped through line 126a and used to dilute the concentrated reactant solution from reactant supply 105 and fed through line 106 where it is used to treat the starting crude oil in the first reactor 110 to produce the first raffinate collected in first separator 110c.

[0026] In the second implementation shown in FIG. 3, a partial counter current strategy is implemented where fresh water from aqueous tank 150 is utilized as the input for the second reactor 120, the third reactor 130, and the fourth reactor 140 through lines 125b, 135b and 145b, respectively, while only the water from the third separator 130c and the fourth separator 140c are recycled back into the first reactor 110 via lines 136b and 146b and the in-process water collected in the second separator 120c drains directly to the effluent tank 160 via line 126b.

[0027] FIGS. 4 and 5 depict additional partial counter current strategies. In FIG. 4, fresh water from aqueous tank 150 is utilized as the input for the first reactor 110 and the fourth reactor 140Patent Application Attorney Docket No. 58566.45WO01through lines 115b and 145b, respectively, while the water from the fourth separator 140c is recycled back into the third reactor 130 via line 146b, the water from the third separator 130c is recycled back into the second reactor 120 via line 136b, and the in-process water collected in the second separator 120c drains directly to the effluent tank 160 via line 126b. In FIG. 5, fresh water from aqueous tank 150 is supplied to the first reactor 110, the second reactor 120, and the fourth reactor 140 through lines 115b, 125b, and 145b, respectively while only the water from the fourth separator 140c is recycled back into the third reactor 130 via line 146b while the in-process water collected in the second separator 120c and the third separator 130c drains directly to the effluent tank 160 via lines 126b and 136b, respectively. It will be appreciated that additional partial counter current configurations are possible and contemplated herein. In some embodiments, any reactor may include water input(s) from any one or more of the separators (including the separator associated with said reactor) and / or from the aqueous tank 150. In some embodiments, water from a separator may be directed in part to a reactor and in part to another reactor or the effluent tank 160. The system described herein may include appropriate piping and valves to accommodate switching between modes of operation.

[0028] In both partial and full counter current modes of operation, the first reactor 110 in the multistage reactor series is used to first contact the two immiscible phases- the crude triglyceride mixture (the edible oil) and the aqueous (basic) solution. The fiber reactors allow the stable maintenance of the desired operating temperature range and enable the continuous formation of fresh interfaces between the immiscible fluids as a function of the enhanced surface area inherent in the plurality of the fiber packing material. Without being bound by theory, the generated surfactants subsequently adsorb onto the freshly created interfaces which are continuously generated and controlled via the shear rate which can be modified by controlling the injection flowrate of the solutions and the reactor pack density. The gradient in surfactant concentration affects the flow around the interfaces and enables the separation of surfactants from the edible oil phase into the aqueous effluent. The net result is a facile, simultaneous neutralization of the injected edible oil and separation from the aqueous effluent phase.

[0029] The counter current processes disclosed herein incorporates the staging of fiber reactors in series that continuously remove FFAs, phospholipids, and metals from natural, unrefined cocoa butter. As described above, the reactor train is an improvement from prior iterations by both reducing the overall water usage and by decreasing yield loss by reprocessing the water in a counterPatent Application Attorney Docket No. 58566.45WO01current orientation. In doing so, trace amounts of oil entrained in the aqueous phase can be recovered as they are reprocessed through the reactor towers. Similarly, should they form, this system configuration works to break down intractable emulsions that deposit at the interface by reprocessing the emulsion through the tower. In doing so, this design improves upon prior configurations by utilizing the tower to both break apart stable emulsions and recover oil that can become finely dispersed in the aqueous phase when these systems are run at high rates.

[0030] Also provided herein are methods of operating the system 100. Methods may include neutralization of the edible oil described herein followed by one or more water washings while utilizing counter current or partial counter current aqueous flow.

[0031] EXAMPLES

[0032] Example 1: Cross current water usage as the benchmark

[0033] Four 5’ long fiber reactor columns with 1” inner diameter (ID) and 50 micron fibers disposed therein were positioned in series and run at a flow rate of 80 mL / min cocoa butter (CB) with counter current aqueous flow and a concentrated reactant being supplied to reactor 1 (see FIG. 2). The highest linear velocity achieved was 83.73 cm / min (80 + 200 mL / min) and the lowest linear velocity experienced was 37.32 cm / min (80 + 44.8 mL / min). Tests were run starting with an organic to aqueous ratio (O:A) of 1 :7 and reducing to a O: A of 1 :5. At an O:A of 1 :4, the tests could not be sustained without emulsion overtaking separator 4. The aqueous fluid was distributed to each reactor before being drained into the waste system (no water recycling occurred).

