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WO2011071842A2 - Procédé permettant d'augmenter la quantité d'éthanol produite à partir de céréales - Google Patents

Procédé permettant d'augmenter la quantité d'éthanol produite à partir de céréales Download PDF

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Publication number
WO2011071842A2
WO2011071842A2 PCT/US2010/059164 US2010059164W WO2011071842A2 WO 2011071842 A2 WO2011071842 A2 WO 2011071842A2 US 2010059164 W US2010059164 W US 2010059164W WO 2011071842 A2 WO2011071842 A2 WO 2011071842A2
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WIPO (PCT)
Prior art keywords
grain
cavitation
liquid medium
based liquid
enzyme
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Ceased
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PCT/US2010/059164
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WO2011071842A3 (fr
Inventor
Oleg Kozyuk
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Arisdyne Systems Inc
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Arisdyne Systems Inc
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Priority to CA2764909A priority Critical patent/CA2764909C/fr
Publication of WO2011071842A2 publication Critical patent/WO2011071842A2/fr
Publication of WO2011071842A3 publication Critical patent/WO2011071842A3/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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Classifications

    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P7/00—Preparation of oxygen-containing organic compounds
    • C12P7/02—Preparation of oxygen-containing organic compounds containing a hydroxy group
    • C12P7/04—Preparation of oxygen-containing organic compounds containing a hydroxy group acyclic
    • C12P7/06—Ethanol, i.e. non-beverage
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E50/00—Technologies for the production of fuel of non-fossil origin
    • Y02E50/10—Biofuels, e.g. bio-diesel

