MXPA98010678A - Process to manufacture granu l-lysine forage supplements - Google Patents

Process to manufacture granu l-lysine forage supplements

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Publication number
MXPA98010678A
MXPA98010678A MXPA/A/1998/010678A MX9810678A MXPA98010678A MX PA98010678 A MXPA98010678 A MX PA98010678A MX 9810678 A MX9810678 A MX 9810678A MX PA98010678 A MXPA98010678 A MX PA98010678A
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MX
Mexico
Prior art keywords
lysine
broth
percent
measured
drying
Prior art date
Application number
MXPA/A/1998/010678A
Other languages
Spanish (es)
Inventor
Michael Stevens Joseph
P Binder Thomas
Original Assignee
Archer Daniels Midland Company
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Filing date
Publication date
Application filed by Archer Daniels Midland Company filed Critical Archer Daniels Midland Company
Publication of MXPA98010678A publication Critical patent/MXPA98010678A/en

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Abstract

The present invention relates to a process that produces a forage supplement of L-Lysine with a final L-Lysine purity in the theoretical range of between about 35% and 80%, measured as a percent of the free base per Kg, and more preferably between about 50% and 80% L-Lysine. The process comprises adding a material containing L-Lysine to a L-Lysine fermentation broth or to a fraction of a L-Lysine fermentation broth. The aggregate material is in an amount, which leads to a final L-Lysine forage supplement with a purity of L-Lysine in a theoretical range of between about 35% and 80%, measured as per one percent of the free base per Kg, and more preferably between about 50% and 80% L-Lysine. The fraction of the L-Lysin fermentation broth is obtained by any suitable separation means such as ultrafiltration or centrifugation. The process also comprises the drying step which may involve any suitable drying means such as a spray granulator, spray dryer, tray dryer, drum dryer, rotary dryer, and tuna dryer.

Description

PROCESS FOR MANUFACTURING GRANULAR L-LYSINE FORAGE SUPPLEMENTS This invention relates to a process for producing a forage supplement of granular L-Lysine derived from fermentation broth of L-Lysine, and more particularly, with the production of a forage supplement of L-Lysine in which the L-Lysine content does not depend solely on the initial concentration of L-Lysine in the L-Lysine fermentation broth.
Background of the Invention Lysine is an amino acid widely used in the animal feed industry. The main form of which is L-Lysine HCl (L-Lysine Monohydrochloride). For many years, L-Lysine HCl - solid has been produced by a process of fermentation, purification, crystallization and drying. After fermentation, the resulting broth can be released from cells by filtration or centrifugation. After filtration, the L-Lysine can be recovered from the fermentation broth by an ion exchange step, which produces a liquid that is substantially free base of the L-Lysine. This solution can then be concentrated by evaporation.
Usually hydrochloric acid is added to the free base of the concentrated L-Lysine to form the L-Lysine HCl. This concentrated L-Lysine HCl solution is crystallized to produce a product in the form of L-Lysine HCl dihydrate (L-Lysine HCl: 2H20). This crystallized solid is subsequently dried until it has less than 1% moisture. This conventional product may have drawbacks. For example, it is dusty. During the handling of the product, the dust results in a loss of valuable material and sometimes causes an incomplete formulation. Also, human working conditions become less healthy and more difficult as a result of the contribution of dust by L-LysineHCl. In addition, the product sometimes develops clods during storage, which are difficult to break at the time of final use. In addition, the extensive use of an ion exchange step makes this procedure expensive. The direct spray drying of a L-Lysine fermentation broth avoids the extensive purification steps associated with the L-Lysine hydrochloride processes, in particular the use of an expensive ion exchange step. However, the consistency of the concentration of L-Lysine in the final dry product is difficult to achieve because the concentration of L-Lysine in a fermentation broth can vary considerably. Also, the dry product can be dusty and difficult to use. The 5,431,933 patent describes a process for the production of an amino acid forage supplement, which 'still contains the majority of the solids content of the fermentation broth.' The production of an industrial scale fermentation broth with 40% to 50% The content of L-Lysine is very difficult to achieve from an operational point of view: fermenter malfunctions, contamination, power interruptions and operator errors are very common and probably lead to a fermentation material that has less of about 40% L-Lysine and therefore little value.This difficulty is added to the impurities associated with the components of the media, many of which are not refined and vary in the content of solids and nutritional value of the batch. To avoid variations of the media, fermentation is restricted to specific and expensive means, which can lead to an increase in performance, which is necessary to produce a product with 40% to 50% L-Lysine, leading to high manufacturing costs, which can be prohibitive. In addition, the broth is dried to produce a powder that is difficult to handle and can have harmful effects on the health of workers due to the inhalation of dust.
