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US20160255862A1 - L-amino acid-containing feedstuff additive - Google Patents

L-amino acid-containing feedstuff additive Download PDF

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Publication number
US20160255862A1
US20160255862A1 US15/031,258 US201415031258A US2016255862A1 US 20160255862 A1 US20160255862 A1 US 20160255862A1 US 201415031258 A US201415031258 A US 201415031258A US 2016255862 A1 US2016255862 A1 US 2016255862A1
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Prior art keywords
weight
amino acid
fermentation broth
content
lysine
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Abandoned
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US15/031,258
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English (en)
Inventor
Ansgar Oelmann
Hans Christian Alt
Wilfried Blümke
Franz Ulrich Becker
Christopher John Conrad
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Evonik Operations GmbH
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Evonik Degussa GmbH
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Assigned to EVONIK DEGUSSA GMBH reassignment EVONIK DEGUSSA GMBH ASSIGNMENT OF ASSIGNORS INTEREST (SEE DOCUMENT FOR DETAILS). Assignors: BECKER, FRANZ ULRICH, OELMANN, ANSGAR, BLÜMKE, Wilfried, Conrad, Christopher John, ALT, HANS CHRISTIAN
Publication of US20160255862A1 publication Critical patent/US20160255862A1/en
Assigned to EVONIK OPERATIONS GMBH reassignment EVONIK OPERATIONS GMBH CHANGE OF NAME (SEE DOCUMENT FOR DETAILS). Assignors: EVONIK DEGUSSA GMBH
Abandoned legal-status Critical Current

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    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K20/00—Accessory food factors for animal feeding-stuffs
    • A23K20/10—Organic substances
    • A23K20/142—Amino acids; Derivatives thereof
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K10/00—Animal feeding-stuffs
    • A23K10/10—Animal feeding-stuffs obtained by microbiological or biochemical processes
    • A23K10/12—Animal feeding-stuffs obtained by microbiological or biochemical processes by fermentation of natural products, e.g. of vegetable material, animal waste material or biomass
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K20/00—Accessory food factors for animal feeding-stuffs
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K20/00—Accessory food factors for animal feeding-stuffs
    • A23K20/10—Organic substances
    • A23K20/158—Fatty acids; Fats; Products containing oils or fats
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K40/00—Shaping or working-up of animal feeding-stuffs
    • A23K40/10—Shaping or working-up of animal feeding-stuffs by agglomeration; by granulation, e.g. making powders
    • A—HUMAN NECESSITIES
    • A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23K—FODDER
    • A23K40/00—Shaping or working-up of animal feeding-stuffs
    • A23K40/30—Shaping or working-up of animal feeding-stuffs by encapsulating; by coating

Definitions

  • the invention relates to fermentation broth-based feed additives containing L-amino acid, which comprise a surface-active substance, and also a granulation process for preparing these feed additives.
  • L-lysine monohydrochloride L-lysine monohydrochloride
  • L-lysine content ca. 80%. Since L-lysine is produced by fermentation, it must, to prepare the monohydrochloride, first and foremost be separated in complicated method steps from all remaining constituents of the crude fermentation broth, then converted to the monohydrochloride, and the latter must be crystallized. This generates a large number of by-products and the reagents required for processing in the form of waste.
  • EP 0 533 039 relates to methods for preparing a fermentation broth-based amino acid animal feed supplement, wherein the supplement may be obtained directly from the fermentation broth by means of spray-drying. In one variant, some of the biomass in this case is removed before the spray-drying step.
  • EP 0 615 693 discloses a method for preparing a fermentation broth-based animal feed additive, in which the fermentation broth, optionally after removal of some of the constituents, is spray-dried to give fine particles of which at least 70% by weight have a maximum particle size of 100 ⁇ m, and furthermore these fine particles are enlarged in a second stage to give granules comprising the fine particles at not less than 30% by weight.
  • a concentrate containing L-lysine is prepared from a fermentation broth, which, before concentration, is acidified with HCl to a pH of ca. 6.4 and to which bisulphite is added for stabilization purposes. After the evaporation, the product is further acidified to a pH of 4.0 and the desired product is obtained by spray-drying.
  • additives in the further processing is described in GB 2 293 304 A, such as the spraying of aerosols of mineral oils for suppression of dust formation.
  • WO 2004/054381 describes the preparation of a lysine-containing feedstuff, based on fermentation broth, and the addition of additives in the processing, wherein the addition of mineral oils, vegetable oils or mixtures of vegetable oils, particularly soybean oil, olive oil and mixtures of soybean oil with lecithin are mentioned which influence the abrasion of the granules and the dust formation.
  • a disadvantage of such granulated products is generally the low subsequent bulk density of the granulate which cannot be influenced, which results in disadvantages in packing volume and related increased transport costs.
