Systems and methods for stillage fractionation

Information

  • Patent Grant
  • 11905502
  • Patent Number
    11,905,502
  • Date Filed
    Wednesday, March 31, 2021
    3 years ago
  • Date Issued
    Tuesday, February 20, 2024
    9 months ago
Abstract
Systems and methods for fractionating whole stillage from an ethanol production facility are provided. Whole stillage undergoes a separation of its liquid portion (thin stillage) from the solid portion (fiber cake). In some embodiments, the solids and liquids in whole stillage may be separated utilizing a screening centrifuge. The fiber cake may be dried to generate a high fiber animal feed. The thin stillage may be provided to a three-phase separator for separation into an oil emulsion, an aqueous clarified stillage, and a protein paste. The protein paste may be dried to generate a high protein animal feed with greater than about 45% protein content. The clarified thin stillage is condensed to yield a syrup with greater than around 60% solids. The oil emulsion is subjected to a pH adjustment to liberate the oil from the emulsion, which is then separated.
Description
FIELD

The subject disclosure relates to systems and methods for fractionating thin and whole stillage in an ethanol production facility.


BACKGROUND

Ethanol traditionally has been produced from grain-based feedstocks (e.g., corn, sorghum/milo, barley, wheat, soybeans, etc.), or from sugar (e.g., sugar cane, sugar beets, etc.).


In a conventional ethanol plant, corn, sugar cane, other grain, beets, or other plants are used as a feedstock and ethanol is produced from starch contained within the corn, or other plant feedstock. In the case of a corn facility, corn kernels are cleaned and milled to prepare starch-containing material for processing. Corn kernels can also be fractionated to separate the starch-containing material (e.g., endosperm) from other matter (such as fiber and germ). Initial treatment of the feedstock varies by feedstock type. Generally, however, the starch and sugar contained in the plant material is extracted using a combination of mechanical and chemical means.


The starch-containing material is slurried with water and liquefied to facilitate saccharification, where the starch is converted into sugar (e.g., glucose), and fermentation, where the sugar is converted by an ethanologen (e.g., yeast) into ethanol. The fermentation product is beer, which comprises a liquid component, including ethanol, water, and soluble components, and a solids component, including unfermented particulate matter (among other things). The fermentation product is sent to a distillation system where the fermentation product is distilled and dehydrated into ethanol. The residual matter (e.g., whole stillage) comprises water, soluble components, oil, and unfermented solids (e.g., the solids component of the beer with substantially all ethanol removed, which can be dried into dried distillers grains (DDG) and sold, for example, as an animal feed product). Other co-products (e.g., syrup and oil contained in the syrup) can also be recovered from the whole stillage.


In a typical ethanol plant, a massive volume of whole stillage is generally produced. In fact, for a typical ethanol plant the amount of whole stillage produced can be nearly 13.4 gallons per bushel of corn processed. Roughly, a third of the corn feedstock is present in the whole stillage as dissolved and suspended solids. The stillage contains almost 90% water. Whole stillage is responsible for a substantial portion of the wastewater generated by ethanol plants. The financial cost of the water, its treatment and disposal (typically through evaporation) can be significant.


While stillage is typically viewed as a liability for an ethanol plant, it is possible to generate a number of high value co-products from the stillage. For example, oil in stillage, high protein feeds, and syrups are all able to be generated from stillage and sold as higher value co-products. Currently, in the interest of improving efficiencies of ethanol plants, whole stillage is often separated into two components: a solid component and a liquid component. Separation may be performed using centrifugation, or filter and press. The solid component may be dried to generate dried distillers grain (DDG) which is sold as animal feed. The liquid component, known as thin stillage, may be dried and used to increase the fat content of DDG to make DDGS (Distillers Dried Grains with Solubles). This process requires the drying of a large amount of water, which is very energy intensive and costly. Thin stillage may also be recycled into the plant, such as for replacement of some portion of the water used during fermentation (fermentation backset).


Further, there is currently a strong push to generate corn oil from stillage, as oil is a particularly high value commodity, and for regulatory and legal considerations. Ideally, an ethanol plant would generate a minimum of 1.33 pounds of oil product per bushel of corn processed. A number of oil recovery methods are known, but to date none has achieved more than about one pound of oil per bushel. Further, conventional processes for recovering oil from fermentation products often sacrifice oil quality such that the oil contains high levels of free fatty acids. The presence of a high level of free fatty acids can hamper the production of end products such as, for example, the yield and quality of any bio-diesel eventually produced with the oil as a feedstock.


For example, the patent application PCT/US2009/045163 (entitled “METHODS FOR PRODUCING A HIGH PROTEIN CORN MEAL FROM A WHOLE STILLAGE BYPRODUCT AND SYSTEM THEREFORE”) discloses a process for separating whole stillage into a solid portion and a thin stillage. The thin stillage is again separated to a protein and a water-soluble portion. An oil fraction may be separated from the water portion via evaporation. In the method of the PCT application, oil is recovered post evaporation, which likely results in yield reductions and oil quality sacrifices.


Another current method of oil recovery is disclosed by U.S. Pat. No. 7,829,680 (entitled “SYSTEM AND METHOD FOR ISOLATION OF GLUTEN AS ACO-PRODUCT OF ETHANOL PRODUCTION”). In this method, a plurality of screens is utilized to separate a fiber product from an oil/protein product. The oil and protein may then be separated via centrifugation.


While these known systems and methods may generate valuable co-products from ethanol production stillage, they have inherent drawbacks related to oil quality, quantity of oil recovered, water balance issues, and composition of the protein products isolated.


SUMMARY

The disclosed aspects relate to systems and methods for fractionating whole stillage from an ethanol production facility. The system of fractionation generates multiple valuable co-products while reducing the demand for energy over many traditional methods of treatment of stillage.


In the disclosed systems and methods, the whole stillage undergoes a separation of its liquid portion (thin stillage) from its solid portion (fiber cake). This separation may be performed utilizing membranes, screw presses, centrifuges, or other suitable means. In some embodiments, the solids and liquids in whole stillage may be separated utilizing a screening centrifuge.


The fiber cake may be dried to generate a high fiber animal feed. The thin stillage may be provided to a three-phase separator for separation into an oil emulsion, an aqueous clarified stillage, and a protein paste. In some embodiments, the three-phase separator may include a disk nozzle centrifuge or other suitable separator device.


