EP1991687A2 - Extraction of fermentation-inhibiting substances from a fluid - Google Patents
Extraction of fermentation-inhibiting substances from a fluidInfo
- Publication number
- EP1991687A2 EP1991687A2 EP07722009A EP07722009A EP1991687A2 EP 1991687 A2 EP1991687 A2 EP 1991687A2 EP 07722009 A EP07722009 A EP 07722009A EP 07722009 A EP07722009 A EP 07722009A EP 1991687 A2 EP1991687 A2 EP 1991687A2
- Authority
- EP
- European Patent Office
- Prior art keywords
- whey
- container
- fluid
- bioreactor
- ethanol
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Withdrawn
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12C—BEER; PREPARATION OF BEER BY FERMENTATION; PREPARATION OF MALT FOR MAKING BEER; PREPARATION OF HOPS FOR MAKING BEER
- C12C1/00—Preparation of malt
- C12C1/02—Pretreatment of grains, e.g. washing, steeping
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12C—BEER; PREPARATION OF BEER BY FERMENTATION; PREPARATION OF MALT FOR MAKING BEER; PREPARATION OF HOPS FOR MAKING BEER
- C12C7/00—Preparation of wort
- C12C7/04—Preparation or treatment of the mash
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12G—WINE; PREPARATION THEREOF; ALCOHOLIC BEVERAGES; PREPARATION OF ALCOHOLIC BEVERAGES NOT PROVIDED FOR IN SUBCLASSES C12C OR C12H
- C12G1/00—Preparation of wine or sparkling wine
- C12G1/02—Preparation of must from grapes; Must treatment and fermentation
- C12G1/0203—Preparation of must from grapes; Must treatment and fermentation by microbiological or enzymatic treatment
-
- 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 present invention relates to a process for the degradation of gärhemmender substances from a fluid, a process for the production of ethanol, in particular from whey, and an array of bioreactors for carrying out the process for producing ethanol from whey.
- ethanol can be obtained from saccharide-containing substances, in particular sugar or glucose. It cereals, sugar beet, potatoes and whey are known as glucose suppliers, which are suitable for ethanol production. But other saccharide-containing foods and food residues can be fermented.
- Object of the present invention is therefore to provide a method by which gärhemmende substances can be easily removed and thereby a simple and inexpensive ethanol production, especially from the whey, guaranteed.
- This object is achieved by a process for the degradation of fermentation-inhibiting substances from fluids according to claim 1, a process for producing ethanol according to claim 13, a process for producing ethanol from whey according to claim 14, and an arrangement of bioreactors for producing ethanol from whey according to Claim 29 solved.
- the present invention is based on the finding that the low ethanol yield in the ethanol production from saccharide-containing foods or food residues, such as whey, is due to two problems: For one thing, when using whey as a food residue, ie. There were inhibitors in the whey as a waste product from cheese dairies, which severely restricted the production of ethanol. These inhibitors include, in particular, copper, which makes the fermentation of whey into ethanol almost impossible, as well as mold fungi which settle by non-immediate further processing of the whey. Such inhibitors are also present in other saccharide-containing fermentable foods, such as grapes or barley, and must be removed from the fluid to be fermented for ethanol production.
- the fluid to be fermented with a microbiotic mixture of photosynthetic microorganisms and light-emitting microorganisms is applied, which is designed to degrade the gärhemmenden Stofffe. If the whey is not yet heavily loaded, adding hops can also provide sufficient bacteriostatic effects.
- the microbiotic mixture is not added directly to the fluid, but the materials from which the fluid is made are pretreated with the microbiotic mixture. This is particularly advantageous in the production of wine or beer, in which the grapes or apples or malting barley are treated before applying must or mash with the microbiotic mixture. This allows fermentation-inhibiting substances, such as mildew, to be removed before the fermentation process and can not contaminate must or mash.
- the photosynthetic microorganisms contained in the microbiotic mixture are prochlorophytes, cyanobacteria, green sulfur bacteria, purple bacteria, chloroflexus-like forms, heliobacteria and heliobacillus-like forms, and mixtures of two or more thereof and the light-emitting microorganisms contained in the microbiotic mixture Photobacterium phosphoreum, Vibrio fischeri Vibrio harveyi, Pseudomonas lucifera or Beneckea or mixtures of two or more there are more of them. Furthermore, it may be advantageous if the microbiotic mixture additionally contains plant extracts, enzymes, trace elements, polysaccharides, alginine derivatives and / or other microorganisms individually or in combination.
- a method is proposed in which, in a first step, such inhibitors, such as copper, are removed from the whey.