  • the object of the invention is achieved by the addition of a surface-active component to the fermentation broth before carrying out the spray-drying, namely that a comparatively high bulk density of the product may be achieved and at the same time the granulation properties can be improved.
  • the improved granulation properties observed particularly consist of low residual moisture content at high spray rates and low granulation temperatures can be achieved by the addition of the surface-active component to the fermentation broth before carrying out the spray-drying, which enables more rapid and at the same time more energy-efficient granule production.
  • the comparatively high bulk density of the product is a result of fewer cavities and a more compact structure of the granulate, as cross sections of the granulate show.
  • the present invention therefore provides a method for preparing a fermentation broth-based feed additive containing L-amino acid, characterized in that a fermentation broth containing L-amino acid, which has a water content of 35 to 75% by weight and a content of surface-active substance of 0.025 to 20% by weight, is converted by drying into a particulate composition.
  • the present invention also relates to a method for preparing a fermentation broth-based feed additive containing L-amino acid, comprising the following steps:
  • the fermentation broth containing L-amino acid is preferably obtained by fermentation of an L-amino acid-producing microorganism in an aqueous culture medium under aerobic conditions. Preferred fermentation methods according to the invention are further illustrated in detail below.
  • Fermentation broth is understood to mean a fermentation medium in which a microorganism has been cultivated for a certain time and at a certain temperature.
  • the fermentation medium or the media used during the fermentation comprises/comprise all of the substances or components which ensure proliferation of the microorganism and formation of the desired amino acid.
  • the cells of the microorganism e.g. coryneformes bacterium
  • L-amino acid particularly L-lysine
  • Organic by-products include substances which are generated, if applicable, in addition to the target product, from the microorganisms used in the fermentation and are optionally separated. These include other L-amino acids which, compared to the desired L-amino acid (particularly L-lysine), account for less than 30%, 20% or 10%. These further include organic acids which bear one to three carboxyl groups such as acetic acid, lactic acid, citric acid, malic acid or fumaric acid. Finally, sugars such as trehalose are also included here.
  • Suitable fermentation broths for industrial purposes typically have an L-amino acid content (particularly L-lysine content) of 40 g/kg to 180 g/kg or 50 g/kg to 150 g/kg.
  • the biomass content (as dried biomass) in the fermentation broth is generally 20 to 50 g/kg, but in low biomass fermentation the biomass content can also be below this level.
  • the fermentation broth preferably comprises an L-amino acid selected from L-lysine, L-methionine, L-threonine, L-valine or L-tryptophan.
  • the fermentation broth particularly preferably comprises the L-amino acid L-lysine.
  • the L-amino acid is L-lysine
  • the method comprises an additional method step, which is carried out before the start of the drying, in which ammonium sulphate and/or sulphuric acid is added to the fermentation broth, in order to establish a sulphate/L-amino acid ratio of at least 0.5, preferably 0.85 to 1.2.
  • the fermentation broth in a preferred embodiment according to the invention is the direct product of a fermentation process using L-amino acid-producing bacteria.
  • the biomass can, however, optionally be partially or completely removed from the fermentation broth before or after addition of the surface-active component.
  • at most 80% by weight, particularly preferably at most 50% by weight, in particular at most 30, 20 or 10% by weight of the biomass is removed before carrying out the drying to give a particulate composition.
  • the entire biomass remains present in the fermentation broth.
  • the biomass may be removed, if desired, particularly by centrifugation, filtration or decanting or by combinations of these methods.
  • the biomass is removed by ultrafiltration.
  • the organic by-products dissolved in the fermentation broth and the dissolved constituents of the fermentation medium (ingredients) which are not consumed remain at least in part in the product (>0% by weight), at preferably not less than 25% by weight, particularly preferably not less than 50% by weight and very particularly preferably not less than 75% by weight. Optionally, these also remain entirely (100% by weight) or virtually entirely, i.e. >95% by weight or >98% by weight, in the product.
  • “fermentation broth-based” means that the product comprises at least some of the constituents of the fermentation broth.
  • the fermentation broth used according to the invention preferably has the following properties on completion of the fermentation:
  • biomass content of 1 to 5% by weight, preferably 2 to 4.5% by weight, particularly preferably 2.5 to 3.5% by weight
  • L-amino acid content preferably L-lysine, (as amino acid base) of 5 to 20% by weight
  • solids content including biomass
  • sulphate to L-amino acid, particularly L-lysine, of 0.8 to 1.2
  • pH 3.5 to 7.0, preferably 4.0 to 5.0.
  • Solids content in accordance with the invention is understood to mean the mass which remains on complete removal of the liquid. This dry mass also includes, in addition to suspended substances if applicable (such as the biomass), dissolved substances which only crystallize out or precipitate on drying. The solids content is in this respect complementary to the water or moisture content.