The protein paste may be dried to generate a high protein animal feed. In some cases, this feed may have greater than about 45% protein content. In alternate embodiments, the protein paste may be returned to the fiber cake prior to drying in order to alter the nutritional makeup of the animal feed produced.


The clarified thin stillage may be utilized as fermentation backset, or other makeup water source, within an ethanol production facility, for example. Alternatively, some or all of the clarified stillage may be condensed, utilizing an evaporator or other suitable device, to yield a syrup. The syrup (high solid syrup) may be utilized as an animal feed product. Generally, the syrup may contain between about 30% and about 40% moisture, greater than about 10% protein, less than about 1% fiber, between about 6% and about 10% fat, and between about 5% to about 7% ash.


The oil emulsion may be subjected to a pH adjustment to liberate the oil from the emulsion. The pH adjustment may utilize a caustic to bring the emulsion pH to about 8.0 to about 8.5. The oil can be separated from the emulsion utilizing a centrifuge, or other suitable separating device. The oil resulting may include greater than about 97% fat. Further, in some embodiments, about 1.33 or more pounds of oil may be recovered from the whole stillage generated from processing a bushel of com for ethanol.


Note that the various features of the various aspects described above m a y be practiced alone or in combination. These and other features will be described in more detail below in the detailed description and in conjunction with the following figures.





DESCRIPTION OF THE DRAWINGS

In order that the various aspects may be more clearly ascertained, some embodiments will now be described, by way of example, with reference to the accompanying drawings, in which:



FIG. 1 is a perspective view of a biorefinery comprising an ethanol production facility, in accordance with some embodiments;



FIGS. 2A and 2B are process flow diagrams illustrating examples of ethanol production processes from corn to ethanol, in accordance with some embodiments;



FIG. 3 is a schematic block diagram illustrating a system for fractionating stillage, in accordance with some embodiments;



FIG. 4 is an example flowchart illustrating a process of fractionating stillage into valuable co-products, in accordance with some embodiments;



FIG. 5 contains TABLE 1 which lists experimental compositions of stillage fractions, in accordance with some embodiments; and



FIG. 6 contains TABLE 2 which lists expected compositions of commercially derived stillage fractions, in accordance with some embodiments.





DESCRIPTION OF THE EMBODIMENTS

The various aspects will now be described in detail with reference to several embodiments thereof as illustrated in the accompanying drawings. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the various aspects. It will be apparent, however, to one skilled in the art, that embodiments may be practiced without some or all of these specific details. In other instances, well known process steps and/or structures have not been described in detail in order to not unnecessarily obscure the disclosed aspects. The features and advantages of embodiments may be better understood with reference to the drawings and discussions that follow.


The following description relates to systems and methods for fractionating stillage from an ethanol production plant or other processing facility. Ethanol plants generate large quantities of still age as a low value product. Stillage is generally a low value co-product that requires substantial energy to dry into solubles for addition to distillers dried grains, or must be disposed of in some other manner. There is the potential for the generation of high value co-products from stillage, thus, the disclosed aspects provide for systems and methods that improve stillage utilization, which can generate multiple high quality co-products without unduly influencing the water balance of the ethanol production facility. Such systems and methods can provide increased revenue from co-products and a lower impact on the environment.


The disclosed systems and methods provide a means to substantially improve the quality and value of stillage by fractionating the stillage into components, each highly valued in their own right. The fractions generated by the disclosed systems and methods, in addition to being intrinsically valuable, provide an improved water balance for the ethanol production facility, thereby reducing the energy required to process the stillage over traditional evaporation and drying.


Referring to FIG. 1, an example biorefinery 100 comprising an ethanol production facility configured to produce ethanol from corn is shown. The example biorefinery 100 comprises an area 102 where corn (or other suitable material including, but not limited to, biomass, sugars, and other starch products) is delivered and prepared to be supplied to the ethanol production facility. The ethanol production facility comprises apparatus 104 for preparation and treatment (e.g., milling) of the corn into corn flour suitable for fermentation into fermentation product in a fermentation system 106. The ethanol production facility comprises a distillation system 108 in which the fermentation product is distilled and dehydrated into ethanol. The biorefinery may also comprise, in some embodiments, a by-product treatment system 110 (shown as comprising a centrifuge, a dryer, an evaporator, and associated tanks).


Referring to FIGS. 2A and 2B, in an ethanol production process, corn 202 (or other suitable feed material) may be prepared for further treatment in a preparation system 204. As illustrated in FIG. 2B, the preparation system 204 may comprise cleaning or screening 206 to remove foreign material, such as rocks, dirt, sand, pieces of corn cobs and stalk, and other unfermentable material (e.g., removed components). After cleaning or screening 206, the particle size of corn may be reduced by milling 208 to facilitate further processing. The corn kernels may also be fractionated into starch-containing endosperm, fiber, and germ, in accordance with some embodiments. The milled corn 210 orendosperm is slurried with water, enzymes and agents 212 to facilitate the conversion of starch into sugar (e.g. glucose), such as in a first treatment system 214. The sugar (e.g., treated component 216) is converted into ethanol by an ethanologen (e.g. yeast or other agents 218) in a fermentation system 220. The product of fermentation (fermentation product 222) is beer, which comprises a liquid component, including ethanol and water and soluble components, and a solids component, including unfermented particulate matter (among other things). The fermentation product may be treated with agents 224 in a second treatment system 226. The treated fermentation product 228 is sent to a distillation system 230. In the distillation system 230, the (treated) fermentation product is distilled and dehydrated into ethanol 232. In some embodiments, the removed components 234 (e.g., whole stillage), which comprise water, soluble components, oil, and unfermented solids (e.g., the solids component of the beer with substantially all ethanol removed), may be dried into dried distillers grains (DDG) in a third treatment system (where the removed components may be treated with agents) and sold as an animal feed product. Other co-products, for example, syrup (and oil contained in the syrup), may also be recovered from the stillage, as will be described in further detail below.


In some systems, the thin stillage that results when solids are removed from the whole stillage can be used as a backset during the fermentation process and also can be used to increase the fat content of DDGS (Distillers Dried Grains with Solubles). However, the addition of thin stillage to DDGS requires costly evaporation processes that increase the DDGS production cost. Disclosed herein are systems and methods for fractionating the whole stillage in order to generate relevant quantities of valuable co-products in a manner which ultimately reduces the required fuel spent on evaporation.


