巴西专利BR112013018400B1 method for treating lignocellulosic biomass

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SYSTEMS AND METHODS FOR HYDROLYSIS OF BIOMASS These are systems and methods that are presented for the treatment of lignocellulosic biomass to be supplied to a fermentation system for the production of a fermentation product. The systems and methods comprise pre-treating the biomass into the pre-treated biomass and separating the pre-treated biomass into a liquid component comprising sugar components and solids comprising cellulose and lignin. The systems and methods also comprise treating the solids component of the pretreated biomass into a treated component. Biomass comprises lignocellulosic material. Treatment of the solids component comprises applying an enzyme formulation and make-up water to form a slurry. The enzyme formulation comprises a cellulase enzyme. The make-up water includes a fine clarified stillage composition and/or an anaerobic membrane digester effluent composition.
公开号:BR112013018400B1
申请号:R112013018400-0
申请日:2012-01-18
公开日:2021-05-18
发明作者:Neelakantam V. Narendranath；William F. Mcdonald；Jason Alan Bootsma
申请人:Poet Research Incorporated；
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Cross Reference to Related Orders
[001] This application claims the benefit of US provisional application serial number 61/433,864 filed on January 18, 2011 and entitled "SYSTEMS AND METHODS FOR HYDROLYSIS OF BIOMASS", the description of which is incorporated herein by reference . This application incorporates, by reference, the following applications: US patent serial number 12/716,984 entitled "SYSTEM FOR PRE-TREATMENT OF BIOMASS FOR THE PRODUCTION OF ETHANOL", and US patent serial number 61/ 345,486 entitled "SYSTEM FOR HYDROLYSIS OF BIOMASS TO FACILITATE THE PRODUCTION OF ETHANOL" deposited on May 17, 2010. Field
[002] This invention relates to the treatment of biomass in the production of ethanol. The subject of the invention also concerns the treatment of pretreated biomass before the pretreated biomass is supplied to a fermentation system in order to facilitate the efficient production of ethanol. Fundamentals of the Invention
[003] Ethanol can be produced from grain-based raw materials (for example, corn, sorghum/milk, barley, wheat, soy, etc.), from sugar (for example, from sugarcane sugar, beetroot, etc.) and from biomass (eg from cellulosic raw materials such as switchgrass, corn cobs and straw, wood or other plant material).
[004] Biomass comprises vegetable matter that may be suitable for direct use as a fuel/energy source or as a raw material for processing into another bioproduct (for example, a biofuel, such as cellulosic ethanol) produced in a biorefinery (like an ethanol plant). Biomass can comprise, for example, corn cobs and straw (eg, stalks and leaves) available during or after harvesting corn grain, corn seed fiber, grasses, farm or agricultural waste, wood shavings or other wood residues and other vegetable materials. In order to be used or processed, the biomass will be harvested and collected in the field and transported to the location where it will be used or processed.
[005] In a biorefinery configured to produce ethanol from biomass, such as cellulosic feedstocks as indicated above, ethanol is produced from lignocellulosic material (eg, cellulose and/or hemicellulose). Biomass is prepared so that sugars in cellulosic material (such as glucose from cellulose and xylose from hemicellulose) can be accessed and fermented into a fermentation product that comprises ethanol (among other things). The fermentation product is then sent to the distillation system, where ethanol is recovered by distillation and dehydration. Other bioproducts such as lignin and organic acids can also be recovered as co-products. Determining how to most efficiently prepare and treat biomass for ethanol production will depend (among other things) on the form and type or composition of the biomass.
[006] One of the costly steps in the preparation of lignocellulosic materials for fermentation is the hydrolysis of the cellulosic material, which requires the use of enzymes in order to degrade the cellulose into sugars. Typically, large doses of enzymes are required for hydrolysis, as it is believed that lignin can bind to some of the enzymes, rendering them inactive. Since enzymes are a significant part of the overall cost of hydrolysis, there is a lack of efficiency in conventional techniques that have not been addressed. summary
[007] One aspect relates to a method for treating lignocellulosic biomass to be supplied to a fermentation system for the production of a fermentation product. The method comprises pre-treating the biomass into the pre-treated biomass and separating the pre-treated biomass into a liquid component comprising sugar components and solids comprising cellulose and lignin. The method also comprises treating the solids component of the pretreated biomass into a treated component. Biomass comprises lignocellulosic material. Treatment of the solids component comprises applying an enzyme formulation and an agent to form a slurry. The enzyme formulation comprises a cellulase enzyme. The agent may include thin, clear vinasse or effluent from an anaerobic membrane digester in some embodiments.
[008] According to a modality, treating the solids component releases the sugar. According to another modality, the pre-treatment of biomass comprises steeping, wherein the steeping comprises mixing the biomass and applying sulfuric acid to the biomass. Description of Drawings