  • the fermentation broth used in accordance with the invention can optionally already contain a sufficient amount of surface-active substance after completion of the fermentation. This may be achieved by adding a sufficient amount of surface-active substance to the fermentation medium already before the start of the fermentation or by adding appropriate surface-active substance during the fermentation.
  • the fermentation broth does not comprise, or only comprises a relatively low amount of surface-active substance after completion of the fermentation.
  • the surface-active substance or the majority of the surface-active substance is accordingly added to the fermentation broth after completion of the fermentation.
  • the surface-active substance which is already present in the fermentation broth after completion of the fermentation may be, for example, an antifoaming agent.
  • the fermentation broth Before the start of the drying, the fermentation broth preferably has a water content of 35 to 70% by weight, particularly preferably 35 to 50% by weight. This water content may be adjusted, if required, particularly by evaporation of the fermentation broth, for example by means of a rotary evaporator, a thin film evaporator or a falling film evaporator, by reverse osmosis or by nanofiltration.
  • the biomass content, the L-amino acid content and the solids content in the fermentation broth also increase accordingly during the concentration.
  • the “surface-active substance” in the context of the present application can be a pure substance which consists exclusively of a surface-active compound. However, it may also be a mixture of different surface-active compounds.
  • “surface-active substance” is however also understood to mean a component comprising a surface-active compound or a mixture of different surface-active compounds in a significant quantity.
  • the surface-active compound(s) is/are present in the component in this case preferably in an amount of at least 3% by weight, particularly at least 5% by weight, particularly preferably at least 10% by weight.
  • the surface-active compound(s) is/are present in the component at not less than 20% by weight, preferably not less than 25% by weight, particularly not less than 40% by weight.
  • the surface-active substance in accordance with the invention is preferably selected from the group consisting of corn steep liquor, lipids, antifoaming agents and surfactants and also mixtures thereof.
  • the antifoaming agent is preferably selected from polysiloxane derivatives, mono- and polyglycols, phospholipids and fatty acid glycerides.
  • the polysiloxane derivative can take in particular the form of a polyalkylsiloxane, especially a polydimethylsiloxane.
  • the polyglycol is preferably a polymer composed of oxyethylene and/or oxypropylene units, preferably a copolymer of oxyethylene and oxypropylene units, or is a compound comprising oxyethylene and/or oxypropylene units, such as a fatty acid alkylpolyglycol ester.
  • the phospholipid is preferably a phosphatidylcholine (lecithin).
  • the fatty acid glyceride may particularly take the form of a mono- or diglyceride, especially a mono- or diglyceride in which the acid residue is selected from acetic acid, lactic acid, citric acid, tartaric acid and mixtures thereof.
  • the corn steep liquor used according to the invention preferably has a dry mass of at least 40% by weight, preferably 45 to 55% by weight, and preferably has a residual sugar content of at most 2% by weight.
  • Corn steep liquor comprises phosphatidylcholine as surface-active constituent.
  • the lipid which may be used in accordance with the invention is preferably selected from mineral oils, vegetable oils and mixtures thereof.
  • the oil used is particularly preferably soybean oil, olive oil, silicone oil or mixtures thereof.
  • the surface-active substance used is phosphatidylcholine or a component containing phosphatidylcholine, preferably corn steep liquor.
  • the surface-active substance in the fermentation broth before the start of the drying is preferably present in an amount of 0.025 to 20% by weight, 0.1 to 20% by weight, 0.2 to 20% by weight, 0.5 to 20% by weight or 1 to 20% by weight. Preferred ranges here are 0.2 to 15% by weight, 0.3 to 15% by weight, 0.5 to 15% by weight and 1 to 10% by weight.
  • a concentration of surface-active substance is preferably set to 0.1 to 5% by weight, particularly 0.2 to 4% by weight, preferably 0.25 to 2% by weight.
  • the surface-active substance is a component which comprises at least 50% by weight, particularly at least 70% by weight, of surface-active compounds.
  • a concentration of surface-active substance is preferably set to 0.1 to 10% by weight, particularly 0.5 to 5% by weight, preferably 1 to 3% by weight.
  • the surface-active substance is a component which comprises less than 30% by weight, particularly 3 to 30% or 3 to 20% by weight, of surface-active compounds.
  • the fermentation broth before the start of the drying has the following properties:
  • biomass content of 2 to 12% by weight, preferably 3 to 10% by weight, particularly 4 to 8% by weight
  • L-amino acid content preferably L-lysine, (as amino acid base) of 12 to 48% by weight, particularly 20 to 40% by weight
  • solids content including biomass
  • surface-active substance content of 0.025 to 20% by weight, particularly 0.1 to 20% by weight, preferably 0.3 to 15% by weight
  • pH 3.5 to 7.0, preferably 4.0 to 5.0.
  • an additive may be added to the fermentation broth provided or to the concentrated fermentation broth, depending on requirements, in order to increase or decrease the L-amino acid content.