Referring now to FIG. 3, an example schematic block diagram of a system for fractionation of the removed stillage component is provided. In this example diagram, the whole stillage 302 is provided to a stillage filter 304 for separation of the stillage into a solids component and a liquid thin stillage 306. The separation may be performed through screw press, centrifugation, decanters, or via filtration type methodologies. In some particular embodiments, the separation may be performed utilizing a screen bowl centrifuge. One of ordinary skill in the art will appreciate that the speed or amount of centrifugal force applied will depend on various factors such as sample size and may be adjusted appropriately depending on such factors. Suitable separators and centrifuges are available from various manufacturers such as, for example, Seital of Vicenza, Italy, Westfalia of Oelde, Germany or Alfa Laval of Lund, Sweden.


The solid component comprises a high fiber cake 308, which may be dried at a dryer 310 to a high fiber dried distillers grain (DDG) 312 product. Such high fiber DDG may be particularly suited for the poly-gastric animal feed markets (ruminant feed). In some embodiments, the fiber cake may additionally undergo a washing step prior to being dried. The wash fluid may be combined with the liquid thin stillage, in some embodiments.


Separation of the fiber cake solids from the thin stillage may be performed soon after initial production of the fermentation product (whole stillage) in order to maintain co-product composition quality and to prevent undue exposure of the co-products to heat, oxygen, and potential contaminants. If the whole or thin stillage is left exposed for extended periods of time in the presence of moisture, hydrolysis of the oils may occur which leads to the formation of free fatty acids, which degrades the quality of oil produced.


The resulting liquid thin stillage 306 is provided to a three phase separator 314, which may include a disk nozzle type centrifuge or suitable filtration type system. The three phase separator 314 separates the thin stillage 306 into a top layer of oil emulsion 318, a middle aqueous clarified thin stillage 320, and a protein paste 322. One of ordinary skill in the art will appreciate that the speed or amount of centrifugal force applied will depend on various factors such as sample size and may be adjusted appropriately depending on such factors. Suitable separators and centrifuges are available from at least the manufacturers listed above.


The protein paste 322 may be dried in a dryer 324 to a high protein DDG product 326. The high protein DDG may be particularly suited for mono-gastric (non-ruminant) and young animal feed. The high protein DDG may have high metabolize-able energy and a lysine content of between about 2% and about 3%, which can be important in feed ration formulations.


The clarified thin stillage 320 may be condensed through evaporation 328 or concentrated by reverse osmosis to yield high solid syrup 330. Due to low levels of suspended solids in the clarified thin stillage, high total solids can be achieved in a concentrated syrup without substantial viscosity limitations. The high solids syrup 330 may have between about 30 and 80 percent solids, dependent upon material handling properties desired, as well as end use. In some particular embodiments, the high solid syrup may contain greater than around 60% solids. High solid syrup 330 may be marketed as a high energy animal feed supplement. In alternate embodiments, some portion of the clarified thin still age may be utilized as a backset for fermentation, thereby further reducing the need for evaporation further.


The oil emulsion 318 may be pH treated by an alkali in order to disrupt the emulsion. The adjustment of pH may be critical for the liberation of the oil from emulsion, and may result in greater oil yields and enhanced oil quality. Particularly, adjusting the pH of the oil fraction separates or breaks the oil fraction such that the resulting oil recovered has a low fatty acid content. The age of the fermented product and the organic acid content of the fermented product can affect the optimum pH for separation, however, the oil fraction is treated with the highest pH possible to reduce the overall free fatty acid content in the separated oil without sacrificing oil quality. In some embodiments, the pH is adjusted to a range of about 7 to about I 0. In some particular embodiments, the pH is adjusted to between around 8.0 and around 8.5.


Oil 332 may be separated from the remaining emulsion/aqueous layer through centrifugation, filtration, distillation or other suitable separator 334. The remaining aqueous layer/emulsion may be high in protein and recycled for addition to DDG or sold as a separate feed product.


The oil composition recovered from the aspects described herein may be further processed in a variety of ways. For example, the crude oil may be filtered and bleached to provide a food grade oil for consumer use. In one embodiment, the crude oil may be degummed, further caustic refined, and subjected to a soap removal step according to commercially available processes. Following these steps, the oil may be subjected to one or more clay bleaching steps to achieve an oil of desired content and color. If one or more clay bleaching steps are used, the clay may be an acid clay or a non-acid clay. In one embodiment, the bleaching step may include, by way of example, an acid clay or a non-acid clay at around 1% to around 5% based on the total weight. In addition to or as an alternative to clay bleaching, after the crude oil has been degummed, caustic refined and subjected to a soap removal step, a food grade oil of a desired color may be achieved using a heat bleaching step.


The oil composition can be used in a wide variety of applications. Such exemplary applications include the areas of oleochemicals, feed (e.g., animal feed) as well as oils suitable for human consumption. Oleochemicals include feedstock chemicals that are suitable for biodiesel production (fatty acid methyl esters). Industrial oleochemicals are useful in the production of soaps, detergents, wire insulation, industrial lubricants, leather treatments, cutting oils, mining agents for oil well drilling, ink removal, plastic stabilizers, ink, and in rubber production. Other industrial applications include waxes, shampoos, personal hygiene and food emulsifier or additive products. It is also possible in some embodiments, to pre-treat oil for downstream uses, such as conversion to bio-diesel.


The recovered oil composition can contain low levels of moisture, insolubles and unsaponifiables (MIU content). Moisture, as contemplated herein, includes water and any volatile material such as, for example, hexane, ethanol, methanol, or a combination thereof. Insoluble matter (i.e., “insolubles”), as contemplated herein, refers to and includes any matter incapable of being dissolved in the aqueous portion, oil fraction or oil composition. Unsaponifiable matter (i.e., “unsaponifiables”) includes any variety of possible non-triglyceride materials that act as contaminants during bio-diesel production. Usaponifiable matter can significantly reduce the end product yields of the oil composition and can, in turn, reduce end product yields of processes such as, for example, bio-diesel production processes.


