| OBSERVATION'S |
Patent on his process for recovering glycerin and other chemicals. Although inventor`s technology has yet to be used commercially, he says he almost won a convert in the early 1990s when French sugar refiner Béghin-Say became interested in using the process to recover chemicals at its sugar beet ethanol operations. The firm was prepared to invest in commercial manufacturing but put the project on hold in 1992 after merging with Italy's Eridania and dropped it altogether in 1994. Inventor says he regained rights to the technology in 1997, after a three-year standstill agreement with Béghin-Say expired, and started approaching fuel ethanol producers. According to inventor recovering the glycerin that is already being made in ethanol plants is just the start for his technology. By playing with yeast strains, pH, temperature, and other variables, he says the fermentation process can be tweaked to yield a full pound per gallon, without any reduction in ethanol yield. He anticipates that 99.7% pure glycerin can be produced for as little as 15 cents per lb, well below the cost for on-purpose makers such as Dow. Further, he says, the equipment installed to separate and recover glycerin can also be directed at lower volume ethanol coproducts such as lactic acid, succinic acid, and the B vitamin inositol. |
| UPDATE | 02.00 |
| LITERATURE REF. | This data is not available for free |
| PATENT NUMBER | This data is not available for free |
| PATENT GRANT DATE | January 5, 1993 |
| PATENT TITLE |
Process for manufacturing ethanol and for recovering glycerol, succinic acid, lactic acid, betaine, potassium sulfate, and free flowing distiller's dry grain and solubles or a solid fertilizer therefrom |
| PATENT ABSTRACT |
This invention relates to the manufacture of ethanol and the recovery of such by-products therefrom as glycerol, betaine, succinic and lactic acid, potassium sulfate and a free flowing distiller's dry grain and solubles useful as an animal feed or a component of food for humans or as a premix for agricultural fertilizer. The process disclosed is an improvement over that of U.S. application Ser. No. 136,415 in the area of enhancement of glycerol recovery from stillage resulting from the fermentation of a biomass mash, and involves production of glycerol in amount in excess of 10 grams per 100 grams of reducing sugar in the starting biomass mash. |
| PATENT INVENTORS | This data is not available for free |
| PATENT FILE DATE | July 18, 1989 |
| PATENT REFERENCES CITED |
"The Merck Index," 10th Ed., Merck & Co., Inc., Rahway N.J. pp. 1189, 4347, 5172 and 8746-1983. Puspito et al., CA 86:122152, 1985. Burris, "Recovery of Chemicals such as Glycerol, Dextrose, and Amino Acids from Dilute Broths", Int. Conf. Fuels Alc. Chem from Biomass, Nov. 10-12, 1986, Miami Beach, Fla. |
| PATENT PARENT CASE TEXT | This data is not available for free |
| PATENT CLAIMS |
What is claimed is: 1. A process for manufacturing ethanol and recovering glycerol as a by-product thereof comprising the steps of: preparing a biomass mash, fermenting the biomass mash with yeast to produce a fermented mash having at least about 9 grams of glycerol and 40 grams of ethanol per 100 grams of reducing sugar in the biomass mash, distilling the fermented mash for producing ethanol and stillage, clarifying the stillage produced from the distillation of the fermented mash by subjecting the liquid portion thereof to a cross-flow microfiltration system having inorganic membranes with pore sizes of 0.1 to about 10 microns, passing the clarified stillage through an ion exclusion material for separating glycerol from other constituents of the clarified stillage, and purifying the separated glycerol. 2. A process for manufacturing ethanol and recovering glycerol and betaine as by-products thereof comprising the steps of: preparing a biomass mash from sugar beets, fermenting the biomass mash with yeast to produce a fermented mash, distilling the fermented mash for producing ethanol and stillage, clarifying the stillage from the distillation of the fermented mash by subjecting the liquid portion thereof to a cross-flow microfiltration system having inorganic membranes with pore sizes of 0.1 to about 10 microns, subjecting the clarified stillage to chromatographic separation by passing the stillage through an ion exclusion material for separating glycerol and betaine from other constituents of the clarified stillage and then from each other, and purifying the separated glycerol and betaine. 3. A continuous process for manufacturing ethanol and recovering glycerol as by product thereof comprising the steps of: preparing a biomass mash, and in a continuous process performing the steps of: fermenting the biomass mash with yeast to produce a fermented mash having at least about 9 grams of glycerol and 40 grams of ethanol per 100 grams of reducing sugar in the biomass mash, distilling the fermented mash for producing ethanol and stillage, clarifying the stillage produced from the distillation of the fermented mash by subjecting the liquid portion thereof to a cross-flow microfiltration system having inorganic membranes with pore sizes of 0.1 to about 10 microns, 4. A continuous process for manufacturing ethanol and recovering glycerol as by-products thereof comprising the steps of: preparing a biomass mash from sugar beets, and in a continuous process performing the steps of: fermenting the biomass mash with yeast to produce a fermented mash, distilling the fermented mash for producing ethanol and stillage, clarifying the stillage produced from the distillation of the fermented mash by subjecting the liquid portion thereof to a cross-flow microfultration system having inorganic membranes with pore sizes of 0.1 to about 10 microns, subjecting the clarified stillage to chromatographic separation for separating a glycerol product stream from other constituents of the clarified stillage, and purifying the separated glycerol product stream. 