• 专利附录
  • 专利说明
  • 权利要求
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    • 专利摘要:
    Bioethanol is produced by adding (10) liquid to cereal flour, including wheat flour, hydrolysis (12) and fermentation (14) of the dough and distillation (16) of the fermented substrate. The distillation residue, which contains fibers and proteins, is treated by: separation (18), essentially without prior dilution, between on the one hand a fraction enriched in fibers and on the other hand a defibrated liquid fraction; centrifugation (22,24) of the defibrated liquid fraction, giving on the one hand a fraction concentrated in proteins and on the other hand an effluent; drying (30) of the concentrated protein fraction, giving a first by-product, of the protein concentrate type; recycling part of the effluent as a flour addition liquid; concentration (26) of another part of the effluent then mixing with the fiber fraction; and drying (28) the mixture, yielding a second by-product, distillers' grains type with DDGS solubles.
    公开号:BE1018899A3
    申请号:E2010/0526
    申请日:2010-09-03
    公开日:2011-10-04
    发明作者:Andreas Redl；Sophie Frederix
    申请人:Syral Sas；
    IPC主号:
    专利说明:

    The invention relates to the production of value-added by-products in a process for the production of bioethanol starting from the production of bioethanol from a cereal raw material, in particular wheat. vegetable matter, especially from wheat, with optimization of water and energy consumption.
    Bioethanol obtained from cereals such as wheat is produced by enzymatic hydrolysis (saccharification) of the starch contained in the cereal, fermentation of sugars resulting from this hydrolysis, and distillation.
    The grain raw material must, however, be processed prior to the saccharification and fermentation stages.
    A first technique is to grind the cereal to eliminate germs and fibers, and then process the flour thus obtained.
    Another technique is to combine grinding and soaking of the cereal. The quenched and ground raw material is then subjected as such to saccharification and fermentation, or it is subjected to a prior separation so as to eliminate the fiber and the seed, by subjecting to saccharification and fermentation only the part containing the starch.
    Yet another technique is to directly process whole grain flour without soaking. The whole flour, along with the sprouts and fibers, is mixed with a thinner to give a paste, which is then diluted again before liquefaction and saccharification. After saccharification, the liquid dispersion can be further diluted before the fermentation step to produce the ethanol. Finally, when the fermentation is complete, the mixture is subjected to distillation to recover the ethanol.
    The invention relates to a method implementing the latter technique.
    In so far as the entire mixture is subjected to fermentation and distillation, after production of the ethanol there is a large volume of residues containing fibers, proteins, as well as other non-fermented materials such as minerals and fats.
    These residues can be valorized to give by-products usable especially in the animal feed as concentrated nutritive elements, in particular as an energy supplement and / or protein. The so-called DDGS (Distiller's Dried Grain with Solubles), which is a dry food product with a moderate protein content between 25 and 35% in dry matter ( Nx5,7) and with a balanced blend of minerals and nutrients. In particular, DDGS can be used as a partial economic substitute for corn and soybeans for livestock and poultry.
    However, the separation of DDGS requires a certain amount of energy, and because of the relatively low value of this by-product, it seems very desirable to be able to increase both the nutritional value (improvement of the composition, especially of protein content) and economic (by cost reduction). In order to provide a protein content sufficient for the growth needs of the animals in a reasonably unmanageable ration volume, a protein content of 45% or more in dry matter is desirable (N × 5.7). In addition these proteins must have a good digestibility, being at 80% or more.
    In this context, US Pat. No. 4,810,647 A (Valpi) proposes a technique for improving the value of the bioethanol distillation by-products, but at the cost of a very complex process involving numerous treatment steps and requiring quantities. significant amounts of water.
    WO 2005/029974 A1 (Heineken Technical Services BV) describes another improved process for recovering fermentation residues, used in the production of ethanol from a cereal. The method described allows for efficient separation of the protein and fibrous components of the residue, thanks to a simple and very robust installation, which can be applied to a process operating continuously. But in this process, one of the critical elements is the addition of water to the fermentation residue to form a suspension before the separation step. Therefore, a significant amount of water is required for the implementation of this technique, especially since the fermentation residue must be very highly diluted, typically a dilution of less than 5% dry matter. The diluted stream is then separated into a fibrous concentrate and a proteinaceous juice. The protein juice is partially recycled to the fermentation residue stream, the remainder being concentrated so as to obtain, on the one hand, a protein concentrate and, on the other hand, an aqueous deprotein flux. This latter stream can also be recycled as a diluent of the fermentation residue stream.