Maintaining low levels of moisture is especially desirable because moisture fosters the formation of free fatty acids instead of esters. In one embodiment, the oil composition contains no greater than around 1% w/w of total moisture content, alone, based on the total weight of the oil composition. In some embodiments, the moisture content, alone, is no greater than about 0.5% w/w or about 0.1% w/w.


In one embodiment, the oil composition comprises no greater than approximately 3% w/w of unsaponifiables, based on the total weight of the oil composition. In some embodiments, the oil composition comprises no greater than around 2% w/w or around 1% w/w of unsaponifiables.


In one embodiment, the oil composition contains no greater than about 1% w/w insolubles, alone, based on the total weight of the oil composition. In some embodiments, the insolubles content, alone, is no greater than approximately 0.5% w/w or approximately 0.1% w/w.


The oil composition may, in some embodiments, exhibit an iodine value acceptable for bio-diesel production and, in some embodiments, exhibits an iodine value higher than that expected from a neat oil sample. The oil can further comprise various carotene, carotenoid, and antioxidant or neutraceutical compounds.


In one embodiment, the oil composition contains no greater than about 5% w/w free fatty acid content, based on the total weight of the oil composition. In some embodiments, the free fatty acid content, is no greater than around 3% w/w.


The fatty acid content of the oil composition is comprised of various fatty acids known in the art. In one embodiment, the oil composition comprises C 16 palmitic acid which represents no greater than about 15% w/w of the total fatty acid content, based on the total weight of the oil composition. In another embodiment, the C 16 palmitic acid content is no greater than around 10% w/w of the total fatty acid content. In one embodiment, the oil composition comprises C 18 stearic acid which represents at least about 3% w/w of the total fatty acid content, based on the total weight of the oil composition. In another embodiment, the C18 stearic acid content is at least about 1.5% w/w of the total fatty acid content. In one embodiment, the oil composition comprises C18-1 oleic acid which represents at least around 30% w/w of the total fatty acid content, based on the total weight of the oil composition. In another embodiment, the C18-1 oleic acid content is at least about 25% w/w of the total fatty acid content. In one embodiment, the oil composition comprises C18-2 linoleic acid which represents at least around 60% w/w of the total fatty acid content, based on the total weight of the oil composition. In another embodiment, the C18-2 linoleic acid content is at least around 50% w/w of the total fatty acid content. In one embodiment, the oil composition comprises Cl 8-3 linolenic acid which represents no greater about 1.5% w/w of the total fatty acid content, based on the total weight of the oil composition. In another embodiment, the C18-3 linolenic acid content is no greater than about 0.5% w/w of the total fatty acid content.


Since the entire thin stillage is not evaporated, in these embodiments, there is substantial fuel and cost savings over traditional stillage handling which includes the substantial evaporation of the thin stillage for addition back to the DDG to generate dried distillers grains with solubles (DDGS). As such, not only are greater quantities of higher value products generated through the disclosed treatment of the whole stillage, but additionally, the process utilizes less fuel thereby reducing pollution generated and reducing operational costs.



FIG. 4 provides an example flow diagram 400 for the process of generating high value co-products. In this process, the whole stillage is separated into solids and the liquid thin stillage (at 402). The solids include a fiber calm which is dried (at 404) to a high fiber dried distiller grain (HF-DDG) co-product.


In some embodiments, due to the composition of the fiber cake, there is less water retention of the product after separation of the thin stillage and washing. As the fiber cake includes less water, there is a substantial reduction in drying costs associated with the production of the high fiber dried distiller grain (HF-DDG) co-product over a more traditional DDG product. In some embodiments, the solid content of the fiber cake may be as high as between around 40% to around 45% solids before drying, as opposed to a wet cake (used to make conventional DDG) which typically includes only about 30% to around 35% solids prior to drying.


In some embodiments, the thin stillage is fractionated (at 406) into an oil emulsion, a protein paste, and a clarified thin stillage. The protein paste, which includes a high lysine content, is dried (at 408) to generate a high protein dried distillers grain (DDG HP). In some embodiments, the protein paste may also be returned to the fiber cake and dried together to generate an enhanced DDG product. Handling of the protein paste may be determined by market considerations, and equipment available at the ethanol production facility.


The thin stillage may then be condensed (at 410) to a high solids content (e.g., between around 30 to 80 percent solids) to generate a high solids syrup. High solids syrups are usable as an effective animal feed substitute, however the generation of practical high solid syrup may be difficult to obtain. This is because most syrups generated from thin stillage, once the solid content approaches about 30 percent, become prohibitively viscous, and are unusable as a marketable co-product. By processing the thin stillage to a clarified thin stillage, ultra high solids content (e.g., greater than about 30%) is achievable in a syrup which retains a viscosity of molasses. Thus, the co-product is easily transported and handled by prospective buyers.


Lastly, the oil emulsion is treated to extract valuable oil (at 412). Oil extraction is facilitated by pH adjusting the emulsion with an alkali. The addition of the caustic agent disrupts the emulsion and liberates the oil. The liberated oil may be extracted from the remaining emulsion via decanting, centrifugation, filtration or other suitable method. In some embodiments, greater than about 1.33 pounds of corn oil are achieved per bushel of corn utilizing the disclosed embodiments.


A series of limited examples were conducted according to an exemplary embodiment of the system (as shown in FIG. 3) in an effort to determine suitable apparatus and operating conditions for the fractionation of whole stillage. The following examples are intended to provide clarity to some embodiments of systems and means of operation; given the limited nature of these examples, they do not limit the scope of the disclosed aspects.


Example 1

In this example experiment, whole stillage was screened utilizing a screen centrifuge in order to obtain a fiber cake and thin stillage. The fiber cake was dried and tested for composition. The thin stillage was further processed by decanter centrifuge to yield an oil emulsion, clarified thin stillage and a protein paste. The protein paste was dried. The clarified thin stillage was evaporated to over 60% solids content. The oil emulsion was treated using a caustic agent to adjust the pH to about 8. The oil emulsion was again subjected to centrifugation in order to remove the oil form emulsion. The oil, dried protein paste and high solid syrup were then subjected to compositional analysis. The results of this analysis are provided in relation to TABLE 1 of FIG. 5.