5. A process according to one of claims 1 or claim 2 or claim 3 or claim 4 wherein the step of fermenting a biomass mash comprises the step of mixing with the mash yeast cells in a concentration in excess of 100 grams per liter. 6. A process according to one of claims 1 or claim 2 or claim 3 or claim 4 wherein the step of preparing a biomass mash comprises the step of preparing a biomass mash having a dextrose equivalent of at least about 80 and the step of fermenting comprises mixing yeast cells with the mash. 7. A process according to one of claim 1 or claim 2 or claim 3 or claim 4 wherein the step of fermenting comprises the step of maintaining the pH of the mash substantially constant during the first two thirds of the fermentation process. 8. A process according to one of claim 1 or claim 2 or claim 3 or claim 4 wherein the step of fermenting the biomass mash comprises producing a fermented mash having at least about 15 grams of glycerol and 40 grams of ethanol per 100 grams of reducing sugar in the biomass mash. 9. A process according to one of claims 1 or claim 2 or claim 3 or claim 4 wherein the step of fermenting a biomass mash comprises the steps of preparing immobilized yeast cells, and mixing the immobilized yeast cells with the biomass mash. 10. A process according to one of claim 1 or claim 2 wherein the step of clarifying further comprises centrifugally separating solids from liquid constituents prior to microfiltration. 11. A process for manufacturing ethanol and recovering at least two of glycerol, betaine, and succinic acid as by-products thereof comprising the steps of: preparing a fermented mash from sugar beets, distilling the fermented mash for producing ethanol and stillage, clarifying the stillage produced from the distillation of the fermented mash by subjecting the liquid portion thereof to a cross-flow microfiltration system having inorganic membranes with pore sizes of 0.1 to about 10 microns, passing the clarified stillage through an ion exclusion material for separating glycerol and succinic acid and betaine one from another and from other constituents of the clarified stillage, purifying the separated glycerol, succinic acid, and betaine, and drying any stillage residue. 12. A process for manufacturing ethanol and recovering glycerol and lactic acid as by-products thereof comprising the steps of: preparing the biomass mash, fermenting the biomass mash with yeast to produce a fermented mash having at least about 9 grams of glycerol and 40 grams of ethanol per 100 grams of reducing sugar in the biomass mash, distilling the fermented mash for producing ethanol and stillage, clarifying the stillage produced from the distillation of the fermented mash by subjecting the liquid portion thereof to a cross-flow microfiltration system having inorganic membranes with pore sizes of 0.1 to about 10 microns, and passing the clarified stillage through an ion exclusion material for separating glycerol and lactic acid one from another and from other constituents of the clarified stillage. 13. A process for manufacturing ethanol and recovering glycerol and betaine as by-products thereof comprising the steps of: preparing a biomass mash from sugar beets, fermenting the biomass mash with yeast to produce a fermented mash, distilling the fermented mash for producing ethanol and stillage, clarifying the stillage produced from the distillation of the fermented mash by subjecting the liquid portion thereof to a cross-flow microfiltration system having inorganic membranes with pore sizes of 0.1 to about 10 microns, subjecting the clarified stillage to chromatographic separation by passing the stillage through an ion exclusion material for separating glycerol and betaine from the other constituents of the clarified stillage and then from each other, and purifying the separated glycerol and betaine. -------------------------------------------------------------------------------- |
| PATENT DESCRIPTION |
FIELD AND BACKGROUND OF INVENTION This invention relates to the manufacture of ethanol, and the recovery, as by-products thereof, glycerol, betaine, succinic and/or lactic acid, potassium sulfate and a free flowing distiller's dry grain and solubles useful as a food for animals or humans or as a premix for agricultural fertilizer. The manufacture and/or recovery of all of the products named has been known heretofore, and all have commercial uses. Ethanol is used as a beverage, a chemical, and a fuel derived from renewable resources, and is typically manufactured by fermentation and distillation processes starting from biological materials such as corn, wheat or other grain, sugar cane or beets, grapes or other fruit, potatoes, cassava, sweet sorghum or the like. Glycerol, while known to be produced as a by-product of ethanol fermentation and distillation processes, has been manufactured commercially only by processes which have soap as the primary product or which synthesize glycerol from petrochemical feedstocks. Betaine is produced synthetically or from liquors of beet molasses. Succinic acid is synthesized from maleic or acetic acid or produced by means of a highly specific fermentation. Lactic acid is produced by fermentation with Lactobacillus delbrueckii, B. dextrolacticus or similar microorganisms. Potassium sulfate is usually obtained by reacting sulfuric acid with potassium chloride. Potassium chloride usually occurs in nature as the mineral sylvine or sylvite. Distiller's dry grain, characterized as with or without solubles, is conventionally produced as a by-product of fermentation