[009] In order that the described aspects can be more clearly determined, some modalities will now be described, by way of example, with reference to the attached drawings, in which: Figure 1A is a perspective view of a biorefinery comprising a installation of ethanol production, according to some modalities; Figure 1B is another perspective view of a biorefinery comprising an ethanol production facility, according to some embodiments; Figure 2 is a system for the preparation of biomass released to a biorefinery, according to some modalities; Figures 3A and 3B are alternative embodiments of a schematic diagram of the cellulosic ethanol production facility, according to some embodiments; Figure 4A is a process flow diagram illustrating the pretreatment process, according to some embodiments; Figure 4B is a schematic perspective view of the pre-treatment process, according to some embodiments; Figure 5 is a process flow diagram illustrating the process for the hydrolysis of C6 biomass solids, according to some embodiments; Figures 6A to 6D are diagrams of operating conditions for hydrolysis of biomass according to an exemplary embodiment; Figure 7 is an example graph for the percentage of theoretical ethanol generated from biomass under various treatment processes, according to some modalities; Figure 8 is a graph of the results of hydrolysis of biomass with and without a fine and clear vinasse additive, according to an exemplary embodiment; Figure 9 is a graph of the results of hydrolysis of biomass with the fine and clear vinasse additive agent, according to an exemplary embodiment; Figure 10 is a graph of residual glucose after fermentation of hydrolyzed biomass with varying levels of a fine and clear vinasse additive, according to an exemplary embodiment; Figure 11 is a graph of the results of hydrolysis of biomass with an anaerobic membrane bioreactor effluent additive agent, according to an exemplary embodiment; Figure 12 is a graph of residual glucose after fermentation of hydrolyzed biomass with varying levels of an anaerobic membrane bioreactor effluent additive agent, according to an exemplary embodiment; Figure 13 is a table of the results of hydrolysis of biomass with varying concentrations of anaerobic membrane bioreactor effluent additive and fine and clear vinasse additive, according to an exemplary embodiment; Tables 1A and 1B list the biomass composition comprising the lignocellulosic plant material of the corn plant according to the exemplary and representative modalities; tables 2A and 2B list the composition of the liquid component of pretreated biomass according to the example and representative modalities; Tables 3A and 3B list the composition of the pretreated biomass solids component according to the example and representative modalities. Description of Modalities
[0010] The various aspects will now be described in detail with reference to the various embodiments thereof, as illustrated in the accompanying drawings. In the following description, a number of specific details are demonstrated in order to provide a complete understanding of the modalities of one or more aspects. However, it will be evident to the person skilled in the art that the modalities can be practiced without some or all of these specific details. In other cases, well-known steps and/or structures of the process have not been described in order not to unnecessarily obscure the various aspects. The features and advantages of the modalities can be better understood with reference to the following drawings and discussions.
[0011] The aspects refer to systems and methods for the enzymatic hydrolysis of the solid portion of the lignocellulosic hydrolyzate, with the addition of an agent, in order to reduce the load requirements and increase the enzyme efficiency. The various aspects presented here provide for the treatment of biomass in ethanol production. Aspects also provide the enhancement of cellulose hydrolysis efficiencies. The systems and methods of the aspects presented here provide a low-cost means to increase the efficiency of converting cellulosic materials to fermentable sugars.
[0012] Referring to Figure 1A, an example biorefinery 100 comprising an ethanol production facility configured to produce ethanol from biomass is shown. The example biorefinery 100 comprises an area where biomass is released and prepared to be supplied to the ethanol production facility. The cellulosic ethanol production facility comprises apparatus for preparing 102, pre-treatment 104 and treating biomass into treated biomass suitable for fermentation into the fermentation product in a fermentation system 106. The cellulosic ethanol production facility comprises a distillation system 108 in which the fermentation product is distilled and dehydrated to ethanol. As shown in Figure 1A, a waste treatment system 110 (shown comprising an anaerobic digester and a generator) may be included in the biorefinery 100. According to alternative embodiments, the waste treatment system may comprise other equipment configured to treat, process and recover components of the cellulosic ethanol production process, such as a solid/waste fuel boiler, anaerobic digester, aerobic digester or other biochemical or chemical reactors.
[0013] As shown in Figure 1B, according to an exemplary embodiment, a biorefinery 112 may comprise a cellulosic ethanol production facility 114 (which produces ethanol from lignocellulosic material and corn plant components) colocalized with a corn-based ethanol production facility 116 (which produces ethanol from the starch contained in the endosperm component of the corn core). As indicated in Figure 1B, by co-locating the two ethanol production units, some plant systems can be shared, for example, the ethanol dehydration, storage, denaturation and transport systems, the energy generation systems / fuel into energy, plant management and control systems, and other systems. Corn fiber (a component of the corn core), which can be made available when the corn core is prepared for milling (eg, by fractionation) at the corn-based ethanol production facility, can be supplied to the facility. production of cellulosic ethanol as a raw material. Fuel or energy sources such as methane or lignin from the cellulosic ethanol production facility can be used to supply energy to one or both of the co-located facilities. Under other alternative modalities, a biorefinery (for example, a cellulosic ethanol production facility) may be co-located with other types of plants and facilities, for example, an electric power plant, a waste treatment facility, a sawmill , a paper mill, or a facility that processes agricultural products.
[0014] Referring to Figure 2, a system 200 for the Preparation of Biorefinery Released Biomass is shown. The biomass preparation system may comprise an apparatus for receiving/discharging biomass, for cleaning (e.g., removal of foreign bodies), for crushing (e.g., milling, reduction or compression) and for transport and conveyance. for plant processing. According to an exemplary modality, biomass in the form of corn cobs and straw can be released to the biorefinery and stored 202 (eg, in packages, piles or boxes, etc.) and managed for use at the facility. According to an exemplary embodiment, the biomass can comprise at least about 20 to 30 percent corn cobs (by weight) with corn husks and other materials. According to other exemplary embodiments, the biorefinery preparation system 204 can be configured to prepare any of a wide variety of types of biomass (e.g., plant material) for treatment and processing into ethanol and other bioproducts. at the plant.