    This technique, if it is effective, does not require less, on the one hand, the use of large quantities of water, which come to encumber all the cost of exploitation of the process and on the other hand , the treatment of large volumes of residues (due to significant dilutions), requiring a corresponding sizing of the installations, with again a repercussion on the costs of both investment and exploitation. The aim of the invention is to overcome the drawbacks of the prior techniques for recovering the by-products of bioethanol production, by proposing a process which: on the one hand enables the quantity of water (and energy) to be limited necessary to obtain by-products; and - on the other hand only requires the processing of small volumes of intermediate flows, so uses only smaller and therefore less expensive installations.
    Compared to the state of the art, it will thus be possible to obtain a more efficient separation of the protein and fibrous components of the fermentation residue.
    More precisely, the process of the invention provides, for the valorization of distillation byproducts resulting from the production of bioethanol from a cereal raw material, in particular wheat, the successive stages of: a) preparation of a paste by adding liquid to flour of said cereal raw material; b) hydrolysis and fermentation of the dough, giving a fermented substrate; c) distilling the fermented substrate, giving an ethanol-containing fraction and a distillation residue containing fibers and proteins, with, in addition, typically the steps of: d) separating the residue, essentially without prior dilution thereof, between on the one hand a fraction enriched in fibers and on the other hand a liquid fraction defibrated; e) centrifugation of the defibrated liquid fraction, giving on the one hand a concentrated protein fraction and on the other hand an effluent; f) drying the concentrated protein fraction of step e), yielding a dry protein concentrate by-product; g) recycling a portion of the effluent from step e) as an addition liquid of step a); h) concentration of another part of the effluent of step e) then mixing with the fiber-enriched fraction of step d); and i) drying the mixture of step h), giving a by-product of dry distillers type with DDGS solubles.
    The separation step d) can in particular be carried out by sieving, or by centrifugal decantation.
    Advantageously, the process further comprises an additional step of concentrating the fiber-enriched fraction of step d) before mixing it in step h) with the effluent of step e).
    The centrifugation step e) is preferably a two-stage centrifugation step, the concentrated protein fractions of each of the centrifugation stages being subjected to drying in step f).
    The concentrated protein fractions from these two stages can be dried together or separately. Thus, when they are dried separately, fractions are obtained respectively concentrated in wheat proteins and in yeast proteins.
    On the other hand, step h) of concentration of another part of the effluent, and / or step c) of distillation, advantageously comprise the recovery of a liquid condensate or a liquid fraction, and recycling this condensate or liquid fraction as the addition liquid of step a) of mixing.
    An example embodiment of the method of the invention will be described, with reference to FIG. 1, which is a block diagram illustrating the various steps of this method, as well as the different flows processed.
    . 0 λ
    The raw material is a whole wheat flour which is added with a liquid in a mixing unit 10 to obtain a paste. The liquid added to the flour may be water, or clarified residues recycled from other process steps (as will be explained below), or a mixture of both. In addition, the water used at this stage may be wholly or partly obtained by recycling condensates of water vapor from the distillation or evaporation steps (units 16 and 26 in the Figure). The next step is to subject the pulp to hydrolysis in unit 12 to obtain fermentable sugars. The composition obtained is then diluted and transferred to a fermentation unit 14, with the addition of yeasts. This dilution before fermentation can be done with condensates. After fermentation, the fermented substrate is transferred to a distillation unit 16 for extracting bioethanol. During this distillation, an aqueous fraction containing ethanol is obtained on the one hand and a residue from which recoverable by-products extracted by the characteristic process of the invention described below can be obtained.
    This aqueous fraction containing the ethanol is then refined according to a distillation process giving firstly pure ethanol and secondly a liquid fraction that can be used as an addition liquid for the mixing step a).
    The distillation residue is mainly formed of the following constituents (these typical values are of course not limiting): - fibers: 10 to 20% on dry matter, - proteins: 25 to 40% on dry matter, - fats: 5 at 10% on dry matter, - starch: less than 5% on dry matter, - other carbohydrates: 20 to 35% on dry matter.
    These five constituents represent at least 75% by weight, most often at least 85% by weight, of the dry matter contained in the resin, knowing that the dry matter content of the liquid residue is usually of the order of 10 to 20%.
    The term "fiber" as used herein is synonymous with "crude fiber" and refers to the skeletal components of the plant cell that are particularly resistant to digestion by the digestive tract enzymes of non-ruminant animals. When referred to below as "fiber content" or "fiber concentration" this content or concentration will be considered as determined by the analytical method described in ISO 6865: 2000E, entitled "Animal Feed". - Determination of crude fiber content - Method with intermediate filtration ".