  • the additive may also alternatively and/or additionally be added during the drying or granulation process.
  • the relevant L-amino acid is preferably added in the form of a concentrate, or optionally as a largely pure substance or salt thereof, in liquid or solid form.
  • ammonium sulphate is preferably added.
  • the additive if used, is preferably added to the fermentation broth in an amount of 0.1 to 10% by weight, preferably 0.1 to 5% by weight, or is preferably added in an amount that adjusts the L-amino acid concentration in the final product to 40 to 60% by weight, particularly 45 to 55% by weight.
  • the drying may be carried out particularly by freeze-drying, preferably by a spray process, particularly spray-drying or spray granulation.
  • further processing steps may follow the drying of the fermentation broth performed according to the invention, in particular, one or more granulation steps, particularly if a granulate is not obtained directly from the drying process.
  • the fermentation broth is converted directly into a granulate in one process step, such that a subsequent granulation is not necessary.
  • the direct conversion into a granulate is preferably carried out by a spray granulation method, particularly preferably by application of a spray granulation method using a circulating fluidized bed as described in patent application WO 2005/006875.
  • dust formed downstream of the granulation is preferably completely or at least partially recirculated into the spray granulation chamber.
  • the granulation temperature is preferably regulated such that the inlet temperature is 200 to 300° C., preferably 250 to 275° C. and the outlet temperature is 60 to 100° C., preferably 70 to 90° C.
  • the granulate obtainable preferably has an L-amino acid content of 40 to 60% by weight, particularly 45 to 55% by weight, particularly preferably 48 to 52% by weight, and a water content (residual moisture content) of at most 5% by weight, preferably at most 3.5% by weight.
  • a particulate composition is obtained by means of the drying process which is preferably free-flowing and also can be fine-grained or coarse-grained.
  • the free-flowing, fine-grained powder may in turn be converted into a coarse-grained, free-flowing and largely dust-free product, which can be stored, by suitable compacting or granulating processes.
  • the granulates may be prepared, for example, by the methods according to EP-B 0 615 693 or EP-B 0 809 940, U.S. Pat. No. 5,840,358 or WO 2005/006875 or WO 2004/054381.
  • Free-flowing is understood to mean powders which flow out unhindered from a series of glass efflux vessels having different size outflow openings at least from a vessel having a 5 mm (millimetre) opening (Klein: Seifen, Ole, Fette, Wachse 94, 12 (1968)).
  • the present invention further relates to a feed additive containing a preferably granular L-amino acid, particularly L-lysine, which is obtainable by a method according to the invention.
  • the present invention further relates to granular feed additives comprising the following features:
  • L-amino acid content preferably L-lysine, (calculated as the amino acid base) of at least 20% by weight, preferably 25 to 60% by weight, particularly 30 to 60 or 40 to 60% by weight, particularly preferably 45 to 55% by weight
  • biomass content of at least 3 or 4% by weight, preferably at least 5 or 6% by weight, particularly preferably at least 7% by weight, particularly 3 to 12% by weight, 4 to 12% by weight, 5 to 12% by weight, 6 to 12% by weight or 7 to 12% by weight
  • surface-active substance content of 0.04 to 35% by weight, preferably 0.15 to 30% by weight, particularly preferably 0.5 to 15% by weight
  • the stated mean particle diameter here refers to the arithmetic mean.
  • the proportion of dust i.e.
  • particles having a particle size ⁇ 63 ⁇ m is preferably 20% by weight or less, 15% by weight or less, 10% by weight or less, 5% by weight or less, 3% by weight or less, 2% by weight, 0 to 1% by weight, 0.5% by weight or less.
  • At least 75% by weight of the particles of the composition obtained particularly preferably have a particle diameter of >63 ⁇ m to ⁇ 2500 ⁇ m, preferably >63 ⁇ m to ⁇ 2000 ⁇ m, wherein the proportion of the particles having a particle diameter of ⁇ 63 ⁇ m is preferably 20% by weight or less.
  • the bulk density of the preferred products is generally 600 to 800 kg/m 3 .
  • the particle size distribution is preferably measured by sieve analysis in a Hosokawa Alpine air jet sieving machine, Type 200 LS-N (sieve set: mesh sizes 20, 32, 45, 63, 100, 150, 200, 250, 280, 300, 400, 500, 600, 630, 710, 800, 1000, 1180, 1400, 1600 and 2000 ⁇ m; sieving time: 3 min.).
  • the particle size may also be determined for example by laser diffraction spectrometry. Possible methods are described in the text book “Teilchengrö ⁇ entown in der Laborpraxis” [Particle size measurement in the laboratory] by R. H. Müller and R. Schuhmann,ticianliche Verlagsgesellschaft Stuttgart (1996) and in the text book “Introduction to Particle Technology” by M. Rhodes, Wiley & Sons (1998).