A process in which a forage product is formed for animals, granular, non-dusty, is that described in the patent 5,622,710. The granulation is carried out in two steps. First, the fermentation broth is spray dried to produce particles that may include a biomass. In the second step, the particles are converted into granules by means of high-cost, expensive cutting equipment. European Application Number 91460051.5 describes a method for producing a granular product of L-Lysine HCl, free-flowing, free-flowing granulated L-Lysine, from a liquid solution or suspension by a spray granulation process. In one embodiment of the invention, the elements of a fermentation broth containing L-Lysine are subjected to ion exchange to produce a pure L-Lysine solution. Hydrochloric acid is then added to the pure L-Lysine solution to produce L-Lysine HCl which is then sprayed onto a drying bed with agitation of L-Lysine particles. The L-Lysine HCl particles are then recovered once they reach a predetermined size. International Publication Number WO / 95/23129 describes the production of non-stoichiometric salt of L-Lysine in granular form. This publication teaches the production of non-stoichiometric salts of L-Lysine in which the amount of the L-Lysine content in the final product is adjustable. Although the requirement for hydrochloric acid is reduced, other materials such as calcium hydroxide, sulfuric acid or phosphoric acid are claimed. In addition, the fermentation broth containing the L-Lysine is subjected to an exhaustive ion exchange. The patent 3,089,824 describes the use of a fluidized bed for the manufacture of compressed tablets for medical use. The process comprises (1) forming a suspension of particles in air, (2) allowing the particles to agglutinate with granulating material, and (3) coating the resulting granules with a lubricant. In one aspect of this invention, the granulating material is atomized and sprayed into the air stream of a fluidized bed of inert particles such as sucrose. The inert particles act as nuclei for the granulation. The resulting granules are coated with a lubricant. This invention provides an extremely useful process for manufacturing a granular, substantially non-dusty L-Lysine product in which the concentration of L-Lysine in the final product is controlled by the addition of the material containing L-Lysine, which is added before the agglomeration step (ie, the granulation step by dew). However, there are notations where a non-granular L-Lysine forage supplement with an adjustable amount of the L-Lysine purity on especially economic bases is desirable. An ultrafiltration step was used to provide a L-Lysine broth substantially free of cells and a cell-rich L-Lysine broth in the form of a permeable fraction and a retained fraction, respectively. If the cell-rich L-lysine broth is abandoned, it is discarded. Therefore, care must be taken in using or appropriately removing the cell-rich L-Lysin broth. The ultrafiltration step also helps considerably in the costs of the plant. If the cell-rich L-lysine broth is treated as a residual by-product, it requires primary and secondary wastewater treatments. If the cell-rich L-Lysine broth is released as untreated waste, it can have a harmful impact on the environment. For convenience in terms of expression, the term 'dryer' will be used later to describe any suitable drying means such as a spray dryer, or drum dryer, tunnel dryer, rotary dryer, tray dryer and spray granulator. In addition, the term 'spray granulation' will be used later to describe a 'fluidized bed of particles'.
The terms 'spray granulation' and 'spray granulation step', and 'agglomeration' will later be considered as equivalent terms.The terms 'retained fraction' and 'cell-rich L-lysine broth' will be considered here later as terms The term "separation" will be used hereinafter to describe the separation of a fermentation broth of L-Lysine into two fractions: a cell-rich L-Lysin broth and a L-Lysine broth substantially free of cells. Any means of separation or combination of suitable separation means can be used.