    The "other carbohydrates" mentioned above correspond to mixtures composed mainly of soluble carbohydrates and their derivatives, including in particular arabinoxylo-oligosaccharides (AXOS), glycerol and organic acids, mainly lactic acid.
    The distillation residue thus defined, sometimes called bottom stills, is first treated by a unit 18 for separating the fibers.
    This step is conveniently carried out by means of a sieve, for example in the form of a grid, perforated plate or fabric, or by means of a centrifugal decanter.
    In the case of a sieve, the orifices thereof may be rectangular, rounded or triangular. Preferably, the screen comprises curved, conical or horizontal vibrating grids. Typically, the screen used for the implementation of the invention has orifice sizes of at least 0.075 mm, in principle not exceeding 1 mm. In a preferred embodiment, the screens have orifice sizes of between 100 and 900 μm, very advantageously between 250 and 750 μm.
    Still in the case of a sieve, the defibration carried out by the separation unit 18 makes it possible to obtain: on the one hand, a defibrinated liquid fraction, rich in proteins, representing from 75 to 90% by volume of the residue of starting distillation, with a solids content of typically between 10 and 15%; - On the other hand, a fraction enriched in fibers, representing 10 to 25% by volume of the treated stream, with a dry matter content typically between 16 and 23%.
    In the case where a centrifugal decanter is used for the separation unit 18, the defibration makes it possible to obtain: on the one hand, a defibrinated liquid fraction, rich in proteins, representing from 85 to 95% by volume of the residue of starting distillation with a dry matter content typically between 10 and 15%; - On the other hand, a fraction enriched in fibers, representing 5 to 15% by volume of the treated stream with a solids content typically between 30 and 40%.
    The fraction enriched in fibers resulting from the defibration stage 18 is advantageously concentrated by an extraction unit 20, for example a press, which makes it possible to separate on the one hand a liquid effluent and on the other hand a fibrous concentrate from which removed most of the liquid constituents with their soluble elements.
    The defibrated liquid from the separation 18, meanwhile, is directed to a settling unit 22, for example a centrifugal decanter for separating a concentrated protein fraction and a supernatant. The supernatant is advantageously subjected to additional centrifugation in unit 24 to obtain a second concentrated protein fraction which will be added to the concentrate from decantation 22.
    This step of separating by centrifugation in one or (preferably as illustrated) two stages is carried out by devices of the centrifugal decanter or nozzle centrifuge type, or by a combination of the two types of apparatus - when two types of apparatus are combined, the first stage is preferably a centrifugal decanter. The setting of the centrifuges depends on the technical characteristics of the equipment and the material to be treated. The centrifugation conditions are adjusted so that the protein content of the concentrated fraction is increased by at least 30%, preferably by at least 40%, very preferably by at least 50% relative to the protein content. of the initial distillation residue. The dry matter content of the protein enriched fraction is correspondingly increased by at least 80%, preferably by at least 1% by weight, relative to the dry matter content of the initial residue.
    The concentrated protein fraction obtained after these centrifugation steps thus contains between 20 and 35% of dry matter, with a protein content of at least 45% on dry matter.
    On the other hand, the composition of this protein enriched fraction mainly comprises wheat gluten proteins, a mixture of wheat gluten proteins and microorganism proteins (yeasts), or mainly microorganism proteins, differences in composition being determined by the operating conditions of the centrifugation steps.
    Regarding the other fraction (clarified supernatant); its composition will also depend on the operating conditions of the centrifugation, with a solids content of between 8 and 12% and a protein content of between 10 and 35% on dry matter.
    The clarified residues from the centrifugation steps 22, 24 are combined with the liquid effluents discharged by the press 20 used to separate the water from the fibers, and the whole is recycled in the process: - partly to serve as an addition liquid wheat flour in the mixing unit 10, to prepare the dough to be hydrolysed; the remainder being concentrated in an evaporator 26 (the condensation water of which may be reused, in particular for the preparation of the dough by the mixer 10), so as to produce concentrated clarified residues.
    The concentrated clarified residues from the evaporator 26 are combined with the fibers extracted from the extraction press 20, and the whole is introduced into a dryer 28 which ultimately produces a DDGS distillery waste with a reduced protein content.
    This step of drying the clarified residues and fibers can be carried out concurrently (i.e. after mixing the fibers and clarified residues as shown in the Figure) or separately. It is operated by means of conventional drying equipment, such as flash dryers, ring dryers or drum dryers.