  • auxiliaries or carriers such as starch, gelatin, cellulose derivatives or similar substances, which are used in food or feed processing as binding agents, gelling agents or thickeners, or other substances such as silicas, silicates (EP-A 0 743 016) or stearates.
  • a product with the desired particle size is optionally obtained from the resulting particulate composition or resulting granulate by sieving, rolling, dust separation, grinding or combinations thereof.
  • Granular feed additives according to the invention are preferably further characterized in that they are coated with an oil, as described in WO 04/054381 for example, wherein the oil is preferably selected from vegetable oil (particularly olive oil, sunflower oil, soybean oil or soybean oil/lecithin mixtures), animal oil or fat and oil obtained from microorganisms by fermentation.
  • an oil is preferably selected from vegetable oil (particularly olive oil, sunflower oil, soybean oil or soybean oil/lecithin mixtures), animal oil or fat and oil obtained from microorganisms by fermentation.
  • the product may also be applied to a customary organic or inorganic support material known in feed processing, such as silicas, silicates, meals, brans, starches, sugars or others and/or be mixed and stabilized with customary thickeners or binders.
  • silicas, silicates, meals, brans, starches, sugars or others and/or be mixed and stabilized with customary thickeners or binders. Examples of applications and methods for this purpose are described in the literature (Die Mühle+Mischfuttertechnik [Milling and compound feed technology] 132 (1995) 49, page 817).
  • the product may also be finished by a coating process with film formers such as metal carbonates, silicas, silicates, alginates, stearates, starches, rubbers and cellulose ethers as described in DE-C 41 00 920.
  • film formers such as metal carbonates, silicas, silicates, alginates, stearates, starches, rubbers and cellulose ethers as described in DE-C 41 00 920.
  • the biomass in feed additives according to the invention preferably comprises bacteria of the genus Corynebacterium or the genus Escherichia and/or cell debris from these bacteria and particularly preferably consists largely of these.
  • the L-amino acid content in feed additives according to the invention is preferably at least 30% by weight, preferably at least 40% by weight, particularly 40 to 60% by weight, particularly preferably 45 to 55% by weight.
  • the L-amino acid in the feed additives according to the invention is preferably selected from the group consisting of L-lysine, L-methionine, L-threonine, L-tryptophan and L-valine and also mixtures thereof; particularly preferably the L-amino acid is L-lysine.
  • the feed additive according to the invention preferably takes the form of a fermentation broth-based feed additive.
  • the surface-active substance present in granular feed additives according to the invention is preferably selected from the surface-active substances mentioned above.
  • the surface-active substance is a polyglycol, particularly a fatty acid alkylpolyglycol ester, or a phospholipid, particularly a lecithin, or mixtures thereof
  • the surface-active substance in the feed additive is preferably present in an amount of 0.15 to 10% by weight, particularly 0.3 to 6% by weight, particularly preferably 0.4 to 4% by weight.
  • the surface-active substance is a component which comprises at least 50% by weight, particularly at least 70% by weight, of surface-active compounds.
  • the surface-active substance is corn steep liquor, optionally in combination with other surface-active substances, the surface-active substance in the feed additive is preferably present in an amount of 3 to 25% by weight, particularly preferably 6 to 20% by weight.
  • the surface-active substance is a component which comprises less than 30% by weight, particularly 3 to 30% or 3 to 20% by weight, of surface-active substance.
  • the distribution of surface-active substance in the particle is preferably homogeneous, wherein “homogeneous” is understood to mean that no major difference in concentration of the surface-active substance is found between any two fractions of the particle.
  • the deviation in the amount of surface-active substance in any two fractions of the particle is preferably at most 30%, preferably at most 25 or 20%, particularly preferably at most 10, 5 or 3%.
  • the homogeneous distribution of the surface-active substance is ensured by the manner of preparation of the feed additive.
  • the particle density of the feed additive is preferably at least 1.138 g/cm 3 , particularly preferably at least 1.140 g/cm 3 , especially preferably at least 1.142 or 1.144 g/cm 3 .
  • Preferred ranges in this context are 1.138 to 1.160 g/cm 3 , particularly 1.140 to 1.155 g/cm 3 , especially 1.142 to 1.154 g/cm 3 or 1.144 to 1.152 g/cm 3 .
  • the bulk density of the feed additive is preferably at least 600 kg/m 3 , particularly 600 to 800 kg/m 3 .
  • the bulk density is preferably determined as follows: An empty measuring cylinder (250 ml volume) is placed on a balance, filled with the granular product and the weight per unit volume is then determined.
  • the void spaces in the measuring cylinder are filled with methanol.
  • the void volumes can thus be determined by the increase in weight and the known density of methanol (0.7918 g/ml). The difference between total volume and the volume of the methanol gives the particle volume.
  • the particle density is then obtained, by basing the weight of the particle previously determined not on the total volume of the measuring cylinder but on the particle volume determined.