[0034] O:A distribution for 1:7 was:Reactor 1- 1:1Reactor 2- 1:2.5Reactor 3- 1:2.5Reactor 4- 1:1

[0035] O:A distribution for 1:5 was:Reactor 1- 1:1Reactor 2- 1:1.8Reactor 3- 1:1.7Reactor 4- 1:0.56

[0036] Deacidification achieved in reactor 1 was 47% with a standard deviation of 3.8% while the final deacidification achieved was 90% with a standard deviation of 1.0% for both the O: A of 1 :7Patent Application Attorney Docket No. 58566.45WO01and 1 :5

[0037] Surge tanks were used between each stage to prevent oscillations of flow between stages as fluid was drained into each tank and the organic residence time for each stage was maintained at 70 minutes.

[0038] Example 2: Impact of internal recirculation from benchmark

[0039] The array and CB flow rate from Example 1 was used with emulsion recirculation as described below. The highest linear velocity experienced was 66.98 cm / min (80 + 144 mL / min) and the lowest linear velocity experienced was 34.21 cm / min (80 + 34.4 mL / min). Tests were run starting with an O:A of 1 :5 and reduced to a O:A of 1 :4. The impact of removing the most dense emulsion at the interface of the separators where it accumulates and redirecting it into the same reactor to be contacted by the aqueous phase again, the separator aqueous phase to be contacted by water again, or into the subsequent surge tank was analyzed. All iterations worked to reduce the accumulation of dense emulsion in the system allowing for increased phase transfer area in the separator to allow for ionized material (primarily ionized fatty acid) to enter into the aqueous phase as desired. The aqueous fluid was distributed to each reactor before being drained into the waste system (no water recycling occurred).

[0040] O:A distribution for 1:5 was:Reactor 1- 1:1Reactor 2- 1:1.8Reactor 3- 1:1.7Reactor 4- 1:0.43

[0041] O:A distribution for 1:4 was:Reactor 1- 1:1Reactor 2- 1:1.3Reactor 3- 1:1.2Reactor 4- 1:0.43

[0042] Deacidification achieved in reactor 1 was 59% with a standard deviation of 6% while the final deacidification achieved was 92% with a standard deviation of 1.0% for both the O:A of 1 :5 and 1 :4. Surge tanks continued to be used as in Example 1 and the organic residence time in the separator was maintained at 70 minutes.

[0043] Example 3- Impact of internal recirculation and partial counter current water usage fromPatent Application Attorney Docket No. 58566.45WO01benchmark

[0044] The array and CB flow rate from Example 2 was used with partial counter current water usage as described below. The highest linear velocity achieved was 74.87 cm / min (80 + 80 + 56 + 34.4 mL / min) and lowest linear velocity experienced was 34.21 cm / min (80 + 34.4 mL / min). Test were run starting with an O:A of 1:3 while utilizing internal recirculation allowed for ionized material (primarily ionized fatty acid) to be removed from the processed organic material; however, with the reduced water usage, an increase in yield loss was observed in later stages. To reduce yield loss and improve extraction efficiency, the discharge from separator 4 was redirected to reactor 3 before being discharged to waste (see FIG. 5). Additionally, to further improve extraction efficiency the discharge of separator 3 was redirected to reactor 1 while the discharge of separator 4 was also redirected to reactor 1 (see FIG. 3). In another variation, the discharge of wastewater from separator 4 was used as feed for reactor 3 and this was repeated until the aqueous stream was discharged to waste from separator 2 (see FIG. 4). A drawback experienced during counter current processing of the aqueous extractant was the generation of dense emulsions that would not disengage in the system when a large quantity of water was utilized. All of the above iterations had the benefit of reusing water, reducing yield loss, and improving aqueous extraction efficiency.

[0045] O:A distribution for 1:3 was:Reactor 1- 1:1Reactor 2- 1:0.8Reactor 3- 1:0.7Reactor 4- 1:0.43

[0046] Deacidification achieved in reactor 1 at a 1:3 O:A without counter current water usage (FIG. 5) was 62% with a standard deviation of 1%, while, with counter current water usage (FIGS.3 and 4), the average deacidification increased to 73% with a standard deviation of 3% while the final deacidification remained constant at 91% with a standard deviation of 1%.