    The concentrated protein fraction from the centrifugation steps 22 and 24 is similarly treated by passing through a dryer 30, so as to obtain a final byproduct of a dry protein concentrate. The dry protein concentrates thus obtained typically have a water content of less than 10%, an ash content of less than 5%, a fat content of 5 to 10%, a crude fiber and arabinoxylan content of approximately 10%. , a protein content greater than 45%, preferably greater than 50% (N × 5.7). The present proteins have an ileal in vitro digestibility of at least 80% (according to the method described by Boisen S., Animal Feed Science & Technology, 1995, pp.29-43).
    The dryer 30 may again be a conventional dryer of the flash dryer type, ring dryer or drum dryer.
    The method just described thus makes it possible to obtain from a whole wheat flour, on the one hand bioethanol, and on the other hand two types of valuable by-products, namely a dry protein concentrate. and DDGS Distillery DDG with reduced protein content. This dry protein concentrate may be composed of a protein mixture obtained during the centrifugation steps 22,24.
    Since it is also possible to dry these two fractions separately, it is also possible to obtain concentrated fractions of wheat proteins and yeast proteins.
    The following three examples illustrate the invention, with indicative numerical values.
    Example 1
    Residues of distillation having a content of 15% of dry matter (DM) at the outlet of the distillation unit 16 were treated without dilution by a Sweco-type grinding unit 18 with sieves of 500 μm aperture, with a feed rate of 650 kg / h at a temperature of 70 ° C. The composition of the input and output streams is given in Table 1 below.
    Table 1: Composition of flows in the defibration stage
    The retained fraction, which is the fiber-enriched fraction, was sent to a water extraction equipment. The through fraction, meanwhile, was treated with a centrifugal decanter to obtain a protein enriched stream. The centrifugal decanter used in this example was a Westfalia AG model CA220 220 mm in diameter and 5100 rpm (50 Hz) maximum speed, corresponding to 3200 g.
    Tests were carried out for different differential speeds, as shown in Tables 2 and 3: Table 2 shows the settler settings, while Table 3 gives the respective compositions of the different flows, for three different speeds.
    Table 2: Settling chamber settings
    Table 3: Composition of the different flows for differential decanter velocities of 4.12 and 24 rpm
    This example shows that it is possible to obtain a concentrated stream of proteins without the need to dilute the distillation residue.
    Example 2
    Residues of distillation having a content of 15% dry matter at the outlet of the distillation unit 16 were treated without dilution by passing through curved defibration screens with 250 μm openings. The feed rate was 600 kg / h at a temperature of 70 ° C. The composition of the input and output streams is given in Table 4 below.
    Table 4: Composition of flows at the separation stage
    The retained fraction, which is the fiber-enriched fraction, was sent to a water extraction equipment. The through fraction, meanwhile, was treated with a centrifugal decanter to obtain a protein enriched stream. The centrifugal decanter used in this example was a Westfalia AG type CA22Q 220 mm diameter and 5100 rpm (50 Hz) maximum speed, corresponding to 3200 g.
    Tests were carried out for different differential speeds, as shown in Tables 5 and 6: Table 5 shows the settler settings, while Table 6 gives the respective compositions of the different flows, for three different speeds.
    Table 5: Settling chamber settings
    Table 6: Composition of the different flows for differential decanter speeds of 6, 8 and 12 rpm
    Example 3
    This example shows the use of a decanter as a fiber separation tool.
    Residues of distillation having a content of 14.1% of dry matter (DM) at the outlet of the distillation unit 16 were treated without dilution by an Andritz type D7 LLC30 C HP settling unit 18, with a feed rate of 40 t / h at a temperature of 70 ° C, the setting of which is optimized for effective fiber separation. The composition of the input and output streams is given in Table 7 below.
    Table 7: Composition of flows at the defibration step
    Part of the supernatant fraction is treated with a centrifugal decanter to obtain a protein-enriched stream. The centrifugal decanter used in this example was a Westfalia AG type CA220 220 mm diameter and 5100 rpm (50 Hz) maximum speed, corresponding to 3200 g.
    Tests were carried out for a differential speed of 12 rpm, as shown in Tables 8 and 9: Table 8 indicates the setting of the decanter, while Table 9 gives the composition of the different flows, for a differential speed of 12 rpm. .