- the lactose present in the whey is broken down into glucose and galactose, whereby the galactose is not treated as a waste product, but, as another particularly preferred embodiment shows, with the aid of a certain yeast strain, the so-called Kluyveromyces. converted to glucose.
- a fermentation agent in particular yeast or bacteria, added in order to convert the now comparatively high concentration of glucose into ethanol.
- copper is removed from the whey by means of electrolysis.
- the percentage of ethanol in the fermentation solution must be taken into account when fermenting to ethanol, since an excessively high alcohol content adversely affects the fermentation process. Therefore, as another advantageous embodiment shows, the alcohol content is maintained at a certain level, preferably below 12%. For this purpose, excess ethanol can preferably be removed from the fermentation solution by means of membrane filtration.
- the method according to the invention takes place in a bioreactor.
- the three main steps of the procedure can be carried out in the same bioreactor. For this, however, the bioreactor must be prepared for the next step between the individual steps.
- the method can also take place in preferably three bioreactors arranged one behind the other, wherein a conversion of the individual bioreactors due to the method steps assigned to them permanently is dispensed with.
- a first bioreactor is preferably equipped with an electrolysis device, so that a removal of copper from the whey is made possible.
- a special equipment of the bioreactor can be used.
- a particularly preferred bioreactor consists of a coated container and a coated filling body, wherein the coatings are chosen such that upon application of an electric field the bioreactor itself acts as an electrolysis device.
- a photocatalytic coating of the bioreactor and an activated carbon coating of the filling body have proved to be particularly advantageous. When the electric field is applied, the filler body then serves as the anode and the copper ions are deposited on the activated carbon layer.
- whey is introduced from a cheese factory and removed the interfering copper from it. If the whey is heavily loaded, for example because it was already stored, the whey may also be added to the microbial mixture here. If the whey is only slightly loaded or fresh, the whey may also be added to hops before it is introduced into the first bioreactor, preferably 100 g of hops per hectolitre of whey, so that on the one hand an already existing load is reduced or at least slowed down, on the other hand it can be ensured that such a burden does not occur at all.
- the whey prepared in this way is then transferred to a second bioreactor in which the lactose contained in the whey is broken down into glucose and galactose by means of lactase.
- a second bioreactor in which the lactose contained in the whey is broken down into glucose and galactose by means of lactase.
- further Kluyveromyces - yeasts may be provided in the second bioreactor, which on the one hand also cause a breakdown of lactose into glucose and galactose, on the other hand, but are also able to convert galactose into glucose.
- a third bioreactor into which the glucose mixture is introduced there are microorganisms, in particular yeasts or fermenting bacteria, which bring about a conversion of glucose by means of alcoholic fermentation into ethanol.
- the ethanol thus produced is then preferably separated from the glucose mixture by means of a membrane.
- bioreactor arrangement in which the individual bioreactors are coated with a photocatalytically active layer, and have one or more recesses for the passage of the whey into the interior of the bioreactor.
- a filler with activated carbon is present, which increases the reaction surface, wherein deposited on the filler preferably copper or settle microorganisms for ethanol production and enzymes can be immobilized.
- an embodiment of the bioreactors in which a longitudinal strip-shaped photocatalytic coating alternates with a longitudinal strip-shaped diamond coating.
- Figure 1 is a schematic drawing of a preferred embodiment of the present invention, in which three bioreactors are connected in series in series to carry out the process according to the invention for producing ethanol from whey;
- Figure 2 a schematic drawing of a preferred embodiment of a bioreactor for the inventive method.
- FIG. 3 shows a schematic drawing of a further exemplary embodiment of the present invention in order to carry out the process according to the invention for producing ethanol from whey.
- FIG. 1 shows a preferred embodiment of an arrangement 1 of bioreactors 2a-c for carrying out the method according to the invention.
- whey which is otherwise produced as a waste product by cheese dairies
- the whey is transferred from a storage or delivery tank 4 via a first line 6 in the arrangement 1 of bioreactors 2a-c.
- the whey could be passed directly through the line 6 from the cheese factory in the arrangement 1, without a tank 4 would be required.
- the whey in the tank can be added to 4 hops, preferably 100 g hops / hl whey. Hops are mycotically selective and suppress the gram-positive bacteria, which means that foreign germs contained in the whey can no longer multiply. This also means that especially the Zuckerverstoffophden bacteria that reduce the ethanol yield due to Zuckergehaltreduzi für be prevented in their multiplication. It is possible to add hops as total substance, but it is also possible to add only the ß - acids of the hops necessary for the bacteriostatic effect of the hops as a hop extract of the whey.