Definitions

  • the invention relates to a process for producing ethanol, and more
  • Alcohols are a renewable and clean fuel source.
  • a grain alcohol commonly used as a fuel source is ethanol, which can be produced, in large part, from corn by the fermentation of starch. Generally, ethanol production is accomplished through a
  • yeast fermentation processes wherein starches are released and converted to sugars, then the sugars are converted to alcohol by the addition of yeast.
  • yeast fermentation processes only convert about one -third of the corn into ethanol.
  • Ethanol production facilities often begin the production process with a dry or wet milling process.
  • dry milling corn, or another suitable grain, is ground up by a hammer or roller mill into a manageable mixture of coarse particles.
  • the dry mixture of particles is combined with water and enzymes to break up the starch from the corn into smaller fragments and then subject the fragments to a saccharification phase wherein the starch is converted to sugar.
  • saccharification phase the resulting sugars are fermented with yeast to facilitate their conversion to ethanol.
  • Ethanol yield is dependent upon the initial starch content of the corn as well as the availability of the starch to the enzymes that are used in the saccharification process.
  • the availability of starch is governed, in part, by the success of the milling or similar step in which the corn is broken up into smaller particles.
  • the production processes currently used in commercial ethanol plants are not able to achieve maximum theoretical ethanol yield, thus more corn than theoretically needed must be used to produce a certain amount of ethanol.
  • the method preferably uses a controlled cavitation device to increase enzyme activity and subsequently increase ethanol yield.
  • an enhanced enzymatic bio-conversion process of starches to ethanol could increase domestically produced bio-fuels and decrease importation of foreign oil.
  • the present invention is a process for producing alcohol, more specifically ethanol, from grain wherein the use of cavitation energy to enhance enzyme activity substantially increases the ethanol yield, comprising mixing a grain-based material with water and enzyme to form mashed pre-gelatinized grain-based liquid medium; and subjecting the said grain-based liquid medium to cavitation activation energy not less than 0.44 kJ and not more than 1.56 kJ per kilogram of said grain-based liquid medium at a temperature in the range of 130 F to 190 F.
  • FIG. 1 is a flow diagram of an ethanol production process using cavitation.
  • FIG. 2 is a cross section view of a controlled flow cavitation apparatus.
  • FIG. 3 is a cross section view of a controlled flow cavitation apparatus.
  • a range such as 5-25 (or 5 to 25) is given, this means preferably at least 5 and, separately and independently, preferably not more than 25. In an example, such a range defines independently not less than 5, and separately and independently, not more than 25.
  • the controlled use of cavitational energy to enhance enzyme activity in an ethanol production process can substantially increases the yield of ethanol from corn.
  • cavitational energy enhances enzyme activity, and thus increasing ethanol yield, is not known, there are several possible explanations.
  • the forces obtained from cavitation are used to disaggregate, disassociate, shake off and/or strip away starch granules from protein, and fiber, as well as disassociate tightly packed granules and tightly packed amyloplasts containing starch granules to make them more accessible to an enzyme for subsequent enzymatic treatment.
  • This increase in accessibility may increase enzyme action.
  • Cavitation energy may also enhance the transport of enzyme macromolecules toward the surface of the grain substrate.
  • absorption of cavitation energy by a protein may produce a transient conformational shift (modifying the 3-dimensional structure) and alter the protein's functional activity.
  • the collapse of cavitation bubbles which can enhance the removal of hydrolysis reaction products from the reaction zone, may contribute to an overall increase in the reaction rate.
  • FIG. 1 shows a starch to ethanol production process, wherein pipes, hoses, or other conventional industrial equipment can be used to facilitate the fluid communication of the elements and streams discussed below.
  • the production process begins when the grain, such as whole kernel corn, is subject to a dry milling phase.
  • the dry milling step is used to grind the grain into meal or powder.
  • corn is the whole grain shown in FIG. 1, any suitable grain for producing alcohol can be used.
  • grains can include corn, rye, sorghum, wheat, beans, barley, oats, rice, or combinations thereof.
  • the term "grain" can comprise a whole grain or portions or particles of a whole grain such as the product from a dry-milling process used in an alcohol production process.
  • the grain-based material is mixed with water and enzyme in a slurry mixer to form a pre-gelatinized grain-based liquid medium, which can be in the form of a slurry.
  • the time in which the grain-based material, water, and enzyme are mixed together is preferably in the range of 15 to 60 minutes, for example at least 15, 20, 30, 40, 50 or 60 minutes.
  • the temperature at which the mixing will take place is preferably in the range of 130 to 190° F, for example at least 130, 137, 140, 150, 160, 170, 180, 185 or 190° F.
  • the enzyme added to the pre-gelatinized grain-based liquid medium can be, but is not limited to, alpha-amylase, glucanase, beta-glucosidases, pectinases, xylanase, amylases, lignainases, proteases, beta-mannosidase, and similar enzymes, or a mixture thereof.