[0015] With reference to Figures 3A and 3B, alternative embodiments of a schematic diagram of the cellulosic ethanol production facility 300a and 300b are shown. According to some modalities, the biomass comprising the material of plant origin from the corn plant is prepared and cleaned in a preparation system. After Preparation, the biomass is mixed with water in a slurry and is pretreated in a 302 pretreatment system. In the 302 pretreatment system, the biomass is decomposed (eg by hydrolysis) to facilitate separation 304 into a liquid component (eg a stream comprising C5 sugars known as pentose liquor) and a solids component (eg a stream comprising cellulose from which C6 sugars can be made available). The liquid component containing the C5 sugar (C5 flux or pentose liquor) can be treated in a 306 pentose cleaning treatment system. Similarly, the pretreated solids component containing the C6 sugar can be treated in a solids treatment system using 308 enzyme hydrolysis to generate the sugars. Under one modality, hydrolysis (such as enzyme hydrolysis) can be performed to access the C6 sugars in cellulose; treatment can also be carried out in an attempt to remove lignin and other non-fermentable components in the C6 stream (or to remove components such as acid or residual acids that may be inhibitory to efficient fermentation). The efficiency of enzymatic hydrolysis can be increased by adding an agent. Such agents may include anaerobic membrane digester effluent, thin and clear stillage, wet cake, whole stillage or other viable protein source, or combinations thereof. Details of the treatment of C6 solids will be described in detail below.
[0016] According to the modalities of Figure 3A, the treated pentose liquor then can be fermented in a 310 pentose fermentation system, and the fermentation product can be fed to a 314 pentose distillation system for the recovery of ethanol. Similarly, treated solids, which do not include substantial amounts of C6 sugars, can be fed to a 312 hexose fermentation system, and the fermentation product can be fed to a 316 hexose distillation system for the recovery of ethanol. The stillage from the distillation can then be treated in a 322 lignin separation system to generate a liquid component and a solid wet cake. The wet cake can then be fed to a 324 Anaerobic Membrane Bioreactor (AnMBR) for further treatment. In some embodiments, effluent from anaerobic membrane bioreactor 324 can be recycled to enzyme hydrolysis tank 308 as an additive agent.
[0017] In the alternative embodiment of Figure 3B, the resulting treated pentose liquor and treated solids can be combined after treatment (eg, as a slurry) for co-fermentation in a 318 fermentation system. fermentation system 318 is supplied to a combined distillation system 320 where ethanol is recovered. According to either modality, a suitable fermentation organism (ethanol production) can be used in the fermentation system. According to some aspects, the selection of an ethanol production can be based on several considerations such as the predominant types of sugars present in the slurry. The dehydration and/or denaturation of ethanol produced from the C5 stream and the C6 stream can be carried out either separately or in combination. As with previously described modalities, stillage from the distillation can be treated in a lignin 322 separation system to generate a liquid component and a solid wet cake. The wet cake can be supplied to a 324 Anaerobic Membrane Bioreactor (AnMBR) for further treatment. In some embodiments, effluent from anaerobic membrane bioreactor 324 can be recycled to enzyme hydrolysis tank 308 as an additive agent.
[0018] During the treatment of the C5 and/or C6 flux, the components can be processed to recover the by-products, such as organic acids and lignin. Components removed during the treatment and production of ethanol from biomass from one or both the C5 stream and the C6 stream (or in distillation) can be treated or processed into bioproducts or fuel (such as lignin for a boiler solid fuel or methane produced by treating waste/removed matter such as acids and lignin in an anaerobic digester) or recovered for utilization or reuse.
[0019] According to one embodiment, the biomass comprises the material of vegetable origin of the corn plant, such as corn cobs, corn plant husks and corn plant leaves and corn stalks (for example, at least the upper half or three quarters of the stem). In some respects, the composition of the material of plant origin (eg, cellulose, hemicellulose and lignin) will be approximately as indicated in Tables 1A and IB (eg, after at least the initial biomass preparation, including the removal of any extraneous matter). According to one modality, the material of vegetal origin comprises corn cobs, husks/leaves and stalks. For example, the plant material may comprise (by weight) up to 100 percent ears, up to 100 percent bark/leaves, approximately 50 percent ears, and approximately 50 percent bark/leaves, approximately 30 percent cobs and approximately 50 percent husks/leaves and approximately 20 percent stalks, or any of a wide variety of other combinations of corn plant ears, husks/leaves and stalks. See Table 1A. According to an alternative embodiment, the lignocellulosic plant material may comprise corn core fiber (eg, in some combination with another plant material). Table 1B provides several ranges believed to be representative of the biomass composition comprising the corn plant lignocellulosic material. According to the exemplary embodiments, the lignocellulosic plant material from a biomass (from the corn plant) may comprise (by weight) cellulose by about 30 to 55 percent, hemicellulose by about 20 to 50 percent and lignin by about 10 to 25 percent. According to another exemplary embodiment, the lignocellulosic plant material from the biomass (e.g. ears, husks/leaves and stalk parts of the maize plant) may comprise (by weight) cellulose in about 35 to 45 per percent, hemicellulose about 24 to 42 percent, and lignin about 12 to 20 percent. According to a specific embodiment, the biomass pretreatment can yield a liquid component comprising (by weight) xylose in no less than about 1.0 percent and a solids component comprising (by weight) cellulose (a from which glucose can be made available) by no less than about 45 percent.