- the whey is already heavily contaminated with foreign germs, it is also advantageous for the whey to add a microbiotic mixture of photosynthetically active microorganisms and light-emitting microorganisms. This microbiotic mixture is also suitable for removing mold in the whey.
- a first bioreactor 2a the whey is separated from inhibitors for ethanol production. This can be done via electrolysis, especially in the presence of copper. In addition, additions of the microbiotic mixture can take place in the bioreactor 2a.
- an electrolysis device 8 is provided, at which the copper ions are deposited at the anode.
- the electrolysis apparatus can also be designed as a coated bioreactor with filler body, in which an electric field is formed by an alternating coating of diamond and, for example, titanium dioxide and an activated carbon coating of the filler body.
- the filler may have the form of a spindle, which in turn has the coating of activated carbon.
- an external power source for the electrolysis should be used for a good result.
- a weak current between 400 and 600 mA, or 0.3 to 2.6 V, preferably 1, 9 V, applied, and the filler used as the anode.
- the copper ions are not freely present in the whey, but are bound to the already contained in the whey for the breakdown of lactose in glucose and galactose responsible lactase enzymes, it makes sense to recover these enzymes back to not unnecessarily many enzymes in it To have to use the following process step of Laktoseaufspaltung.
- the applied current is turned off and initialized a voltage reversal, whereupon the enzymes dissolve from the packing, while the copper ions remain on the packing. If, at the same time, the whey thus treated is removed from the first bioreactor 2a via a further line 10, the lactase enzymes are present in the whey, but no or vanishingly few copper ions.
- the whey comes directly from the cheese factory, it usually has a temperature of 45 0 C - 55 0 C.
- the temperature does not matter, so that the bioreactor 2a does not need to be equipped with a temperature control unit.
- the whey in the bioreactor 2a can still be concentrated. That is, excess water is removed from the whey, so that a high lactose concentration is achieved.
- the whey is passed via the second line 10 into another bioreactor 2b.
- a splitting of lactose into its two components glucose and galactose instead.
- this is done at a temperature of 30 0 C to 35 0 C.
- the bioreactor 2b a cooling or heating unit (not shown here) or integrated into the bioreactor, which brings the whey to the desired temperature before the breakdown of the lactose.
- a temperature sensor (not shown here) can also be arranged in the bioreactor itself, which constantly monitors the reaction temperature.
- the enzyme used is lactase, which is advantageously produced by Kluyveromyces
- - Yeasts is that the lactase they provide not only a breakdown of lactose in glucose and galactose is achieved, but also a conversion of galactose into glucose is possible. This is of decisive advantage for the production of ethanol since it increases the glucose content and thus the amount of ethanol.
- a relatively highly concentrated glucose mixture is obtained which, for further processing in the embodiment shown here, is transferred via a third line 14 into a further bioreactor 2c.
- the bioreactors 2b and 2c can also be integrally formed. This would now be a replacement of the filler be made to retrofit the bioreactor to the fermentation process.
- the bioreactor 2c is equipped with a packing 16 which may contain yeast or bacteria as microorganisms used for fermentation. Since both fermentation processes do not take place at the same temperatures, a simultaneous presence of the two types of microorganisms in the packing is possible, but only the microorganisms for which the corresponding temperature is applied are active. Thus, an alcoholic fermentation by means of yeasts at a temperature of less than 25 0 C 1, preferably between 8 0 C and 10 0 C, instead, while the fermentation with the aid of bacteria, especially Thermoanaerobacter ethanolicus, takes place at 60 0 C to 65 ° C. , To precisely control the temperature, the bioreactor 2c may be preceded or integrated with a cooling or heating unit (not shown). Likewise, a temperature measuring device may be present, which controls whether the temperature meets the requirements.
- microorganisms are immobilized by the packing 14 in the bioreactor 2c, which simultaneously provides an increased reaction area.
- the already produced ethanol must be removed from the bioreactor 2c. This can advantageously be done via a diffusion membrane, not shown here. But it is also conceivable to use a special distillation membrane, which is relatively expensive. Ideally, the alcohol concentration should not exceed 12%.
- the ethanol produced can then be fed via a further line 18 to a storage tank 20.
- FIG 2 shows a schematic diagram of a preferred embodiment of the bioreactor consisting of a container 22 and a packing 24.
- the container 22 is cylindrical, but it may also have any other shapes.