  • Enzyme or a mixture of enzymes can be added at a concentration of 0.015 to 0.5 weight percent by weight of grain, such as corn, in the pre-gelatinized grain-based liquid medium, for example enzyme can be added at a concentration of at least 0.015, 0.016, 0.2, 0.28, 0.3, 0.4 or 0.5.
  • the enzyme can be alpha-amylase and can be present in the grain-based liquid medium in the range of 0.16 to 0.40 weight percent by weight of corn grain in the pre-gelatinized grain-based liquid medium.
  • the grain-based material in the pre-gelatinized grain-based liquid medium can be present at a concentration of 20 to 50 weight percent by weight of the pre-gelatinized grain-based liquid medium, for example, less than 50, 45, 40, 35, 30 or 25 weight percent.
  • the grain-based material is present at less than 35 weight percent.
  • the pre-gelatinized grain-based liquid medium is sent through a cavitation device or apparatus that is used to apply a specified cavitation activation energy to the liquid medium sufficient to activate the enzymes and enhance their activity within the pre-gelatinized grain-based liquid medium.
  • enzyme can be added to form the pre-gelantinized grain-based liquid medium without the need for additional enzyme, such as enzyme addition upstream of the process prior to formation of the pre- gelatinized grain-based medium.
  • a one-time addition of enzyme to a grain-based material prior to applying cavitation activation energy, such as through a cavitation device reduces the need for multiple enzyme additions upstream of liquefaction and increases processing efficiency.
  • enzyme is slurried and mixed with water and grain-based material for less than one hour prior to cavitation.
  • Multiple processing steps prior to cavitation may not be needed, such as long periods of steeping with enzymes, grinding steps, etc.
  • the process therefore can consist of forming mixing a grain-based material, preferably finely ground, with water and enzyme for a period of less than one hour to form a pre-gelatinized grain-based liquid medium prior to application of cavitation activation energy as discussed below.
  • the cavitation activation energy should be applied at least at a level of about 0.4 kJ per kilogram of grain-based or pre-gelantinized grain-based liquid medium.
  • the cavitation activation energy is 0.4 to 1.6 kJ per kilogram of grain-based or pre-gelantinized grain-based liquid medium, for example at least 0.6, 0.8, 1, 1.2 or 1.4 kJ per kilogram.
  • the temperature of the stream of grain-based liquid medium entering the cavitation device can be in the range of 130 to 190° F, for example at least 140, 150, 160, 170 or 180° F.
  • the product exiting the cavitation device can be passed through the cavitation device only one time, or optionally recirculated back through the same cavitation device as many times as desired.
  • the pre-gelatinized liquid medium stream passes through the cavitation device it will then move on to the liquidation and cooling phase, as shown in FIG. 1, wherein the enzymes continue to break down the starch polymers of the liquid medium into shorter sections and create a sugar mash.
  • the mash will be transferred to fermentation containers or tanks wherein yeast will convert the sugars into carbon dioxide and alcohol, such as ethanol.
  • yeast Upon transfer of the sugar mash to the fermentation containers, additional enzyme, urea, and yeast can be added to the sugar mash.
  • the mixture is then left to ferment for a period of time, for example at least 60 hours.
  • the product resulting from the fermentation process is referred to as "beer" and contains alcohol and solids.
  • a distillation phase following the fermentation phase separates the liquid carrier, usually water, ethanol, and whole stillage from each other.
  • the water can be recycled and used, for example, in the slurry tanks.
  • the non-fermentable compounds are further separated in the distillation process, and can also be sold as high- protein animal feed.
  • cavitation can be described as the generation, subsequent growth and collapse of cavitation bubbles and cavities.
  • the bubbles contain mostly steam, although the level of steam fluctuates depending on the temperature at which the bubbles are formed. For instance, cavitation bubbles formed at lower temperatures contain less steam. Cavitation bubbles containing less steam collapse more energetically and generate higher local temperatures and pressures.
  • STP standard temperature and pressure
  • FIG. 2 illustrates a controlled flow cavitation device.
  • FIG. 2 provides a cross section view of a controlled flow cavitation apparatus 10 which can process a grain-based liquid medium, such as a pre-gelatinized grain-based medium.
  • the controlled flow cavitation apparatus 10 comprises a flow-through channel 1 comprising a first chamber 4 and a second chamber 5.
  • the first chamber 4 and second chamber 5 of the flow- through channel 1 are divided by a localized flow constriction 2.
  • the first chamber 4 is positioned upstream of the localized flow constriction 2 and the second chamber 5 is positioned downstream of the localized flow constriction 2, as viewed in the direction of movement of flow, such as a grain-based liquid medium.
  • Second chamber 5 houses the hydrodynamic cavitation zone as discussed below.
  • the hydrodynamic cavitation zone in the second chamber 5 has volume V c .
  • the first chamber 4 has static pressure Pi and the second chamber 5 encompassing the hydrodynamic cavitation zone has static pressure P 2 .
  • Localized flow constriction can be achieved by a diaphragm with one, or more, orifices 3.
  • the controlled flow cavitation apparatus 10 comprises one cylindrical orifice 3.
  • the orifice 3 of the apparatus 10 can be any shape, for example, cylindrical, conical, oval, right-angled, square, etc. Depending on the shape of the orifice 3, this determines the shape of the cavitation jets flowing from the localized flow constriction 2.