[0020] Figures 4A and 4B show the apparatus 400, 450 that can be used for the preparation, pre-treatment and separation of lignocellulosic biomass according to an exemplary modality; As shown, the biomass is prepared on a 402 grinder (eg, a grinder or other suitable apparatus or milling machine). Pre-treatment of the prepared biomass is carried out in a 404 reaction vessel (or a set of 454 reaction vessels) supplied with the prepared biomass and the acid/water, at a predetermined concentration (or pH) and under other operating conditions . The pretreated biomass can be separated in a 406 separator. As shown in Figure 4B, the pretreated biomass can be separated in a 456 centrifuge into a liquid component (C5 stream which mainly comprises liquids with some solids) and a component of solids (C6 stream comprising liquids and solids such as lignin and cellulose from which glucose can be made available for further treatment).
[0021] According to one modality, the pre-treatment of biomass can be carried out as described in US patent serial number 12/716,984 entitled "SYSTEM FOR PRE-TREATMENT OF BIOMASS FOR THE PRODUCTION OF ETHANOL", which is incorporated herein for reference in its entirety.
[0022] According to one modality, in the pretreatment system an acid can be applied to the prepared biomass to facilitate the breakdown of the biomass for separation into the liquid component (pentose liquor) (C5 flow from which the fermentable C5 sugars can be recovered) and the solids component (C6 stream from which fermentable C6 sugars can be accessed). Under some embodiments, acid can be applied to biomass in a reaction vessel under certain operating conditions (eg acid concentration, pH, temperature, time, pressure, solids charge, flow rate, the process water or steam supply, etc.) and the biomass can be stirred/mixed in the reaction vessel to facilitate the breakdown of the biomass. According to the exemplary embodiments, an acid such as sulfuric acid, hydrochloric acid, nitric acid, phosphoric acid, acetic acid, etc. (or an acid formulation/mixture) can be applied to the biomass. According to a specific modality, sulfuric acid can be applied to the biomass in the pre-treatment. According to a specific modality, the prepared biomass can be pretreated with approximately 0.8 to 1.5 percent acid (such as sulfuric acid) and about 12 to 25 percent biomass solids at a temperature from approximately 100 to 180 degrees Celsius for approximately 5 to 180 minutes. The pre-treatment may also comprise a steam explosion step, where the biomass is heated and held (eg hold time) for approximately 150 to 165 degrees Celsius under pressure (eg 100 psi) at a pH of about from 1.4 to 1.6 for one to 15 minutes, and the pressure is relieved to further aid in pulp rupture. After pretreatment, the pretreated biomass is separated into a solids component (C6) and a liquid pentose liquor component (C5), as shown in figures 4A and 4B.
[0023] The liquid component of pentose liquor (C5 stream) comprises water, dissolved sugars (such as xylose, arabinose and glucose) made available for fermentation into ethanol, acids and other soluble components recovered from hemicellulose. (Table 2B provides typical and expected ranges believed to be representative of the biomass composition comprising the corn plant lignocellulosic material.) According to an exemplary modality, the liquid component may comprise approximately 5 to 7 percent solids ( eg suspended solids/residuals such as partially hydrolyzed hemicellulose, cellulose and lignin). According to a specific embodiment, the liquid component can comprise at least 2 to 4 percent xylose (by weight). According to other exemplary embodiments, the liquid component can comprise no less than 1 to 2 percent xylose (by weight). Tables 2A and 2B list the composition of the liquid component of pretreated biomass (from the biomass prepared as indicated in tables 1A and 1B) according to the example and representative modalities.
[0024] The solids component (C6 flux) comprises water, acids, and solids such as cellulose from which sugar, such as glucose, can be made available for fermentation to ethanol and lignin. (Table 3B provides ranges that may be representative of the biomass composition comprising the corn plant lignocellulosic material.) According to an exemplary embodiment, the solids component may comprise approximately 10 to 40 percent solids (in weight) (after separation).
[0025] According to a specific embodiment, the solids component may comprise approximately 20 to 30 percent solids (by weight). In another embodiment, the solids in the solids component can comprise no less than 30 percent cellulose and the solids component can also comprise other dissolved sugars (e.g., glucose and xylose). Tables 3A and 3B list the composition of the solids component of the pretreated biomass (from the biomass prepared as indicated in Tables 1A and 1B) according to the example and representative modalities.
[0026] Referring to figure 5, after the separation of the liquid component of C5 from the solids of C6, the solids can still be treated in an enzymatic hydrolysis system 500. According to a modality, after the pre-treatment, the solids component (C6) is supplied to a vessel 502 for enzymatic hydrolysis (or saccharification) along with enzymes, agents and water. Enzymes can facilitate the breakdown of pretreated cellulose into sugar (eg glucose) to generate an enzymatic hydrolysis product. The sugar-rich enzymatic hydrolysis product can then be fermented to ethanol, or used for any other downstream process.
[0027] In some embodiments, the C6 solids can be subjected to a sequential hydrolysis and fermentation (SHF), in which the solids are subjected to an enzymatic hydrolysis (with a glucan conversion of at least 80%) followed by a fermentation. Although it requires a two-step process, with the SHF approach, enzymatic hydrolysis can be carried out at an ideal pH and temperature for converting cellulose to sugars. Typically, for SHF, solids are treated at about 50 degrees Celsius, pH 5.5 and 15% total solids slurry with cellulase.
[0028] Alternatively, the C6 solids can be subjected to a simultaneous saccharification and fermentation (SSF) process in which enzymatic hydrolysis and fermentation are carried out at about the same time. Simultaneous saccharification and fermentation can be carried out at temperatures suitable for the yeast's production of ethanol (eg around 37°C) which may be less than ideal for the cellulase enzyme. Thus, enzyme efficiency can be reduced. For both SSF and SHF, the binding of cellulase enzymes to lignin can be a specific problem where, depending on the raw material used, lignin can be dispersed into the solids after pretreatment with dilute acid, as discussed above. This can be particularly problematic when corn husk biomass is used as a feedstock.