The separation can be achieved by means of filtration (for example ultra and microfiltration), and mechanical methods such as centrifugation and decanting. The term "ultrafiltration" will be used hereinafter to describe the use of an ultrafilter to filter cells from an L-Lysin fermentation broth to provide a substantially cell-free L-Lysin broth and a cell-rich L-Lysin broth. The ultrafilter used to remove the cells has a molecular weight cut between about 10,000 Daltons and 500,000 Daltons, preferably about 500,000 Daltons.
The term "neutralized L-lysine free base" will be used hereinafter to describe a material containing the free base of L-lysine, which has been neutralized using counterions such as Cl ~ and S02 ~ .The free base of the L Neutralized lysine is obtained by reacting at least a stoichiometric amount of an acid such as hydrochloric acid (HCl) or sulfuric acid (H2SO4) with the free base of L-Lisin. The term "L-Lysine-containing material" is used hereinafter to describe at least one suitable L-Lysine-containing material used alone or in combination with at least one other suitable L-Lysine-containing material. Examples of suitable L-Lysine-containing materials are L-Lysine hydrochloride, L-Lysine sulfate and neutralized L-Lysine. The term 'final L-Lysine forage supplement' will be used hereinafter to describe a final product supplemented with a purity of L-Lysine within a range of '' approximately 35% and 80% L-Lysine, measured as In addition, the term 'final L-Lysine forage supplement' shall be understood hereinafter to mean a final product in which the L-Lysine in the final product is present in its neutralized form. .
Brief Description of the Invention Accordingly, an objective of this invention is to provide a more flexible process for producing an L-Lysine production, in which the concentration of L-Lysine in the final product is controllable. Another object of this invention is to provide an improved process for producing a substantially free, free-flowing, granular L-lysine from a fermentation broth. A more particular goal is to provide a simpler and more economical method to produce granular L-Lysine. In effect, one goal is to produce a product substantially free of dust that does not require a high-cut mixing plant. A further objective is to provide an L-Lysine product that was dried and granulated in one step, a preferred process here is an "agglomeration step." Still another objective is to produce granulated L-Lysine from a fermentation broth in the which L-Lysine concentration is adjustable by adding the free base of L-Lysine or L-Lysine monohydrochloride (hereinafter referred to as 'L-Lysine Hydrochloride'). A more particular objective is to avoid the exhaustive ion exchange of the fermentation broth. A further objective is to provide a non-granular L-Lysine forage supplement with an adjustable amount of L-Lysine where the spray granulation step is replaced with alternative drying methods such as spray drying, drum drying, drying rotating, drying on tray and drying in tunnel.
BRIEF DESCRIPTION OF THE DRAWINGS The characteristics mentioned above and others of this invention and the way to obtain them will be more evident, and the invention will be better understood by referring to the following description of the invention taken in conjunction with the accompanying drawings, in which: FIGURE 1 is a flowchart, showing the main steps in a process for producing granular L-lysine, substantially free of dust, which flows freely, in that way; FIGURE 2 is a flow chart, showing the main steps in a process to produce an L-Lysine forage supplement in which the ultrafiltration step is optional and the water removal step is excluded; FIGURE 2A is a flow diagram, showing the main steps in a process to produce an L-Lysine forage supplement in which a variety of drying media were employed; FIGURE 3 is a flow diagram, showing the main steps in a process for producing an L-Lysine forage supplement in which there are two entry points for a material containing L-Lysine; FIGURE 3A is a flowchart, showing the main steps in a process for producing an L-Lysine forage supplement in which a concentrated cell-rich broth can be recycled for the addition of more L-Lysine-containing material; FIGURE 4 is a flow chart, showing the main steps in a process for producing a L-Lysine forage supplement in which a L-Lysine-containing material was added to a L-Lysine fermentation broth; and FIGURE 5 is a flowchart, showing the major steps in a process for producing an L-Lysine forage supplement in which the L-Lysine-containing material was added to the concentrated L-Lysine broth.