  • the orifice 3 can have any diameter, D 2 , for example, the diameter can be greater thatn 0.1, 1, 2, 3, 5, or 10 mm, and preferably more than 3 mm. In one example, the orifice 3 diameter can be about 3 mm or about 4 mm.
  • the first chamber 4 has a pressure Pi and the second chamber 5 has a pressure P 2 .
  • Flow into the apparatus 10 can be provided with the aid of fluid pumping devices as known in the art, such as a pump, centrifugal pump, positive-displacement pump or diaphragm pump.
  • An auxiliary pump can provide flow under a static pressure Pi to the first chamber 4.
  • pressure Pi is defined as the processing pressure for the controlled flow cavitation apparatus 10.
  • the processing pressure is preferably at least 30, 40, 50, 60, 70, 80, 90, 100, 120, 140, 150, 170, 200, 300, 400, 500, 600, 700, 800, 850, 900, or 1000, psi.
  • the processing pressure is reduced as the grain-based liquid medium or pre- gelantinized grain-based liquid medium passes through the flow-through channel 1 and orifice 3. Maintaining a pressure differential across the orifice 3 allows control of the cavitation intensity in the flow through channel 1.
  • the pressure differential across the orifice 3 is preferably at least 30, 40, 50, 60, 70, 80, 90, 100, 120, 140, 150, 170, 200, 300, 400, 500, 600, 700, 800, 850, 900, or 1000, psi.
  • the velocity of the grain-based liquid medium or pre- gelantinized grain-based liquid medium through the orifice 3 in the controlled flow cavitation apparatus is preferably at least 1, 5, 10, 15, 20, 25, 30, 40, 50, 60 or 70 meters per second (m/s).
  • the controlled flow cavitation apparatus 10 described herein can be used as a single-pass process for enhancing the activity of the enzyme in the pre-gelantinized grain-based liquid medium.
  • Hydrodynamic cavitation arises in the fluid jets flowing from the orifice 3 in the form of intermingling cavitation bubbles and separate cavitation cavities. That is, the orifice 3 creates a hydrodynamic cavitation zone that promotes a high density of cavitation power dissipation locally inside the flow-through channel 1, and more preferably in the orifice 3 chamber and downstream of the orifice 3 in the second chamber 5.
  • the high energy dissipation in the hydrodynamic cavitation zone causes a cavitation activation energy for promoting the activity of the enzymes in the pre- gelatinized grain-based liquid medium for increasing ethanol yield.
  • the given dynamic pressure and residence time of the bubble or steam bubble in the localized flow constriction 2 allows production of cavitation bubbles and cavities in the liquid flow.
  • the cavity sizes are dependent on the magnitude of the dynamic pressure jet as well as the sizes of orifice 3 in the localized flow constriction 2.
  • Increase of the dynamic pressure jet as well as size of orifice 3 leads to the increase in the sizes of cavitation bubbles.
  • Increase of the dynamic pressure of the cavitation fluid jet also promotes increase of the concentration of cavitation bubbles. Therefore, given the dynamic pressure of the cavitation fluid jet, its shape, and the number of fluid jets, it is possible to produce a cavitation field or zone of cavitation bubbles in the downstream second chamber 5.
  • the energy emitted during collapse of cavitation bubbles is directly proportional to the magnitude of the static pressure in the surrounding liquid bubbles. Therefore, the greater the magnitude of P 2 the greater the energy emitted during collapse of cavitation bubbles and the better the dispersion and/or size reduction effect.
  • the level of energy dissipation in the grain-based fluid medium increases as the magnitude of P 2 increases and thus the severity or hardness of collapse of each cavitation bubble separately increases, as well as the level of energy dissipation due to the decrease of the volume in which these bubbles collapse.
  • cavitation generates a specific cavitation activation energy for promoting the activity of the enzymes.
  • the specified range of cavitation activation energies preferably create hydrodynamic steam cavitation bubbles that collapse less energetically to avoid enzyme denaturation and deleterious effect on a reactions in the alcohol production process. Because cavitation bubbles containing less steam collapse more energetically and generate higher local temperatures and pressures, which can be undesirable, the specified cavitation activation energy, processing temperature and pre-gelatinized grain-based liquid medium make up are believed to create steam-filled hydrodynamic cavitation bubbles that avoid these disadvantages.
  • the length (1) in orifice 3 in localized flow constriction 2 is selected in such a manner in order that the residence time of the cavitation bubble, for example a hydrodynamic steam cavitation bubble, in the orifice 3 and/or the second chamber 5 is less than 10 seconds, preferably less than 1 second or preferably less than 0.1 second.
  • the time in the hydrodynamic cavitation zone that is needed to enhance and promote the enzyme activity is much smaller than know methods, such as ultrasonic or acoustic, and thus the controlled flow cavitation apparatus can reduce processing time and costs associated with an alcohol production process.
  • hydrodynamic cavitation is more efficient than acoustic cavitation and much more efficient than conventional agitation and/or heating methods. Further, the scale-up of hydrodynamic cavitation apparatuses is relatively easy compared to other methods, which makes it well suited to the processing of dispersions and slurries, such as those present in an alcohol production process.
  • FIG. 3 provides a cross section view of a cavitation device 20.
  • a bluff body 23 is positioned in the flow-through channel 21 to create a localized flow constrictions 22, wherein two localized flow restrictions are created in parallel to one another, each localized flow restriction positioned between the flow-through channel 21 and the top or bottom of the bluff body 23.