- the side walls of the container 22 are made of stainless steel in the illustrated embodiment and partially be provided with a photocatalytic coating 26. This coating 26 may be formed on the inner peripheral wall of the container 22 and / or - as shown in Figure 2 - on the outer wall 28.
- the container 22 is made of V4A steel and provided with a titanium dioxide coating. Instead of this titanium dioxide, indium tin oxide or the like can also be used.
- the outer wall 28 of the container 22 is provided with a plurality of apertures 30, so that the whey to be converted can reach the interior of the container 22.
- These breakthroughs 30 may be stamped, for example, and it is advantageous if then the burrs protrude inwards.
- the lower end face 32 of the container may be closed, so that the inflow of the whey into the container 22 takes place substantially in the radial direction.
- the upper end face can also be closed. In the case where the upper surface is above the liquid level, sealing may be dispensed with.
- a replaceable filling body 24 is received, which, as shown in the elevational view, a spiral-shaped structure on has.
- this filling body 24 consists of a support 34, which may be, for example, a spirally turned stainless steel sheet.
- a foam material for example a PU foam
- the PU foam forms a pore system, the walls of which are coated with activated carbon, so that a large mass transfer area is provided.
- the carrier 34 consists of a two to three millimeters thick VA grid body, wherein the helical structure is formed by two grid surfaces, between which a semi-hard, open-cell PU foam is introduced with activated carbon coating.
- the arranged on the downward side of the helix bars 36 are provided with a photocatalytic surface, the mesh size is at these down facing large areas about 10 - 12 mm. At the the upwardly facing large area of the spiral forming bars is no coating provided.
- the mesh size here is about 25 to 30 mm.
- microorganisms and enzymes mentioned above can be introduced centrally via a dosing hose into the center of the spiral-shaped filling body 24.
- these microorganisms and enzymes with nanocomposite materials already in the production of the filler 24 in the pore system.
- Very promising have been experiments in which the microorganisms or enzymes and nanocomposite materials are dissolved in chitosan and this mixture added with the nano-composite materials is then applied to the filler, for example by impregnation, so that continuous feeding of microorganisms or enzymes deleted and only at regular intervals replacement of the filler 24 is required.
- the PU foam is coated in the embodiment shown here on the downwardly facing side of the helix with a gel-like material of chitosan.
- the nano-composite materials are embedded, each of which is a piezoelectric ceramic system of PZT Kr c Anlagenn with photocatalytic lytic coatings.
- microorganisms or lactase-producing Kluyveromyces yeasts are also embedded in the fermentation.
- the container 22 is coated both on its inner surface and on its outer surface with the photocatalytically active layer 26 - so for example, the titanium dioxide. This layer is completely applied to the inner surface, that is to say on the side facing the filler body 34, while on the outer surface the titanium dioxide is applied in the form of strips 26, between which regions which are provided with a diamond coating 38 remain.
- Such a diamond coating 38 can be produced synthetically by heating methane and hydrogen and a suitable carrier substance, for example niobium, silicon or ceramic, in a vacuum chamber to temperatures of up to approximately 2000 °. It then comes to a reaction in which a diamond lattice is formed on the carrier. This coating 38 is then applied to the outer wall 28 of the container 22, so that with a photocatalytically active 26 and provided with a diamond layer 38 areas adjacent to each other. These areas 26, 38 extend in the longitudinal direction of the container 22. In the illustrated embodiment, the width of the strips 26 corresponds approximately to the distance of four hole-shaped openings 30, while the width of the areas 38 is substantially smaller and approximately equal to the distance between two adjacent openings 30 ,
- FIG. 3 schematically shows a further embodiment of the present invention in which ethanol is obtained from whey.
- whey is introduced into an aerobic loop reactor 32 of the type already described above. If the whey is heavily loaded, the microbial mixture 33 described above can be added to the aerobic loop reactor of the whey.
- demineralization of the whey can take place in the loop reactor.
- potassium, but also salts, such as NaCl affect the fermentation and can sometimes hinder this strong.
- whey thus treated is then transferred to a buffer tank 34 in which whey is collected from the loop reactor to be available for further processing.
- whey can be brought together from a wide variety of dairies, so that advantageously also a stabilization of the whey takes place. It is particularly advantageous if a whey with a certain lactose content is present in the buffer container.
- the introduced whey can either be diluted or concentrated.
- the enzyme treatment and the breakdown of lactose and galactose into glucose has already been described above.