[0029] According to an example embodiment, an enzyme formulation comprising an enzyme capable of hydrolyzing cellulose is provided to the solids component (C6) to facilitate enzymatic hydrolysis, for example, saccharification through the enzymatic action of cellulose polymeric (eg, polymeric glucan) to accessible monomeric sugars (eg, monomeric glucose). An example of such a cellulase enzyme is Cellic CTEC (eg, NS22074) from Novozymes North America, Inc. of Franklinton, North Carolina. The amount or loading (dose) of enzyme formulation may vary as an operating condition. According to an exemplary embodiment, approximately 2 to 12 milligrams of enzyme protein per gram of cellulose can be added. According to a specific modality, approximately 3 to 9 milligrams of enzyme protein per gram of cellulose can be added. According to some aspects, the addition of agents to enhance enzyme efficiencies is used for the enzymatic hydrolysis of cellulose-containing materials. Since enzymes are responsible for a large portion of the costs associated with the hydrolysis of cellulose materials, reducing the required enzyme load or achieving cellulose conversion efficiency can be beneficial in the marketplace.
[0030] As such, the modalities described herein are directed to adding agents to the reaction vessel 502 in order to improve the efficiency and yield of the enzymatic hydrolysis of pretreated cellulose. Pretreated solids include lignin and other materials that can bind proteins. When enzymes are added to reaction vessel 502, some of these enzymes are bound by lignin and/or other particulates. This can result in less efficient, or even inactive, bound enzymes. Thus, the enzyme's efficiency of all hydrolysis decreases. In order to overcome this reduction in efficiency, traditionally a higher level of enzymes is added.
[0031] When the addition of another protein source is provided, through an agent, these proteins may compete for binding sites in the lignin material. This results in less binding of enzymes and a correlated increase in hydrolysis efficiency. Possible sources of protein-rich bioproducts in an ethanol plant include thin stillage, anaerobic membrane bioreactor (AnMBR) effluent, wet cake, whole stillage, and other bioproducts. Specific examples of agent additives to improve hydrolysis efficiency will be discussed in more detail below.
[0032] According to a first embodiment, the agent may comprise a fine vinasse composition from a conventional ethanol production facility (for example, based on corn). According to a specific modality, the agent may comprise the thin and clear vinasse from one of a conventional ethanol production facility (eg corn-based). Fine, clear stillage can be produced from fine stillage by removing substantially all of the solid particles and oil contained in the fine stillage. Thin and clear vinasse essentially comprises water and soluble thin vinasse components. According to an embodiment, the agent comprises as an active component at least a part of the soluble components comprised in the fine vinasse.
[0033] According to a second embodiment, the agent may comprise an effluent composition of the anaerobic membrane bioreactor of a cellulosic ethanol production facility (e.g., based on biomass). The lignin cake that results after distillation into biomass-based vegetable ethanol is digested in an anaerobic-type membrane bioreactor. Digestion of wet cake materials by anaerobic microorganisms substantially maintains the nutritional value of the material. The membrane separates the relatively clean effluent from solids and microorganisms. The digester effluent may have high levels of extracellular polymeric substances (EPS) which include proteins, lipids and nucleic acids.
[0034] The active protein components that are present in fine vinasse and anaerobic membrane bioreactor effluent may also be present in other fermentation products or co-products and intermediate products, such as beer, whole vinasse, wet cake, syrup , dried grains from stills (with or without solubles), any of which can be used as a component of the agent, according to a modality. According to an alternative embodiment, the agent may comprise corn germ steep liquor, which can be produced by steeping corn germ (produced, for example, in a fractionation system from corn kernels) in water or in a water-based liquid. Other agents (eg potassium hydroxide or sodium hydroxide for pH adjustment) may also be supplied to the treatment vessel.
[0035] The amount of fine vinasse, fine and clear vinasse and/or anaerobic membrane bioreactor effluent applied to the treatment of the solids component (C6) can range from about 1 to 90 percent of all the liquid present, according to an example modality. According to an embodiment, the amount of thin stillage, thin and clear stillage, or anaerobic membrane bioreactor effluent can range from about 20 to 70 percent of all liquid present.
[0036] Figures 6A to 6D show the operating conditions for the parameters for the treatment of the pretreated biomass solids component for the hydrolysis of cellulose to sugar according to an exemplary embodiment. Operating conditions are shown in the form of nested bands that comprise an acceptable operating range (the outer/wide range shown), an example operating range (the middle range shown), and a specific example operating range (the range shown). inner/narrow shown) for each condition or parameter of the subject.
[0037] According to an example embodiment, the temperature during the treatment of the solids component (C6) can be approximately 30 to 60 degrees Celsius. According to one embodiment, the temperature during treatment of the solids component (C6) can be approximately 45 to 55 degrees Celsius. According to a specific modality, the temperature during the treatment of the solids component (C6) can be approximately 49 to 51 degrees Celsius.
[0038] According to an example embodiment, the treatment time of the solids component (C6) can be approximately 48 to 144 hours. According to one modality, the treatment time of the solids component (C6) can be approximately 60 to 120 hours, and according to a specific modality, the treatment time of the solids component (C6) can be approximately 72 to 96 hours.