  • the localized flow constrictions such as the bottom localized flow constriction 22, divide the flow-through channel 21 into two chambers, a first chamber 24 having static pressure Pi and a second cavitation chamber 25 having static pressure P 2 .
  • Second chamber 25 houses the hydrodynamic cavitation zone as discussed below.
  • the hydrodynamic cavitation zone in the second chamber 25 has volume V c .
  • liquid such a the pre- gelatinized grain-based liquid medium
  • the specified range of cavitation activation energies preferably create hydrodynamic steam cavitation bubbles that collapse less energetically to avoid enzyme denaturation and deleterious effect on a reactions in the alcohol production process and thereby enhance the activity in the pre-gelatinized grain-based liquid medium.
  • the cavitation activation energy through any of the cavitation devices of Figures 2-3 can be calculated from the following equation: _ ( 1 - 2) . g . t
  • ⁇ (kJ/kg) cavitational energy
  • PI (Pa) is the static pressure in the first chamber
  • P2 (Pa) is the static pressure in the second cavitation chamber
  • Q (m 3 /sec) is the flow rate of the liquid medium through the cavitation apparatus
  • t (sec) is the residence time in the hydrodynamic cavitation zone
  • Vc (m 3 ) is the volume of the downstream cavitation zone
  • p (kg/m 3 ) is the density of the pre-gelantinized grain-based liquid medium.
  • Examples of static cavitational energy sources that can be used to apply cavitational energy to the pre-gelatinized grain-based liquid medium include, but are not limited to, static mixers, orifice plates, perforated plates, nozzles, Venturis, jet mixers, eductors, cyclonettes (e.g., Fluid- Quip, Inc.), and control flow cavitation devices (e.g., Arisdyne systems, Inc), such as those described in U.S. Pat. Nos. 5,810,052; 5,931,771; 5,937,906; 5,971,601; 6,012,492; 6,502,979; 6,802,639; 6,857,774 and 7,667,082.
  • static mixers orifice plates, perforated plates, nozzles, Venturis, jet mixers, eductors, cyclonettes (e.g., Fluid- Quip, Inc.), and control flow cavitation devices (e.g., Arisdyne systems,
  • dynamic cavitational energy sources that can be used include, but are not limited to, rotary milling devices (e.g., EdeniQ CellunatorTM), rotary mixers (e.g.,
  • rotor-rotor e.g., Eco-Fusion Canada Inc.
  • rotor- stator devices e.g., IKA® Works, Inc., Charles Ross & Son Company, Silverson Machines, Inc., Kinematica Inc.
  • Achieving increased alcohol yield within a particular type of cavitation process is dependent on many factors, including the location of the process at which the cavitation is applied, intensity of the cavitation, duration of time spent in hydrodynamic cavitation zone, pressure maintained in cavitation chamber, temperature, amount of enzyme, and others process variables.
  • Corn flour was fed into a slurry mixer where it was mixed with hot process water.
  • Total dry solids concentration was of 30.9% (w/w). Residence times in the slurry mixer were 30 minutes. A dose of a-amylase was included in the mixture that was supplied to the slurry mixer (0.016% w/w enzyme based on the weight of corn flour in the slurry) such that a pre- gelatinized grain-based liquid medium was formed. The temperature, level and pH of the slurry were continuously measured using online instrumentation. Next, the pre-gelatinized grain-based liquid medium was passed from the slurry mixer to a cavitation device as illustrated in FIG. 2.
  • the pre-gelatinized grain-based liquid medium was treated by cavitation at one of two temperatures (137°F and 170°F) and one of four cavitation activation energies (0.00, 0.44, 0.94, and 1.56 kJ per kilogram of the pre-gelatinized grain-based liquid medium), as shown in Table 1.
  • the pre-gelatinized grain-based liquid medium was passed through the cavitation device one time as a single -pass operation.
  • the cavitation device had an orifice of 5 mm. Flowrates of the pre-gelatinized grain-based liquid medium ranged from 10 to 18 gpm. Pressure in the first chamber was 100, 200 and 300 psi and static pressure in the second chamber was at least 50 psi. Duration of the pre-gelatinized grain-based liquid medium in the hydrodynamic cavitation zone was less than 0.1 second.
  • the flasks were left to incubate for 1 hour at 180°F. Subsequently, the flasks were transferred to an incubator shaker to facilitate the cooling of the samples, wherein the temperature was held to 68°F and the flasks were shaken at 150 rpm. After all of the samples were liquefied and cooled, glucoamylase, urea, and yeast nutrients were added to the flasks. The samples were then left to ferment for at least 60 hours.

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Abstract

La présente invention concerne un procédé permettant d'augmenter la quantité d'éthanol produite à partir de céréales. Ledit procédé comprend une étape consistant à mélanger des céréales, de l'eau et une enzyme afin d'obtenir un milieu liquide à base de céréales. On fait passer ledit milieu liquide à base de céréales à travers un dispositif de cavitation à une vitesse et sous une pression capables de générer une énergie d'activation de la cavitation au moins égale à 0,4 kJ par kilogramme de milieu liquide à base de céréales afin de favoriser l'activité de l'enzyme et d'augmenter la production d'éthanol.
PCT/US2010/059164 2009-12-09 2010-12-07 Procédé permettant d'augmenter la quantité d'éthanol produite à partir de céréales Ceased WO2011071842A2 (fr)

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CA2764909A CA2764909C (fr) 2009-12-09 2010-12-07 Procede permettant d'augmenter la quantite d'ethanol produite a partir de cereales

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US26790009P 2009-12-09 2009-12-09
US61/267,900 2009-12-09

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