In summary, the oil product had 0.9% moisture content, 3.03% free fatty acids (FFA), <0.01% insolubles, and 1.13% unsaponifiables. The high solids syrup composition was 31.6% moisture, 10.9% protein, 0.1% fiber, 6.1% ash, and 8.2% fat. The protein paste composition was 58.6% protein, 12.6% fat, and <1% fiber. The high fiber DDG composition was 26.0% protein, 10% fiber, 3.5% fat, and 0.7% ash.


The yields of the four products on a percentage basis are approximately 9% oil, 13% syrup, 40% protein, and 38% fiber. These yields correspond to 1.3 lb oil, 2 lb syrup, 6 lb protein, and 6 lb fiber on a pound per bushel basis. The yields expected can lead to changes to the expected compositions due to tradeoffs between yield and purity. The expected compositional ranges from commercial production of these products are show in TABLE 2 of FIG. 6.


The embodiments as disclosed and described in the application (including the FIGURES and Examples) are intended to be illustrative and explanatory. Modifications and variations of the disclosed embodiments, for example, of the apparatus and processes employed (or to be employed) as well as of the compositions and treatments used (or to be used), are possible; all such modifications and variations are intended to be within the scope of the various aspects presented herein.


The word “exemplary” is used to mean serving as an example, instance, or illustration. Any embodiment or design described as “exemplary” is not necessarily to be construed as preferred or advantageous over other embodiments or designs, nor is it meant to preclude equivalent exemplary structures and techniques known to those of ordinary skill in the art. Rather, use of the word exemplary is intended to present concepts in a concrete fashion, and the disclosed subject matter is not limited by such examples.


Reference throughout this specification to “one aspect,” or “an aspect,” or “one embodiment,” or “an embodiment” means that a particular feature, structure, or characteristic described in connection with the aspect or embodiment is included in at least one aspect or one embodiment. Thus, the appearances of the phrase “in one aspect,” or “in an aspect,” or “in one embodiment,” or “in an embodiment” in various places throughout this specification can, but are not necessarily, referring to the same aspect or embodiment, depending on the circumstances. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more aspects or embodiments.


The term “or” is intended to mean an inclusive “or” rather than an exclusive “or.” To the extent that the terms “comprises,” “has,” “contains,” and other similar words are used in either the detailed description or the claims, for the avoidance of doubt, such terms are intended to be inclusive in a manner similar to the term “comprising” as an open transition word without precluding any additional or other elements.

Claims
  • 1. A method for processing whole stillage in an ethanol plant, comprising: a) separating thin stillage liquid and fiber cake from the whole stillage;b) separating protein paste output and oil emulsion from the thin stillage liquid;c) drying protein paste output via a dryer system to form a protein animal feed product;d) separating oil from the oil emulsion to form a residual aqueous layer, wherein the residual aqueous layer comprises protein; ande) combining at least a portion of the residual aqueous layer with at least a portion of the fiber cake.
  • 2. The method of claim 1, wherein the protein animal feed product has at least 45% protein.
  • 3. The method of claim 1, wherein separating protein paste output from the thin stillage liquid comprises separating the thin stillage liquid into a clarified liquid stillage, an oil emulsion and the protein paste output.
  • 4. The method of claim 3, further comprising sending at least a portion of the clarified liquid stillage to an evaporation system to concentrate the clarified liquid stillage into a concentrated, clarified liquid stillage.
  • 5. The method of claim 1, further comprising forming an animal feed product with the at least a portion of the residual aqueous layer and the at least a portion of the fiber cake.
  • 6. The method of claim 5, wherein the at least a portion of the residual aqueous layer and the at least a portion of the fiber cake are dried in a dryer system to form an animal feed product.
  • 7. The method of claim 1, wherein separating thin stillage liquid from the whole stillage comprises separating thin stillage liquid from the whole stillage via filtration, centrifugation, pressing, and combinations thereof, and wherein separating protein paste output and oil emulsion from the thin stillage liquid comprises separating protein paste output and an oil emulsion from the thin stillage liquid via filtration, centrifugation, and combinations thereof.
  • 8. The method of claim 1, wherein separating thin stillage liquid from the whole stillage comprises separating thin stillage liquid from the whole stillage via one or more membranes, one or more screw presses, one or more decanters, one or more centrifuges, one or more filters, and combinations thereof, and wherein separating protein paste output and oil emulsion from the thin stillage liquid comprises separating protein paste output and an oil emulsion from the thin stillage liquid via a separation system comprising one or more separators, wherein the one or more separators are chosen from a three phase separator, a disk nozzle type centrifuge, a decanter centrifuge, and combinations thereof.
  • 9. The method of claim 1, wherein separating thin stillage liquid from the whole stillage comprises separating thin stillage liquid from the whole stillage via one or more filtration centrifuges.
  • 10. A method for processing whole stillage in an ethanol plant, comprising: a) separating thin stillage liquid and fiber cake from the whole stillage;b) separating protein paste and oil emulsion from the thin stillage liquid;c) separating oil from the oil emulsion to form a residual aqueous layer, wherein the residual aqueous layer comprises protein; andd) forming an animal feed product with at least a portion of the residual aqueous layer and at least a portion of the protein paste.
  • 11. The method of claim 10, wherein separating thin stillage liquid and fiber cake from the whole stillage is performed via filtration, centrifugation, pressing, and combinations thereof, and wherein separating protein paste output and oil emulsion from the thin stillage liquid is performed via filtration, centrifugation, and combinations thereof.
  • 12. The method of claim 10, wherein separating thin stillage liquid and fiber cake from the whole stillage is performed via one or more membranes, one or more screw presses, one or more decanters, one or more centrifuges, one or more filters, and combinations thereof, and wherein separating protein paste output and oil emulsion from the thin stillage liquid is performed via a separation system comprising one or more separators, wherein the one or more separators are chosen from a three phase separator, a disk nozzle type centrifuge, a decanter centrifuge, and combinations thereof.
  • 13. The method of claim 10, wherein separating oil from the oil emulsion to form a residual aqueous layer comprises contacting the oil emulsion with alkali to break the emulsion and form the oil and the residual aqueous layer.
  • 14. The method of claim 13, wherein oil is separated from residual aqueous layer via centrifugation, decanting, and combinations thereof.
  • 15. The method of claim 10, wherein the forming an animal feed product comprises forming an animal feed product with the at least a portion of the residual aqueous layer, the at least a portion of the protein paste, and at least a portion of the fiber cake.
  • 16. A method for processing whole stillage in an ethanol plant, comprising: separating thin stillage liquid and fiber cake from the whole stillage;separating protein paste and oil emulsion from the thin stillage liquid;separating oil from the oil emulsion to form a residual aqueous layer output, wherein the residual aqueous layer output comprises protein; andcombining at least a portion of the residual aqueous layer output with at least a portion of the fiber cake.
  • 17. The method of claim 16, wherein separating thin stillage liquid and fiber cake from the whole stillage is performed via filtration, centrifugation, pressing, and combinations thereof, and wherein separating protein paste output and oil emulsion from the thin stillage liquid is performed via filtration, centrifugation, and combinations thereof.
  • 18. The method of claim 16, wherein separating thin stillage liquid and fiber cake from the whole stillage is performed via one or more membranes, one or more screw presses, one or more decanters, one or more centrifuges, one or more filters, and combinations thereof, and wherein separating protein paste output and oil emulsion from the thin stillage liquid is performed via a separation system comprising one or more separators, wherein the one or more separators are chosen from a three phase separator, a disk nozzle type centrifuge, a decanter centrifuge, and combinations thereof.
  • 19. The method of claim 16, wherein separating oil from the oil emulsion to form a residual aqueous layer comprises contacting the oil emulsion with alkali to break the emulsion and form the oil and the residual aqueous layer.
  • 20. The method of claim 19, wherein oil is separated from residual aqueous layer via centrifugation, decanting, and combinations thereof.
  • 21. The method of claim 16, wherein the combining comprises combining the at least a portion of the residual aqueous layer output with the at least a portion of the fiber cake and at least a portion of the protein paste.
Parent Case Info