[0039] According to an exemplary embodiment, the solids content of the solids component (C6) supplied to the treatment system can be approximately 5 to 25 percent by weight. According to one embodiment, the solids content of the solids component (C6) can be approximately 10 to 20 percent by weight. According to a specific embodiment, the solids content of the solids component (C6) can be approximately 12 to 17 percent by weight.
[0040] According to an exemplary embodiment, the pH during the treatment of the solids component (C6) may be approximately 4.8 to 6.2. According to an embodiment, the pH during treatment of the solids component (C6) can be approximately 5.2 to 5.8. According to a specific modality, the pH during the treatment of the solids component (C6) can be approximately 5.4 to 5.6.
[0041] As illustrated in the graph in figure 7, a glucose yield that can be achieved during the enzymatic hydrolysis of biomass (eg corn cobs, husks, leaves and/or stalks) with the use of cellulase enzymes available, without the addition of thin stillage, thin clear stillage or anaerobic membrane bioreactor effluent may be in the range of about 35 to 40 percent of the theoretical (eg calculated) glucose 702 yield value for saccharification and simultaneous fermentation (SSF) 704 and between about 55 to 70 percent of the theoretical glucose yield for sequential hydrolysis and fermentation (SHF) 704. Exact glucose yields may vary depending on pretreatment procedures. For example, as illustrated in the graph, the inclusion of steam explosion pretreatment, as described above, can increase glucose conversion yields for biomass processed by SHF. According to the modalities, an increase of up to 45 to 110 percent in glucose yield during enzymatic hydrolysis can be achieved through the addition of a lignin binding agent such as fine clear vinasse and/or bioreactor effluent of anaerobic membrane (AnMBR). Examples
[0042] A series of limited examples were conducted according to an example modality of the system in an effort to assess the effect of using various agents in the treatment of the solids component (C6). Experiments and tests were conducted to evaluate the glucose yields for the hydrolysis of C6 with the addition of various agents. The following examples are intended to provide clarity to some modalities of systems and means of operation and are not intended to limit the scope of the aspects presented.
[0043] The system used for the examples comprised a temperature-controlled reaction vessel and a pressure tube. Biomass comprising about 35 percent ear, 45 percent bark and leaves and 20 percent stem was pretreated by maceration with approximately 1 to 1.3 percent acid (eg, sulfuric acid) at 140 degrees Celsius with 14.3 percent solids for 50 minutes and by steam explosion at pH 1.5, and around 154 degrees Celsius and a hold time of 4 minutes. Pretreated biomass slurry was supplied to the reaction vessels along with makeup water and enzymes to achieve 12 to 15 percent solids and was studied for the conversion of cellulose to glucose. Fermentation yields for the resulting hydrolysis product were also measured. Example 1
[0044] In the first example, the pretreated biomass was supplied to two reaction vessels with the make-up water. Make-up water in one container consisted of water, and make-up water in another container comprised 40 percent water and 60 percent thin, clear vinasse. The thin and clear vinasse was generated by centrifuging the thin vinasse (7% solids) at 5000 rpm for 20 minutes. After centrifugation, three layers are present: a solid pellet, a liquid middle layer and an oil emulsion top layer. The middle liquid layer contains 4% solids and is considered thin and clear vinasse. This layer has been removed and used for the following examples.
The pH of the slurry was adjusted to 5.5 with potassium hydroxide and about 7.2 milligrams of cellulase containing the enzyme formulation (eg, Cellic CTec2, available from Novozymes North America, Inc. from Franklinton, North Carolina, USA) per gram of cellulose was added to each container. Enzyme hydrolysis was conducted at 50 degrees Celsius. The amount of glucose in each container was measured at 0, 24, 48, 72 and 96 hours by high pressure liquid chromatography (HPLC).
[0046] It was observed that in 96 hours, the biomass glucose yield with water was only approximately 52.6% of the theoretical, and the biomass glucose yield with water and thin and clear vinasse was approximately 76.1 Percent. The use of fine and clear vinasse in the enzymatic hydrolysis of biomass resulted in an approximately 45 percent increase in yield. The results are shown in Figure 8. Example 2
[0047] In a second example, a dose-response study to determine the optimal level of use of thin and light vinasse (CTS) in saccharification was conducted at two enzyme dosages: 5.6 and 8.4 mg of cellulase that contains the enzyme formulation per gram of glucan. The Ctec2 enzyme was used. The thin and clear vinasse was used at 0 (control), 10, 20, 30, 40, 50 and 60% of the water replacement in 15% of total solids slurry. The saccharification was carried out for 96h at 50 °C, initial pH of 5.5 followed by a fermentation of 48h to 72h at 32 °C, initial pH of 5.5. The results of total glucose (w/v) 902 are plotted as a function of the concentration of thin and clear vinasse (CTS) 904 used in water replacement, as shown in the example graph in figure 9. use of thin and clear vinasse significantly improved the glucose yield in the saccharification process. Furthermore, the results of this SHF study showed only slight differences in glucose production from the addition of CTS between 20 and 60% of the total water as observed for both doses of enzymes tested. Example 3
[0048] In the third example experiment, after 96h of enzymatic hydrolysis, the reactors were cooled to 32 degrees Celsius and the pH adjusted back to up to 5.5. Urea was added at 0.06 g/L (as a nitrogen source) and Lactoside247 was added at 5 ppm. Yeast was inoculated at 0.5 g (dry)/L. Fermentations were carried out for up to 72 hours. Measurements of residual glucose levels were collected after 24 hours.
[0049] The residual glucose after 24 hours of fermentation 1002 was then plotted against the percentage of CTS in the make-up water, as shown in the figure of example 10. Interestingly, the fermentation in reactors that had CTS in make-up from 20% to 60 % of water completed in 24 hours (i.e. substantially all residual starch has been consumed). While with no added CTS, it took 72h to complete the fermentation, even with the low sugar content present in the reactor (not shown).