  • the particle density can also be determined using a pycnometer.
  • the particle density is determined in this case by gas displacement. Inert gases such as helium or nitrogen are preferably used as displacement medium.
  • Granular feed additives according to the invention are preferably characterized in that they comprise the L-amino acid L-lysine, wherein said L-amino acid is preferably present at least in part as a sulphate salt, in which the molar ratio of sulphate to L-lysine is preferably at least 0.5, particularly preferably 0.8 to 1.2.
  • feed additives according to the invention preferably have a pH of 3.5 to 6.5, particularly 4.0 to 5.0, preferably 4.2 to 4.8, measured in aqueous suspension.
  • a 10% by weight suspension in deionized water is prepared and the pH measured with a pH electrode at 25° C. The measured value becomes constant after ca. 1 minute.
  • the water content of the feed additive according to the invention is preferably between 0.1% by weight and no more than 5% by weight.
  • the water content is preferably at most 4% by weight, particularly preferably at most 3% by weight and especially preferably at most 2.5% by weight. Water contents of at most 2% by weight are also possible.
  • Feed additives according to the invention are further preferably characterized in that they have a very compact structure, wherein “compact structure” is understood to mean that they have relatively few cavities. This is not least as a result of the use of the surface-active substance. Feed additives according to the invention are preferably characterized in that they have cavities less than 25% by volume, particularly less than 20% by volume, particularly preferably less than 15% by volume, especially preferably less than 10% by volume.
  • the present invention further relates to the use of a granular feed additive according to the invention for preparing feedstuff.
  • the preparation by fermentation of L-amino acids such as L-lysine, L-methionine, L-threonine, L-tryptophan, L-valine, particularly L-lysine, is achieved by cultivation by fermentation of an amino acid-overproducing bacterial strain.
  • the fermentation is preferably conducted with coryneform bacteria, particularly from the genus Corynebacterium , particularly preferably of the type Corynebacterium glutamicum , and/or from the genus Escherichia , particularly preferably of the type Escherichia coli , by a so-called fed-batch process (feed processes).
  • the fermentation can also be carried out continuously or batchwise in a batch process (batch cultivation) or repeated fed batch process (repetitive feed process) with the aim to produce L-amino acids (particularly L-lysine).
  • the fermentation medium used is optimized according to the requirements of the respective production strain.
  • a general review of known cultivation methods is available in the textbook by Chmiel (Bioreaktoren and periphere bamboo [Bioreactors and Peripheral Devices] (Vieweg Verlag, Braunschweig/Wiesbaden, 1994)).
  • the culture medium or fermentation medium to be used has to satisfy the demands of the particular strains in a suitable manner. Descriptions of culture media of different microorganisms are present in the handbook “Manual of Methods for General Bacteriology”, of the American Society for Bacteriology (Washington D. C, USA, 1981). The terms culture medium and fermentation medium or medium are mutually interchangeable.
  • the carbon sources used may be sugars and carbohydrates such as glucose, sucrose, lactose, fructose, maltose, molasses, sucrose-containing solutions from sugarbeet or sugarcane production, starch, starch hydrolysate and cellulose, oils and fats such as soybean oil, sunflower oil, groundnut oil and coconut fat, fatty acids such as palmitic acid, stearic acid and linoleic acid, alcohols such as glycerol, methanol and ethanol and organic acids such as acetic acid. These substances may be used individually or as a mixture.
  • sugars and carbohydrates such as glucose, sucrose, lactose, fructose, maltose, molasses, sucrose-containing solutions from sugarbeet or sugarcane production, starch, starch hydrolysate and cellulose, oils and fats such as soybean oil, sunflower oil, groundnut oil and coconut fat, fatty acids such as palmitic acid, stearic acid and linoleic acid, alcohols
  • the nitrogen sources used may be organic nitrogen compounds such as peptones, yeast extract, meat extract, malt extract, corn steep liquor, soybean meal and urea or inorganic compounds such as ammonia, ammonium sulphate, ammonium phosphate, ammonium carbonate and ammonium nitrate, preferably ammonia or ammonium sulphate.
  • the nitrogen sources may be used individually or as a mixture.
  • the phosphorus sources used may be phosphoric acid, potassium dihydrogen phosphate or dipotassium hydrogen phosphate or the corresponding sodium salts.
  • the culture medium must additionally contain salts, for example in the form of sulphates of metals such as sodium, potassium, magnesium, calcium and iron, for example magnesium sulphate or iron sulphate, which are needed for growth.
  • salts for example in the form of sulphates of metals such as sodium, potassium, magnesium, calcium and iron, for example magnesium sulphate or iron sulphate, which are needed for growth.
  • essential growth factors such as amino acids, for example homoserine, and vitamins, for example thiamine, biotin or pantothenic acid, may be used in addition to the substances mentioned above.