This application is a Continuation of application Ser. No. 16/534,165 filed Aug. 7, 2019, which is a Divisional of Ser. No. 15/015,355 filed Feb. 4, 2016, which is a Divisional of application Ser. No. 14/112,897 filed Apr. 11, 2014, which is a U.S. national stage filing of Patent Cooperation Treaty (PCT) application serial number PCT/US2012/033346 filed on Apr. 12, 2012, which claims the benefit of U.S. Provisional Application Ser. No. 61/476,702, filed Apr. 18, 2011, wherein the entirety of each of said patent applications is incorporated herein by reference.

US Referenced Citations (164)
Number Name Date Kind
2446913 Erlich Aug 1948 A
2478937 Niethamer Aug 1949 A
2698826 Peltzer, Sr. Jan 1955 A
3538551 Joa Nov 1970 A
3761027 Mendoza Sep 1973 A
4056636 Muller Nov 1977 A
4361651 Keim Nov 1982 A
4565330 Katoh Jan 1986 A
5195684 Radzins Mar 1993 A
5248449 Mitchell Sep 1993 A
5250182 Bento et al. Oct 1993 A
5662810 Willgohs Sep 1997 A
5795477 Herman et al. Aug 1998 A
6106673 Walker Aug 2000 A
6117321 Johnston Sep 2000 A
6230995 Niemi et al. May 2001 B1
6475132 Zettier Nov 2002 B2
6509180 Verser et al. Jan 2003 B1
6962722 Dawley et al. Nov 2005 B2
7083954 Jakel et al. Aug 2006 B2
7101691 Kinley et al. Sep 2006 B2
7300680 Prevost et al. Nov 2007 B2
7384010 Horigane et al. Jun 2008 B2
7497955 Scheimann et al. Mar 2009 B2
7507562 Verser et al. Mar 2009 B2
7572353 Vander Griend Aug 2009 B1
7601858 Cantrell et al. Oct 2009 B2
7608729 Winsness et al. Oct 2009 B2
7699255 Kapper Apr 2010 B2
7829680 Sander et al. Nov 2010 B1
7842484 Lewis Nov 2010 B2
7857608 Fabbricante et al. Dec 2010 B2
7858140 Paustian et al. Dec 2010 B2
7886996 Horigane et al. Feb 2011 B2
7888082 Verser et al. Feb 2011 B2
7915458 Bruckmayer Mar 2011 B2
7919289 Lewis Apr 2011 B2
7935370 Prevost et al. May 2011 B1
7954734 Hata Jun 2011 B2
8017365 Rein et al. Sep 2011 B1
8093023 Prevost et al. Jan 2012 B1
8103385 Macharia et al. Jan 2012 B2
8126606 Hung Feb 2012 B2
8168037 Winsness May 2012 B2
8192627 Gallop et al. Jun 2012 B2
8236086 Janssen et al. Aug 2012 B2
8236977 Woods et al. Aug 2012 B2
8257951 Prevost et al. Sep 2012 B2
8449728 Redford May 2013 B2
8454802 Redford Jun 2013 B2
8524473 Hammond et al. Sep 2013 B2
8563282 Galvez, III et al. Oct 2013 B2
8597917 Medoff et al. Dec 2013 B2
8603786 Redford Dec 2013 B2
8679353 Winsness Mar 2014 B2
8702819 Bootsma Apr 2014 B2
8722372 Kiuchi et al. May 2014 B2
8722911 Bleyer et al. May 2014 B2
8735544 Prevost et al. May 2014 B1
8748141 Lewis et al. Jun 2014 B2
8778433 Lee Jul 2014 B2
8813973 Lee et al. Aug 2014 B2
8927239 Allen et al. Jan 2015 B2
8956460 Ahmed et al. Feb 2015 B2
8962059 Froderman et al. Feb 2015 B1
8986551 Kohl et al. Mar 2015 B2
9012191 Lee Apr 2015 B2
9012668 Winsness Apr 2015 B2
9029126 Bleyer et al. May 2015 B2
9040270 Prevost et al. May 2015 B2
9061987 Bootsma Jun 2015 B2
9108140 Winsness Aug 2015 B2
9114114 Anderson et al. Aug 2015 B2
9150790 Thorn et al. Oct 2015 B2
9169498 Woods et al. Oct 2015 B2
9212334 Cantrell et al. Dec 2015 B2
9290728 Bootsma Mar 2016 B2
9320990 Winsness Apr 2016 B2
9328311 Jenkins et al. May 2016 B2
9340767 Narendranath May 2016 B2
9353332 Lewis et al. May 2016 B2
9375731 Dieker et al. Jun 2016 B2
9714267 Emanuele et al. Jul 2017 B2
9745540 Sungail et al. Aug 2017 B2
9896643 Redford Feb 2018 B2
10837029 Bootsma et al. Nov 2020 B2
11078500 Hansen et al. Aug 2021 B2
11104873 Bootsma Aug 2021 B2
20040087808 Prevost et al. May 2004 A1
20040192896 Finch Sep 2004 A1
20040234649 Lewis et al. Nov 2004 A1
20050233030 Lewis et al. Oct 2005 A1
20050239181 Lewis et al. Oct 2005 A1
20060194296 Hammond et al. Aug 2006 A1
20070031953 Dunson, Jr. et al. Feb 2007 A1
20070036881 Griffith Feb 2007 A1
20070141691 Hirl Jun 2007 A1
20070148318 Rubio et al. Jun 2007 A1
20070190626 Wilkening et al. Aug 2007 A1
20070238691 Thompson et al. Oct 2007 A1
20070254089 Hickey et al. Nov 2007 A1
20080009048 Bhargava et al. Jan 2008 A1
20080110577 Winsness May 2008 A1
20080193991 Allen et al. Aug 2008 A1
20080277264 Sprague Nov 2008 A1
20090093027 Balan et al. Apr 2009 A1
20090176289 Friedmann Jul 2009 A1
20090250412 Winsness et al. Oct 2009 A1
20090269817 Lantero Oct 2009 A1
20090311397 Whalen et al. Dec 2009 A1
20100055741 Galvez, III et al. Mar 2010 A1
20100159519 Diner et al. Jun 2010 A1
20100199062 Sancho-Dominguez et al. Aug 2010 A1
20100221804 Veit et al. Sep 2010 A1