[0050] Ethanol produced in 24 hours was greater than 70% of the theoretical glucan value or more than 80% of the theoretical maximum of glucan at 5.6 mg EP/g glucan and 8.4 mg EP/g glucan, respectively. These ethanol yields were obtained when CTS was used in 20 to 60% of the replacement water. With no CTS added during saccharification, the final ethanol produced after 72 hours of fermentation was 56% and 60% of the theoretical maximum glucan in the two tested enzyme dosages, respectively. Thus, it appears that the addition of the lignin binding agent not only increases the enzyme's conversion of cellulose to glucose, but also increases the fermentation efficiency. Example 4
[0051] In the fourth example experiment, a study was conducted to identify the optimal dose for the AnMBR effluent in enzymatic hydrolysis. For this example experiment, 5.8 mg of enzyme per gram of glucan dose was tested. Again, the Ctec2 enzyme was used. AnMBR effluent was used at 0 (Control), 15, 30, 45 and 60% water replacement in 15% total solids slurry. The saccharification was performed for 115h at 50 degrees Celsius, initial pH of 5.5 followed by 47h of fermentation at 32 degrees Celsius, initial pH of 5.5.
[0052] The percentage theoretical yield of 1102 glucose after 115 hours of saccharification that depends on the percentage of AnMBR 1104 effluent replacement for this experiment is illustrated in Figure 11. The results showed that the AnMBR effluent was added to 30% of total make-up water produced at maximum glucose. This suggests that AnMBR effluent can be used as a viable efficiency enhancing agent in the saccharification of lignocellulosic C6 solids.
[0053] An advantage of using AnMBR effluent as an efficiency enhancing agent is that the use of AnMBR effluent stream maintains the process water balance. While thin stillage is a viable option, as noted above, the use of AnMBR effluent does not require the transfer of water from the corn grain ethanol plant to the pulp mill. In addition to simplifying water balance, the use of AnMBR effluent over fine vinasse, or most other agents, avoids the possibility of cross-contamination between the cellulose plant and the corn grain ethanol plant. Example 5
[0054] In the fifth example experiment, after 115h of enzymatic hydrolysis, the reactors were cooled to 32 degrees Celsius and the pH adjusted back to 5.5. Urea was added at 0.06 g/L (as a nitrogen source) and Lactoside247 was added at 5 ppm. Yeast was inoculated at 0.5 g (dry)/L. Fermentations were carried out for up to 47 hours. Measurements for residual glucose were collected from the samples at 24 and 47 hours.
[0055] The residual glucose 1202 after 24 and 47 hours of fermentation was then plotted against the percentage of AnMBR 1204 effluent in the make-up water, as shown in the example in Figure 12. Interestingly, fermentation in reactors that had AnMBR effluent on replenishment from 15% to 60% of the water was finished in 47 hours (ie, substantially all residual starch was consumed). While no AnMBR effluent has been added, after 47 hours there is still residual sugar in the fermentation tank. Again, it appears that the addition of the lignin binding agent not only increases the enzyme's conversion of cellulose to glucose, but also increases fermentation efficiency. Example 6
[0056] In the sixth example experiment, an experiment was carried out to determine whether the combination of fine and clear vinasse (CTS) with an anaerobic membrane bioreactor (AnMBR) effluent provides more additional efficiency for the hydrolysis of C6 solids. Here, a full factorial design 3 (CTS levels) x 4 (AnMBR effluent levels) was performed to evaluate the interaction effect, if any, between the two additives. The levels of CTS (fine and clear vinasse) were 0, 10 and 25% of the total water at replacement and the effluent levels of AnMBR were 0, 10, 20 and 30% of the total water at the replacement. Novozymes' Ctec2 enzyme was used at a dose of 6 mg protein per gram of glucan. A total 15% solids saccharification was performed for 120 hours. The results of the experiment are illustrated in example figure 13.
[0057] The results indicated that there is an interaction effect observed between CTS and the AnMBR effluent when used in combination to aid in the saccharification of lignocellulosic C6 solids. It appears that the maximum glucose production (80.2% glucan to glucose conversion) was observed when CTS and AnMBR effluent are used in 10% each of the total make-up water in the present modality. However, using AnMBR effluent at 30% of the total make-up water helps with the water balance in the production facility, in addition to aiding in a good glucan to glucose conversion around 79%. Thus, depending on water load requirements, it may be helpful to change the makeup of the make-up water to optimize plant operations while simultaneously improving the hydrolysis efficiency of C6 solids.
[0058] The modalities as presented and described in the application (including figures and examples) are intended to be illustrative and explanatory of the aspects described. Modifications and variations of the embodiments shown, for example, of the apparatus and processes employed (or to be employed), as well as the compositions and treatments used (or to be used) are possible; all such modifications and variations are intended to be within the scope of one or more aspects.
[0059] The word "exemplifier" is used to mean that it serves as an example, case or illustration. Any embodiment or design described as "exemplifiers" is not necessarily to be construed as preferred or advantageous over other embodiments or designs, nor is it intended to preclude equivalent exemplary structures and techniques known to those skilled in the art. On the contrary, the use of the word exemplifier is intended to show the concepts in a concrete way, and the subject presented is not limited to these examples.
[0060] The term "or" is intended to mean an inclusive "or", rather than an exclusive "or". To the extent that the terms "comprises", "has", "includes", and other similar terms are used either in the detailed description or in the claims, for the avoidance of doubt such terms are intended to be inclusive in a manner similar to the term "which understands" as an open transition word, without excluding any additional or other elements.