  • suitable precursors of the particular amino acid can be added to the culture medium.
  • the feedstocks mentioned may be added to the culture in the form of a single mixture or may be fed in during the cultivation in a suitable manner.
  • pH control of the culture basic compounds such as sodium hydroxide, potassium hydroxide, ammonia or aqueous ammonia, preferably ammonia or aqueous ammonia, or acidic compounds such as phosphoric acid or sulphuric acid, are used in a suitable manner.
  • the pH is generally adjusted to a value of 6.0 to 9.0, preferably 6.5 to 8.
  • antifoams for example fatty acid polyglycol esters.
  • suitable selective substances for example antibiotics, can be added to the medium.
  • oxygen or oxygenous gas mixtures for example air, are introduced into the culture.
  • liquids enriched with hydrogen peroxide is likewise possible.
  • the fermentation is conducted at elevated pressure, for example at a pressure of 0.03 to 0.2 MPa.
  • the temperature of the culture is normally 20° C. to 45° C. and preferably 25° C. to 40° C.
  • the cultivation is continued until a maximum of the desired amino acid has formed. This aim is normally achieved within 10 hours to 160 hours. In continuous processes, longer cultivation times are possible.
  • a plurality of upstream growth fermenter steps with successively increasing fermenter volumes are necessary.
  • Examples of suitable fermentation media are found, inter alia, in the patent specifications U.S. Pat. No. 5,770,409, U.S. Pat. No. 5,840,551 and U.S. Pat. No. 5,990,350, U.S. Pat. No. 5,275,940 or U.S. Pat. No. 4,275,157. Further examples of fermentation media are found in Ozaki and Shiio (Agricultural and Biological Chemistry 47(7), 1569-1576, 1983) and Shiio et al. (Agricultural and Biological Chemistry 48(6), 1551-1558, 1984). Methods for determining L-lysine and other L-amino acids are known from the prior art. The analysis can proceed, for example, as described in Spackman et al.
  • the fermentation broth thus produced is subsequently processed in accordance with the invention.
  • the biomass or the fermentation broth comprising the biomass is preferably thermally inactivated during a suitable method step before the biomass is completely or partially removed.
  • an additional process step is preferably carried out, as already mentioned previously, which is carried out before the start of the drying process, in which ammonium sulphate and/or sulphuric acid are added to the fermentation broth, in order to establish a molar ratio of sulphate/L-amino acid of at least 0.5.
  • the molar ratio of sulphate/L-lysine is preferably in this case at least 0.6, 0.8, 0.9 or 0.95, particularly 0.85 to 1.2, preferably 0.9 to 1.1, particularly preferably >0.95 to ⁇ 1.1.
  • the broth may also be used preferably with sodium bisulphite (sodium hydrogensulphite) or another salt, for example ammonium, alkali metal or alkaline earth metal salt of sulphurous acid, which leads to stabilization and brightening of the product.
  • sodium bisulphite sodium hydrogensulphite
  • another salt for example ammonium, alkali metal or alkaline earth metal salt of sulphurous acid, which leads to stabilization and brightening of the product.
  • a particularly preferred method according to the invention comprises the following steps:
  • a surface-active component such that a content of surface-active component of 0.025 to 20% by weight, particularly 0.1 to 20% by weight, preferably 0.2 to 15% by weight, particularly preferably 0.3 to 10% by weight, is set;
  • Sulphate-containing compounds in the context of the method steps mentioned above particularly relate to ammonium sulphate and sulphuric acid.
  • a product is obtained with an L-amino acid content (particularly L-lysine) of 10 to 70% by weight (calculated as amino acid, based on the total amount) and in the case that the L-amino acid is L-lysine, L-lysine is present in a molar ratio of sulphate/L-lysine of at least 0.5, preferably 0.6, 0.8, 0.9, 0.95, 1.0, 1.05, 1.1, 1.2, more preferably 0.85 to 1.2, preferably 0.9 to 1.1, particularly preferably >0.95 to ⁇ 1.1.
  • one or more of the salts of sulphurous acid (sulphites), selected from the group consisting of ammonium salt, alkali metal salt, and alkaline earth metal salt, is added to the fermentation broth in an amount of 0.01 to 0.5% by weight, preferably 0.1 to 0.3% by weight, particularly preferably 0.1 to 0.2% by weight, based on the fermentation broth.
  • sulphurous acid selected from the group consisting of ammonium salt, alkali metal salt, and alkaline earth metal salt
  • the sulphites are preferably added as a solution before concentrating the fermentation broth.
  • the amount used is preferably considered when adjusting the sulphate/L-amino acid ratio.