- the thus pretreated whey - actually now the glucose-containing fluid - is now transferred to a fermentation tank 37, in the fermentation yeast, which was preferably pretreated in a yeast fermenter 38, is added. After fermentation is carried out in another container 39, the yeast deposition in order to obtain ethanol in the purest possible form. Thereafter, the ethanol thus obtained is transferred to another container 40 in which the last residues of yeast and sugar are fermented to ethanol.
- a microbiotic mixture in particular a mixture of photosynthetic microorganisms and light-emitting microorganisms
Abstract
Description
Claims
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
EP10193564A EP2322639A1 (en) | 2006-03-09 | 2007-03-09 | Process for the production of ethanol from lactose-containing materials |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
DE102006010985 | 2006-03-09 | ||
PCT/DE2007/000434 WO2007101434A2 (en) | 2006-03-09 | 2007-03-09 | Extraction of fermentation-inhibiting substances from a fluid |
Publications (1)
Publication Number | Publication Date |
---|---|
EP1991687A2 true EP1991687A2 (en) | 2008-11-19 |
Family
ID=38323853
Family Applications (2)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP10193564A Withdrawn EP2322639A1 (en) | 2006-03-09 | 2007-03-09 | Process for the production of ethanol from lactose-containing materials |
EP07722009A Withdrawn EP1991687A2 (en) | 2006-03-09 | 2007-03-09 | Extraction of fermentation-inhibiting substances from a fluid |
Family Applications Before (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
EP10193564A Withdrawn EP2322639A1 (en) | 2006-03-09 | 2007-03-09 | Process for the production of ethanol from lactose-containing materials |
Country Status (3)
Country | Link |
---|---|
US (1) | US20090130256A1 (en) |
EP (2) | EP2322639A1 (en) |
WO (1) | WO2007101434A2 (en) |
Families Citing this family (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2008141631A1 (en) * | 2007-05-21 | 2008-11-27 | Georg Fritzmeier Gmbh & Co. Kg | Method and device for initiating conversion processes by magnetic fields and/or oxygen donators |
DE102010007559B4 (en) | 2010-02-10 | 2014-01-09 | Sartorius Stedim Biotech Gmbh | Bioreactor container with an optical foam sensor |
GB2481411A (en) * | 2010-06-22 | 2011-12-28 | Peter Sage-Passant | Waste disposal apparatus |
EP3467371A1 (en) * | 2017-10-04 | 2019-04-10 | Valeo Iluminacion | Lighting device |
CN114317341B (en) * | 2021-12-27 | 2024-01-09 | 宁波希诺亚海洋生物科技有限公司 | Vibrio harveyi variety capable of producing lactase and application thereof |
Family Cites Families (7)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US4004994A (en) * | 1972-07-12 | 1977-01-25 | Stauffer Chemical Company | Electrochemical removal of contaminants |
WO1985001064A1 (en) * | 1983-08-25 | 1985-03-14 | Munir Cheryan | Continuous fermentation process |
RU2036231C1 (en) * | 1992-09-24 | 1995-05-27 | Колодкин Александр Михайлович | Whey-base ferment for food ethanol production |
US20040044087A1 (en) * | 1999-03-05 | 2004-03-04 | Maye John Paul | Use of hop acids in fuel ethanol production |
EP1272613A1 (en) * | 2000-04-10 | 2003-01-08 | Midwest Research Institute | Method for the selective removal of fermentation inhibitors from biomass hydrolyzate |
DE10062812B4 (en) * | 2000-12-18 | 2009-07-09 | Georg Fritzmeier Gmbh & Co. Kg | Microbiological composition |
DE10361996A1 (en) | 2003-07-08 | 2005-02-24 | Umwelttechnik Georg Fritzmeier Gmbh & Co. | Bioreactor for communal/industrial sewage, in a small sewage processing plant, has a sieve body with a mixture of microorganisms containing photosynthesis and light-emitting organisms |
-
2007
- 2007-03-09 EP EP10193564A patent/EP2322639A1/en not_active Withdrawn
- 2007-03-09 US US12/282,284 patent/US20090130256A1/en not_active Abandoned
- 2007-03-09 WO PCT/DE2007/000434 patent/WO2007101434A2/en active Application Filing
- 2007-03-09 EP EP07722009A patent/EP1991687A2/en not_active Withdrawn
Non-Patent Citations (1)
Title |
---|
See references of WO2007101434A2 * |
Also Published As
Publication number | Publication date |
---|---|
EP2322639A1 (en) | 2011-05-18 |
WO2007101434A3 (en) | 2008-01-17 |
WO2007101434B1 (en) | 2008-03-27 |
US20090130256A1 (en) | 2009-05-21 |
WO2007101434A2 (en) | 2007-09-13 |
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