权利要求:
Claims (13)
[0001]
1. Method for the treatment of lignocellulosic biomass to be supplied to a fermentation system for the production of a fermentation product, CHARACTERIZED by the fact that it comprises: pre-treating the biomass into pre-treated biomass; separating the pretreated biomass into a liquid component comprising sugars and a solids component comprising cellulose and lignin; adding a protein-rich by-product of ethanol production to biomass, wherein the protein-rich by-product comprises anaerobic bioreactor effluent; and treating the pretreated biomass solids component into a treated component; wherein the biomass comprises lignocellulosic material; wherein treating the solids component comprises applying an enzyme formulation and make-up water to form a slurry; and wherein the enzyme formulation comprises a cellulase enzyme.
[0002]
2. Method according to claim 1, CHARACTERIZED by the fact that the treatment of the solid component comprises the release of sugar.
[0003]
3. Method according to claim 2, CHARACTERIZED by the fact that sugars comprise glucose.
[0004]
4. Method according to claim 1, CHARACTERIZED by the fact that the protein-rich by-product of an ethanol production process comprises between 30% and 70% of the anaerobic bioreactor effluent.
[0005]
5. Method according to claim 4, CHARACTERIZED by the fact that a glucose yield is at least 90 percent of the theoretically available glucose.
[0006]
6. Method according to claim 5, CHARACTERIZED by the fact that a glucose yield is at least 60 percent of the theoretically available glucose.
[0007]
7. Method according to claim 1, CHARACTERIZED by the fact that the protein-rich by-product of an ethanol production process comprises at least 10% of anaerobic bioreactor effluent and at least 10% of fine vinasse.
[0008]
8. Method according to claim 1, CHARACTERIZED by the fact that the treatment of the solids component is carried out at a pH of 4.8 to 6.2.
[0009]
9. Method according to claim 1, CHARACTERIZED by the fact that the treatment of the solids component further comprises maintaining the solids component at a temperature of 30 to 60°C.
[0010]
10. Method according to claim 1, CHARACTERIZED by the fact that the treatment of the solid component further comprises treating the solid component for 48 to 144 hours.
[0011]
11. Method, according to claim 1, CHARACTERIZED by the fact that the pre-treatment of the biomass further comprises maceration, and wherein the maceration comprises mixing the biomass with water to achieve at least 10 percent of the content of solids and apply sulfuric acid to the biomass at a concentration of 0.8 to 1.3 percent by weight, and hold the biomass at a temperature of 130 to 180°C for 5 to 12 minutes.
[0012]
12. Method according to claim 11, CHARACTERIZED by the fact that the pre-treatment of biomass further comprises steam explosion, and in which steam explosion comprises (a) maintaining the macerated biomass at a temperature of 150 to 165°C and a pressure of 0.52 to 0.86 MPa (75 to 125 pounds per square inch) and (b) relieve pressure.
[0013]
13. Method according to claim 1, CHARACTERIZED by the fact that the lignocellulosic material comprises corn cobs, corn plant husks, corn plant leaves and corn stalks, wherein the corn cobs comprise 25 to 50 percent of the lignocellulosic material, corn plant husks and corn plant leaves comprise 30 to 60 percent of the lignocellulosic material, and corn stalks comprise 10 to 30 percent of the lignocellulosic material.

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同族专利:

公开号 | 公开日

CN103547677B|2016-10-12|

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MX2013008370A|2014-01-20|

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CN103547677A|2014-01-29|

EP2665823A1|2013-11-27|

WO2012099967A1|2012-07-26|

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法律状态:
2018-04-03| B06F| Objections, documents and/or translations needed after an examination request according [chapter 6.6 patent gazette]|

2019-06-11| B06T| Formal requirements before examination [chapter 6.20 patent gazette]|

2020-09-15| B07A| Technical examination (opinion): publication of technical examination (opinion) [chapter 7.1 patent gazette]|

2021-03-16| B09A| Decision: intention to grant [chapter 9.1 patent gazette]|

2021-05-18| B16A| Patent or certificate of addition of invention granted|Free format text: PRAZO DE VALIDADE: 20 (VINTE) ANOS CONTADOS A PARTIR DE 18/01/2012, OBSERVADAS AS CONDICOES LEGAIS. |

优先权:

申请号 | 申请日 | 专利标题

US201161433864P| true| 2011-01-18|2011-01-18|

US61/433,864|2011-01-18|

PCT/US2012/021731|WO2012099967A1|2011-01-18|2012-01-18|Systems and methods for hydrolysis of biomass|

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