[0047] Surge tanks and internal recirculation continued to be used as before and the organic residence time in the separator was maintained at 70 minutes.

[0048] Example 4- Water Treatment skid with an acid splitting system

[0049] The combined waste water streams from all stages in the cocoa butter process were directed into a surge tank which delivered the flow of wastewater through a static mixer that ensured atPatent Application Attorney Docket No. 58566.45WO01least 1.7 equivalents acid per equivalent alkalinity as phosphoric acid (0.5 equivalents excess of acid) is contacting the wastewater, which was then directed into a cotton (glass may be used) fiber filled reactor that was placed on top of a separator that was maintained at 75+°C. A static mixer is not required, but the acid must contact the wastewater before it enters the separator. A cotton or glass contact is not required, but it has been observed to enhance the size of the acidified oil droplets and reduce the quantity of oil droplets suspended in water.

[0050] A 24 hour trial was conducted and the average oil in the aqueous phase was 4.45% and the yield loss was ~1% of non-FFA materials. After treatment of the waste stream with acid and passing through the cotton fiber reactor and allowing the remade organic material to flocculate in the separator, the average oil in the aqueous phase was 0.21% which is a 95% oil recovery. Using an alternate method to assess the wastewater treatment method, the COD value of the wastewater reduced from an average of 110,000 mg / L in the wastewater to 6,200 mg / L which is a 94% decrease. A third analysis method of turbidity was used to assess the scattered particles present in the wastewater before and after treatment and it also decreased by 94% from an average of 3,500 FAU to 200 FAU.

[0051] Although various embodiments have been shown and described, the disclosure is not limited to such embodiments and will be understood to include all modifications and variations as would be apparent to one of ordinary skill in the art. It is understood that variations may be made in the foregoing without departing from the scope of the present disclosure. In several example embodiments, the elements and teachings of the various illustrative example embodiments may be combined in whole or in part in some or all of the illustrative example embodiments. In addition, one or more of the elements and teachings of the various illustrative example embodiments may be omitted, at least in part, and / or combined, at least in part, with one or more of the other elements and teachings of the various illustrative embodiments.

Claims

Patent Application Attorney Docket No. 58566.45WO01CLAIMSWhat is claimed is:

1. A system for refining an edible oil, comprising:a first fiber reactor comprising a first end, a second end, and a first plurality of fibers disposed therein;a first separator in fluid communication with the first fiber reactor, positioned proximate the second end thereof, configured to collect first reaction products comprising a first oil and a first aqueous effluent, and comprising a first oil outlet for removing the first oil from the first separator and a first effluent outlet for removing the first aqueous effect from the first separator;a second fiber reactor comprising a first end, a second end, and a second plurality of fibers disposed therein, the first end of the second fiber reactor being in fluid communication with the first oil outlet of the first separator;a second separator in fluid communication with the second fiber reactor, positioned proximate the second end thereof, configured to collect second reaction products comprising a second oil and a second aqueous effluent, and comprising a second oil outlet for removing the second oil from the second separator and a second effluent outlet for removing the second aqueous effect from the second separator; a third fiber reactor comprising a first end, a second end, and a third plurality of fibers disposed therein, the first end of the third fiber reactor being in direct or indirect fluid communication with the second oil outlet of the second separator;a third separator in fluid communication with the third fiber reactor, positioned proximate the second end thereof, configured to collect third reaction products comprising a third oil and a third aqueous effluent, and comprising a third oil outlet for removing the third oil from the third separator and a third effluent outlet for removing the third aqueous effect from the third separator;an oil supply vessel in fluid communication with the first end of the first fiber reactor and comprising the edible oil, the edible oil comprising at least one impurity;an aqueous reactant supply vessel in fluid communication with the first end of the first fiber reactor and comprising a concentrated aqueous reactant; andPatent Application Attorney Docket No. 58566.45WO01a fresh water supply vessel comprising water;wherein the system is configurable between a counter current mode and a partial counter current mode;wherein, in the counter current mode, the fresh water supply vessel is in fluid communication with the first end of the third fiber reactor and is not in fluid communication with the first end of the first fiber reactor nor the first end of the second fiber reactor; andwherein, in the partial counter current mode, the fresh water supply vessel is in fluid communication with the first end of the third fiber reactor and one of the first end of the first fiber reactor or the first end of the second fiber reactor.