    Table 8: Adjusting the clarifier
    Table 9: Composition of the different flows for a differential speed of decanter of 12 rpm
    权利要求:
    Claims (8)
    [1]
    1. A process for the recovery of distillation byproducts from the production of bioethanol from a cereal raw material, in particular wheat, this process comprising the successive steps of: a) preparation of a paste (10) adding liquid to flour of said cereal raw material; b) hydrolyzing (12) and fermenting (14) the dough, giving a fermented substrate; c) distilling (16) the fermented substrate, giving a fraction containing ethanol and a distillation residue containing fibers and proteins, characterized in that it further comprises the following steps: d) separation (18) the residue, essentially without prior dilution thereof, between firstly a fraction enriched in fibers and secondly a liquid fraction defibrated; e) centrifuging (22, 24) the defibrated liquid fraction, giving on the one hand a concentrated protein fraction and on the other hand an effluent; f) drying (30) the concentrated protein fraction of step e), yielding a dry protein concentrate by-product; g) recycling a portion of the effluent from step e) as an addition liquid of step a); h) concentration (26) of another part of the effluent of step e) then mixing with the fiber-enriched fraction of step d); and i) drying (28) of the mixture of step h), giving a by-product of dry distillers type with DDGS solubles.
    [2]
    2. The process of claim 1, wherein the separation step (d) (18) is carried out by sieving.
    [3]
    The process of claim 1, wherein the separation step (d) (18) is carried out by centrifugal decantation.
    [4]
    The process of claim 1, further comprising an additional step of concentrating (20) the fiber-enriched fraction of step d) prior to mixing in step h) with the effluent of step e ).
    [5]
    5. The process of claim 1, wherein the centrifugation step (e) (22, 24) is a two-stage centrifugation step, the concentrated protein fractions of each of the centrifugation stages being subjected to drying (30). of step f).
    [6]
    The method of claim 5, wherein the protein concentrated fractions of each of the centrifugation stages are separately subjected to drying (30) of step f).
    [7]
    The process of claim 1, wherein the step (h) of concentrating (26) another portion of the effluent comprises recovering a liquid fraction and recycling that liquid fraction as an addition liquid. of step a) of mixing (10).
    [8]
    8. The process of claim 1, wherein the distillation step (c) (16) comprises recovering a liquid condensate or a liquid fraction, and recycling said condensate or liquid fraction as liquid. addition of mixing step (a) (10).
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    同族专利:
    公开号 | 公开日
    FR2954892B1|2012-04-20|
    FR2954892A1|2011-07-08|
    FR2949645B1|2011-10-28|
    FR2949645A1|2011-03-11|
    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    GB2091293A|1981-01-21|1982-07-28|Bijenkorf Zetmeel|The production of starch and alcohol from starch-bearing grains|
    EP0443813A1|1990-02-20|1991-08-28|Kirin Beer Kabushiki Kaisha|Protein-rich products of brewer's spent grain origin|
    WO2005029974A1|2003-09-30|2005-04-07|Heineken Technical Services B.V.|Method of isolating a protein concentrate and a fibre concentrate from fermentation residue|EP2778330A1|2013-03-11|2014-09-17|Joseph Talpe|Hinge assembly|
    GB2489967A|2011-04-13|2012-10-17|Ensus Ltd|Method of producing an animal feed by hydrolysis and fermentation|
    GB2493547A|2011-08-10|2013-02-13|Agri Ltd Ab|Yeast and protein recovery from an ethanol fermentation process|
    GB2505502A|2012-09-03|2014-03-05|Ensus Ltd|Hydrolysis and fermentation process for producing bioethanol|
    FR3028525B1|2014-11-14|2017-10-13|Roquette Freres|METHOD FOR THE VALORISATION OF YEAST BIOMASS FROM THE PRODUCTION OF ETHANOL|
    PL422196A1|2017-07-12|2019-01-14|Wioletta Kosecka|Method for wasteless obtaining of bioethanol, fodder yeast and carbon dioxide and the system for production of these products|
    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    FR0956035|2009-09-04|
    FR0956035A|FR2949645B1|2009-09-04|2009-09-04|PROCESS FOR THE VALORISATION OF DISTILLATION BY-PRODUCTS FROM THE PRODUCTION OF BIOETHANOL FROM A CEREAL RAW MATERIAL, IN PARTICULAR WHEAT|
    FR1050163|2010-01-12|
    FR1050163A|FR2954892B1|2009-09-04|2010-01-12|PROCESS FOR THE VALORISATION OF DISTILLATION BY-PRODUCTS FROM THE PRODUCTION OF BIOETHANOL FROM A CEREAL RAW MATERIAL, IN PARTICULAR WHEAT|
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