20100281765 Schwartz Nov 2010 A1
20110003341 Nojiri et al. Jan 2011 A1
20110086149 Bootsma Apr 2011 A1
20110142788 Sellier et al. Jun 2011 A1
20110143411 Yuan et al. Jun 2011 A1
20120051980 Gallop et al. Mar 2012 A1
20120064213 Lee Mar 2012 A1
20120244590 Lee Sep 2012 A1
20130165678 Kohl et al. Jun 2013 A1
20130295661 Roesch et al. Nov 2013 A1
20140024084 Galvez, III et al. Jan 2014 A1
20140110512 Lee Apr 2014 A1
20140155639 Sticklen et al. Jun 2014 A1
20140178946 Galvez, III et al. Jun 2014 A1
20140242251 Bootsma Aug 2014 A1
20140273166 Narendranath Sep 2014 A1
20140315259 Woods et al. Oct 2014 A1
20150024451 Williams Jan 2015 A1
20150037857 Redford Feb 2015 A1
20150056327 Redford Feb 2015 A1
20150076078 Gallop Mar 2015 A1
20150118727 Escudero et al. Apr 2015 A1
20150147786 Clarkson et al. May 2015 A1
20150152196 Phanopoulos et al. Jun 2015 A1
20150152372 Kohl et al. Jun 2015 A1
20150181911 Redford Jul 2015 A1
20150181912 Redford Jul 2015 A1
20150182882 Gallop et al. Jul 2015 A1
20160024406 Javers et al. Jan 2016 A1
20160145650 Lewis et al. May 2016 A1
20160152931 Bootsma Jun 2016 A1
20160222135 Lee Aug 2016 A1
20170051322 Bushong et al. Feb 2017 A1
20170107452 Dasari et al. Apr 2017 A1
20170114293 Jakel et al. Apr 2017 A1
20170166834 Jakel Jun 2017 A1
20170166835 Jakel Jun 2017 A1
20170226165 Franko et al. Aug 2017 A1
20170253892 Bootsma Sep 2017 A1
20170268024 Bootsma et al. Sep 2017 A1
20180016602 Franko et al. Jan 2018 A1
20180044620 Bootsma Feb 2018 A1
20180126302 Gallop May 2018 A1
20180242626 Froderman et al. Aug 2018 A1
20180355387 Javers et al. Dec 2018 A1
20190017080 Bootsma Jan 2019 A1
20200140899 Bootsma May 2020 A1
20210017547 Bootsma Jan 2021 A1
20210251256 Gibbons et al. Aug 2021 A1
20220015381 Rindsig et al. Jan 2022 A1
Foreign Referenced Citations (8)
Number Date Country
2833395 Feb 1996 AU
2005029974 Apr 2005 WO
2010138110 Dec 2010 WO
2017059083 Apr 2017 WO
2017091760 Jun 2017 WO
2017091766 Jun 2017 WO
2018215965 Nov 2018 WO
2018217202 Nov 2018 WO
Non-Patent Literature Citations (40)
Entry
Pleasant Hill Grain, “ABC Hansen Disc Mill”, website catalog pp. 1-8, retrieved on Aug. 9, 2015, (8 pages).
Rausch et al., “Particle Size Distributions of Ground Corn and DDGS from Dry Grind Processing”, Transactions of the ASAE, vol. 48, No. 1, pp. 273-277, 2005, (5 pages).
“Disc Mill DM 400-Retsch-Powerful grinding and robust design”, retrieved from “https://www.retsch.com/products/milling/disc-mills/dm-400/function-features/”, on Aug. 19, 2015, (2 pages).
Kotrba, “Ethanol Producers Talk Shop”, restreived from “http://www.ethanolproducer.com/articles/2213/ethanol-producers-talk-shop”, dated Aug. 1, 2006, (3 pages).
“Corn Wet Milling Process Description”, Fluid Quip-Ethanol Industry, website pp. 1-6, retrieved on Aug. 19, 2015, (6 pages).
International Standard, ISO 13320:2009(E), Particle Size Analysis—Laser Diffraction Methods, pp. 1-58, 2009, (58 pages).
Akinoso et al., “Work Index and Milling Efficiency of Size Reduction of Maize Using Plate Mill”, Agricultural Engineering Today, vol. 36, pp. 22-28, 2012, (3 pages). (Abstract Only).
Rosentrater, “Production and use of evolving corn-based fuel ethanol coproducts in the U.S”, Biofuels—Status and Perspective, Chapter 5, pp. 81-98, 2015, (18 pages).
Olson, “A Lecture on Pressure Screening”, Mechanical Engineering Department, University of British Columbia, 2003, (17 pages).
Kim et al., “Process simulation of modified dry grind ethanol plant with recycle of pretreated and enzymatically hydrolyzed distillers' grains”, Bioresource Technology, vol. 99, pp. 5177-5192, 2008, (16 pages).
Nouroddini et al., “Stagewise Dilute-Acid Pretreatment and Enzyme Hydrolysis of Distillers' Grains and Corn Fiber”, Appl Biochem Biotech, vol. 159, pp. 553-567, 2009, (15 pages).
Sluiter et al., “Determination of Total Solids in Biomass and Total Dissolved Solids in Liquid Process Samples”, National Renewable Energy Laboratory, pp. 1-9, 2008, (9 pages).
Sluiter et al., “Determination of Ash in Biomass”, National Renewable Energy Laboratory, pp. 1-8, 2005, (8 pages).
Hames et al., “Determination of Protein Content in Biomass”, National Renewable Energy Laboratory, pp. 1-8, 2008, (8 pages).
Sluiter et al., “Determination of Extractives in Biomass”, National Renewable Energy Laboratory, pp. 1-12, 2005, (12 pages).