2. The system of claim 1, wherein, in the counter current mode, the third effluent outlet is in fluid communication with the first end of the second fiber reactor and the second effluent outlet is in fluid communication with the first end of the first fiber reactor to dilute the concentrated aqueous reactant.

3. The system of claim 1, further comprising a fourth fiber reactor comprising a first end, a second end, and a fourth plurality of fibers disposed therein; anda fourth separator in fluid communication with the fourth fiber reactor, positioned proximate the second end thereof, configured to collect fourth reaction products comprising a fourth oil and a fourth aqueous effluent, and comprising a fourth oil outlet for removing the fourth oil from the fourth separator and a fourth effluent outlet for removing the fourth aqueous effect from the fourth separator; and wherein the fourth fiber reactor is positioned between the second fiber reactor, the first end of the fourth fiber reactor is in fluid communication with the second oil outlet of the second separator, and the first end of the third fiber reactor is in fluid communication with the fourth oil outlet of the fourth separator.

4. The system of claim 3, wherein, in the counter current mode, the third effluent outlet is in fluid communication with the first end of the fourth fiber reactor, the fourth effluentPatent Application Attorney Docket No. 58566.45WO01outlet is in fluid communication with the first end of the second fiber reactor, and the second effluent outlet is in fluid communication with the first end of the first fiber reactor to dilute the concentrated aqueous reactant.

5. The system of claim 3, wherein, in the partial counter current mode, the third effluent outlet or the fourth effluent outlet is in fluid communication with the first end of the first fiber reactor.

6. The system of claim 5, wherein the second effluent outlet is in fluid communication with an effluent tank configured.

7. The system of claim 6, wherein the first effluent outlet is in fluid communication with the effluent tank.

8. The system of claim 7, wherein the at least one impurity comprises free fatty acids;wherein the effluent tank comprises an acid splitting system configured to treat the first aqueous effluent and the second aqueous effluent by reprotonating fatty acid salts and saponifiable matter and to remove a resulting water insoluble product; and wherein the effluent tank is in fluid communication with the fresh water supply vessel.

9. The system of claim 1, further comprising a first surge tank positioned between the first fiber reactor and the second fiber reactor.

10. The system of claim 1, further comprising at least one of:a first emulsion reprocessing loop comprising a first emulsion outlet configured to remove a first emulsion from the first separator and a first pump configured to recycle the first emulsion from the first emulsion outlet to the first end of the first separator;a second emulsion reprocessing loop comprising a second emulsion outlet configured to remove a second emulsion from the second separator and a second pump configured to recycle the second emulsion from the second emulsion outlet to thePatent Application Attorney Docket No. 58566.45WO01first end of the second separator; ora third emulsion reprocessing loop comprising a third emulsion outlet configured to remove a third emulsion from the third separator and a third pump configured to recycle the third emulsion from the third emulsion outlet to the first end of the third separator.

11. The system of claim 1, wherein the edible oil is solid at room temperature and the system is maintained at a temperature equal to or greater than a melting point of the edible oil.

12. The system of claim 1, wherein the edible oil is liquid at room temperature.

13. The system of claim 1, wherein the concentrated aqueous reactant comprises an alkali solution.

14. The system of claim 1, wherein at least one impurity comprises free fatty acids and the system is configured to remove at least 75 wt% of the free fatty acids from the edible oil.

15. The system of claim 1, wherein at least one impurity comprises free fatty acids and the system is configured to be operated controllably to remove a subset of the free fatty acids describing less than 75 wt% of the free fatty acids from the edible oil.

16. The system of claim 1, wherein the at least one impurity comprises free fatty acids and phospholipids or metals.

17. The system of claim 16, further comprising an effluent tank configured to receive the first aqueous effluent; andwherein the effluent tank comprises an acid splitting system configured to treat the first aqueous effluent by reprotonating fatty acid salts and saponifiable matter in the aqueous effluent and to remove a resulting water insoluble product.

18. The system of claim 17, wherein the effluent tank comprises a membrane filtration skidPatent Application Attorney Docket No. 58566.45WO01configured to remove the water insoluble product.

19. The system of claim 17, wherein the effluent tank comprises a reverse osmosis treatment skid configured to remove the water insoluble product.

20. The system of claim 17, wherein the effluent tank comprises a treated water outlet for removing the treated first aqueous effluent and the treated water outlet is in fluid communication with the fresh water supply vessel.

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