and distillation processes, and is usually sufficiently infused with sticky by products such as glycerol as to have poor flowing qualities and be difficult to handle. If the substrate from which distillates are produced is a sugar cane or beet material, then the residue is typically used only as a liquid fertilizer or treated as a waste. The manufacture of ethanol is sufficiently well known that the interested reader is referred to the available literature for descriptions of the basic processes. The manufacture of glycerol is, by way of example, discussed in Hildebrandt U.S. Pat. No. 2,160,245; Wallerstein U.S. Pat. 2,400,859; and Frankel U.S. Pat. No. 2,772,207, to which the interested reader is referred. The manufacture of succinic acid and free flowing distiller's dry grain by processes such as those to be described hereinafter has not, insofar as is known to the present inventor, been described in any prior patent other than that which has resulted from the aforementioned priority application. The processes and apparatus of the present invention contemplate the production of each or all of the products mentioned in a commercially feasible manner in a fermentation and distillation or similar process. BRIEF DESCRIPTION OF INVENTION More particularly, it is an object of this invention to produce glycerol as a valuable co-product of a fermentation process such as may produce ethanol. In realizing this object of the present invention, the efficiency of the known ethanol producing fermentation and distillation processes is essentially maintained, while an additional valuable product is derived. More particularly, ethanol production follows known and widely published pathways of biochemical reactions. The present invention contemplates imposing pressures on such pathways in ways which result in enhanced generation of glycerol and succinic acid, and has determined that such enhancement is achieved with relatively little if any reduction of efficiency in the production of ethanol. Likewise, a further object of this invention is the manufacture of betaine or betaine-HCl as a co-product of a fermentation from a substrate of sugar beets or similar materials. Yet a further object of this invention is the recovery of lactic acid from those fermentation processes, such as wet milled corn and certain wine fermentations, where lactic acid is produced in substantial quantities. -------------------------------------------------------------------------------- BRIEF DESCRIPTION OF DRAWING Some of the objects of the invention having been stated, other objects will appear as the description proceeds, when taken in connection with the accompanying drawing, in which a schematic representation of the flow of materials in the processes and apparatus of the present invention is shown . DETAILED DESCRIPTION OF INVENTION While the present invention will be described more fully hereinafter with reference to the accompanying drawing, in which a preferred embodiment of the present invention is shown, it is to be understood at the outset of the description which follows that persons of skill in the appropriate arts may modify the invention here described while still achieving the favorable results of this invention. Accordingly, the description which follows is to be understood as being a broad, teaching disclosure directed to persons of skill in the appropriate arts, and not as limiting upon the present invention. Referring now more particularly to the drawing accompanying this disclosure, the drawing represents certain steps and apparatus which, in the sequence disclosed hereinafter, accomplish the objects of this invention. Certain steps and apparatus, being well known to those having skill in the relevant arts, have not been shown but will be described for the reader. It is known that the formation of ethanol in a fermentation process with yeast cells or other microorganisms is growth associated and that the formation of glycerol and succinic acid is interrelated. More specifically, in the Embden-Meyerhof pathway, NADH from triose phosphate oxidation exceeds the rate of acetaldehyde reduction, thus accounting for normal glycerol formation when the cell starved for ATP from glycolysis shifts excess NADH to the reduction of dihydroxyacetone phosphate to glycerol. Additional NADH is supplied through the Kreb's citric acid cycle. As used herein, NADH refers to nicotinamide adenine dinucleotide and ATP to adenosine triphosphate. In a well run fermentation process without the recycle of stillage, some 48 grams of ethanol, 4.0 grams of glycerol, 0.6 gram of succinic acid, and small quantities of lactic acid are formed per 100 grams of reducing sugar consumed. Ethanol producers using a corn wet milling process generally have substantial quantities of lactic acid present in their fermented mash, as do certain wine and other fermentations. The commercially feasible recovery of the glycerol and succinic acid constituents, resulting in the production of free flowing DDG and/or DDGS, has been disclosed in the aforementioned priority application which is hereby incorporated herein by reference, and the present invention contemplates the further enhancement of the production of the by-products to be recovered and the recovery of additional by-products not contemplated by the previously disclosed invention. The processes by which such further enhancement and additional products are obtained and the result of operation in accordance with the present invention will be discovered from comparison of the processes given by the examples in the prior specification and those now to be described. |
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| PATENT PHOTOCOPY | Available on request |
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