  • FIGS. 1 a and 1 b A cross section of granulate embedded in synthetic resin is shown in FIGS. 1 a and 1 b , which was obtained from the fermentation broth without addition of a surface-active substance ( FIG. 1 a ) compared to a cross section of a granulate to which corn steep liquor had been added before carrying out the spray granulation ( FIG. 1 b ). Distinct cavities are visible in FIG. 1 a , while the granulate in FIG. 1 b has a more compact structure without visible cavities.
  • the laboratory experiments were conducted in a laboratory granulator.
  • the laboratory granulator operates with a fluidized bed.
  • the fermentation broth containing lysine is sprayed into the reactor from above.
  • the fluidized bed supply air may be adjusted in amount and temperature by controllable blower speeds and electrical heating.
  • the air flow is adjusted such that a well-mixed fluidized bed is achieved.
  • the spray nozzle is a pneumatic dual component nozzle.
  • the atomizing air pressure was adjusted to 0.5 bar in each experiment.
  • the broth was preheated to 60° C. and conveyed by means of a peristaltic pump with variable speed settings.
  • the fermentation broth containing lysine was evaporated to a water content of ca. 40% by weight before the spray-drying process and the surface-active substance was subsequently added.
  • the primary fluidized bed was generated, in which seeds were charged, which were removed from the production and were sieved to a particle size of 200 to 710 ⁇ m.
  • the particle density was selected as target parameter, since a good correlation was established between production and laboratory and a direct dependency of the particle size on the bulk density could be detected.
  • the bulk density was determined as follows: An empty measuring cylinder (250 ml volume) was placed on a balance, filled with the granular product and the weight per unit volume was then determined.
  • the void spaces in the measuring cylinder were filled with methanol.
  • the void volumes could thus be determined by the increase in weight and the known density of methanol (0.7918 g/ml). The difference between total volume and the volume of the methanol gives the particle volume.
  • the particle density is then obtained, by basing the weight of the particle previously determined not on the total volume of the measuring cylinder but on the particle volume determined.
  • the particle density can also be determined using a pycnometer.
  • Fermentation broth containing lysine sulphate was evaporated to a water content of ca. 40% by weight.
  • the fermentation broth provided in this manner already comprised 0.13% by weight of antifoaming agent CLEROL FBA 975-US.
  • the fermentation broth was then treated with various amounts of the fatty acid alkylpolyglycol ester (CLEROL FBA 975-US) and was then converted into a granulate using a laboratory granulator.
  • the concentrated fermentation broth was subjected to spray granulation without subsequent addition of the fatty acid alkylpolyglycol ester as comparative example.
  • the influence of the subsequent addition of the fatty acid alkylpolyglycol ester on the particle density can be seen in the following table.
  • Fermentation broth containing lysine sulphate was evaporated to a water content of ca. 40% by weight.
  • the fermentation broth provided in this manner already comprised 0.13% by weight of antifoaming agent CLEROL FBA 975-US.
  • the fermentation broth was then treated with various amounts of lipid-containing components.
  • the lipid-containing components used were lecithin (Aquagran CP 100) and also corn steep liquor (“CSL”), which contains lecithin.
  • the fermentation broth was subsequently processed to a granulate in the spray granulation process.
  • the concentrated fermentation broth was used in the spray granulation without subsequent addition of lipid-containing components as comparative example. The results are shown in the following table.
  • the fermentation medium was first concentrated after completion of the fermentation to a water content of ca. 40% by weight. Corn steep liquor was then added in an amount of ca. 8% by weight. Corn steep liquor was omitted in the corresponding comparative experiment.
  • the bulk density is significantly increased by addition of corn steep liquor prior to the spray granulation.

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US10531679B2 (en) * 2013-07-16 2020-01-14 Evonik Degussa, GmbH Method for drying biomass
US10619175B2 (en) 2014-10-02 2020-04-14 Evonik Operations Gmbh Process for producing a PUFA-containing feedstuff by extruding a PUFA-containing biomass
US10842174B2 (en) 2014-10-02 2020-11-24 Evonik Operations Gmbh Method for producing biomass which has a high exopolysaccharide content
US11076616B2 (en) 2013-10-24 2021-08-03 Evonik Operations Gmbh L-amino acid-containing feedstuff additive
US20220030914A1 (en) * 2018-12-07 2022-02-03 Cj Cheiljedang Corporation Granular feed additive
US11324234B2 (en) 2014-10-02 2022-05-10 Evonik Operations Gmbh Method for raising animals
US11464244B2 (en) 2014-10-02 2022-10-11 Evonik Operations Gmbh Feedstuff of high abrasion resistance and good stability in water, containing PUFAs

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KR20250001187A (ko) * 2023-06-28 2025-01-06 씨제이제일제당 (주) pH 조절 및 PVA 첨가를 이용한 L-발린 결정 및/또는 과립의 제조방법

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US11464244B2 (en) 2014-10-02 2022-10-11 Evonik Operations Gmbh Feedstuff of high abrasion resistance and good stability in water, containing PUFAs
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