Sluiter et al., “Determination of Structural Carbohydrates and Lignin in Biomass”, National Renewable Energy Laboratory, pp. 1-18, 2012, (18 pages).
Sluiter et al., “Determination of starch in solid biomass samples”, National Renewable Energy Laboratory, pp. 1-7, 2005, (4 pages). (Abstract only).
Ankom, “Acid Detergent Fiber in Feeds—Filter Bag Technique (for A2000 and A2000I)”, ADF method, pp. 1-2, 2017, (2 pages).
Cheetham et al., “Variation in crystalline type with amylase content in maize starch granules: an X-ray powder diffraction study”, Carbohydrate Polymers, vol. 36, pp. 277-284, 1998, (8 pages).
Nara et al., “Studies on the Relationship Between Water-satured State and Crystallinity by the Diffraction Method or Moistened Potato Starch”, Starch, vol. 35, Issue 12, pp. 407-410, 1983, (3 pages). (Abstract only).
Beneditti et al., “X-ray diffraction methods to determine crystallinity and preferred orientation of lithium disilicate in Li—Zn-silicate glass-ceramic fibres”, Journal of Materials Science, vol. 18, pp. 1039-1048, 1983, (8 pages). (Abstract Only).
AOAC International “AOAC 965.22-1966”, p. 1, 1996, (1 page).
Wongsagonsup et al., “Effects of Different Mill Types on Ethanol Production Using Uncooked Dry-Grind Fermentation and Characteristics of Residual Starch in Distiller's Dried Grains (DDG)”, Cereal Chemistry, vol. 94, Issue 4, pp. 645-653, 2017, (2 pages). (Abstract only).
Chatzifragkou et al., “Biorefinery strategies for upgrading distillers' dried grains with solubles (DOGS)”, Process Biochemistry, vol. 50, pp. 2194-2207, 2015, (14 pages).
Unpublished United States Utility U.S. Appl. No. 17/666,092, filed Feb. 7, 2022 (no attachment).
Unpublished United States Utility U.S. Appl. No. 17/675,928, filed Feb. 18, 2022 (no attachment).
Svonja, “From Operating Ease to Operating Costs: Weighing Differences in DDGS Dryers”, retreived from http://ethanolproducer.com/articles/3032/from-operating-ease-to-operating-costs-weighing-differences-in-ddgs-dryers, May 22, 2007, (3 pages).
Flash Dryer, retrieved from https://www.gea.com/en/products/dryers-particle-processing/flash-dryers-coolers/flash-dryer.jsp, on Jun. 9, 2020, (11 pages).
Ring Dryer, retrieved from https://www.gea.com/en/products/dryers-particle-processing/ring-dryers/ring-dryer.jsp, on Jun. 9, 2020, (12 pages).
“Thin Stillage Solids Separation System”, retrieved on Jun. 26, 2018 via http://www.icminc.com/products/thin-stillagesolids-separation-system.html, (2 pages).
“About Harvesting Technology: Bringing Profitable Innovation for Ethanol Production”, retrieved on Jun. 26, 2018 via http://harvestingtech.com/#benefits, (11 pages).
Office Action for Mexican Patent Application No. MX/a/2013/012195 dated Jun. 27, 2016, (2 pages).
Non-Final Office Action for U.S. Appl. No. 14/112,897 dated May 21, 2015, (19 pages).
Hunt, et al. “Corn Stillage as a Feedstuff for Broilers and Turkeys”, Applied Poultry Science, Inc., Research Report 1997, published online at http://japr.fass.org/contenl/6/3/310.full.pdf, (9 pages).
Intemational Search Report and Written Opinion for PCT Application Serial No. PCT/US2012/033346, dated Sep. 20, 2012, (14 pages).
European Search Report for European Application No. EP12774824.2 dated Jan. 26, 2015, (5 pages).
Abdel-Tawwab et al., “Evaluation of commercial live bakers' yeast, Saccharomyces cerevisiae as a growth and Immunity promoter for Fry Nile tilapia, Oreochromis niloticus (L.) challenged in situ with Aeromonas hydrophila”, Aquaculture, vol. 280, Issues 1-4, pp. 185-189, 2008, (5 pages).
Kim et al., “Composition of corn dry-grind ethanol by-products: DDGS, wet cake, and thin stillage”, ScienceDirect, Bioresource Technology, vol. 99, pp. 5165-5176, 2008, (12 pages).
Rausch et al., “The Future of Coproducts From Corn Processing”, Applied Biochemistry and Biotechnology, vol. 128, pp. 47-86, 2006, (40 pages).
Yamada et al., “Yeast (Saccharomyces cerevisiae) Protein Concentrate: Preparation, Chemical Composition, and Nutritional and Functional Properties”, Journal of Agricultural and Food Chemistry, vol. 53, No. 10, pp. 3931-3936, 2005, (6 pages).
Related Publications (1)
Number Date Country
20210214659 A1 Jul 2021 US
Provisional Applications (1)
Number Date Country
61476702 Apr 2011 US
Divisions (2)
Number Date Country
Parent 15015355 Feb 2016 US
Child 16534165 US
Parent 14112897 US
Child 15015355 US
Continuations (1)
Number Date Country
Parent 16534165 Aug 2019 US
Child 17218508 US