Brief Description of the Preferred Modes The main steps in one embodiment are a process to produce granular L-lysine, substantially free of dust, which flows freely (FIGURE 1) with an adjustable amount of L-Lysine purity in a range between about 35% and 80% L-Lysine, measured as a percent of the free base per kg. Those steps comprise: (a) ultrafiltration of a L-Lysin fermentation broth to provide a permeable fraction of L-Lysine substantially free of cells 28; (b) removing the water from the L-Lysine permeable fraction from step (a) to provide a concentrated L-Lysine broth substantially free of 40 cells; (c) adding a material containing L-Lysine to the L-Lysine broth of step (b) to produce a L-Lysine broth enriched substantially free of CSCFELB cells ") 54; and (d) agglomerating the L-L broth. Lysine from step (c) to provide a forage supplement in the form of a granular L-lysine product, substantially free of dust, which flows freely at 96. The main steps of a process of the invention (FIGURE 2) described herein produce a forage supplement of L-Lysine with a purity of L-Lysine in a range that is theoretically between about 35% and 80%, measured as a percent of the free base per kg, and more preferably between approximately 50% and 80% L-Lysine The ultrafiltration step can be replaced with a centrifugation step and the water removal step can be excluded in a process, which comprises: (a) separating, for any suitable means such as centrifugation, a broth of faith L-Lysine in two fractions; a cell-rich L-Lysine broth ("CRLB") 32 and an L-Lysine broth substantially free of CSCFLB cells "); (b) adding an L-Lysine-containing material, such as L-Hydrochloride; Lysine or the free base of L-Lysine, in 48 to the L-Lysine broth of step (a) in a mixing tank 52 to provide an L-lysine broth enriched substantially cell-free ('SCFELB'), the Aggregate material is in an amount, which leads to a final L-Lysine forage supplement with a purity of L-Lysine within a range of between about 35% and 80% L-Lysine, measured as a percent of the free base per kg; (c) agglomerating the L-Lysine broth from step (b) using a spray granulator 60 to provide L-Lysine particles; and (d) sifting the particles from step (c) to provide the final L-Lysine forage supplement 96. Alternatively, the substantially cell-free L-Lysine broth from step (ii) can be spray dried ( 60 in FIGURE 2A) to provide a forage supplement of L-Lysine 96. An L-Lysine 96 forage supplement can also be produced by tunnel drying, drum drying, rotary drying or drying in L-broth tray. -Lysine enriched substantially cell-free (62 in FIGURE 2A). Excess water can be removed (63 in FIGURE 2A), and preferably removed by evaporation. The main steps of one aspect of the process of the invention (FIGURE 3) described herein produce a forage supplement of L-Lysine with a final L-Lysine purity in the theoretical range of between about 35% and 80%, as measured as a percent of the free base per kg, more preferably between about 50% and 80% of L-Lysine. The main steps comprise: (a) a L-Lysine fermentation broth separated into two fractions to produce a substantially cell-free L-Lysine broth ('SCFLB') 28 and a cell-rich L-Lysin broth ('CRLB') 32; (b) adjust the purity of the L-Lysine of the L-Lysine broth rich in cells of step (a) to provide a rich broth in enriched cells 52; (c), remove the water from the cell-rich broth enriched from step (b) to produce a concentrated cell-rich broth 36; and (d) drying the concentrated cell-rich broth from step (c) to provide a forage supplement of L-Lysine (96) or mix the concentrate-rich broth from step (c) with more L-Lysine-containing material at 104 and then dry to provide a forage supplement of L-Lysine 96. The broth rich in concentrated cells can be mixed with more material Containing L-Lysine in the base of batches or seedlings as described in FIGURE 3a The main steps in another process of the invention (FIGURE 4) to produce a forage supplement of L-Lysine with an adjustable amount of purity of L-Lysine comprises: (a) adjusting the purity of the L-Lysine of a cald or fermentation of L-Lysine to provide a fermentation broth of enriched L-Lysine; and (b) converting the enriched L-Lysin fermentation broth from step (a) into an L-Lysine forage supplement through the step of spray granulation, spray drying, tunnel drying, tray drying, rotary drying or drum drying. The main steps in yet another alternative process (FIGURE 5) to produce a forage supplement of L-Lysine in a manner similar to that described by FIGURE 4 with the optional step of removing the water, preferably by evaporation, from the fermentation broth of L-Lysine at 36 to provide a concentrated L-Lysine broth with between about 30% and 70% solids by weight. A L-Lysine-containing material is added to the concentrated L-Lysine broth at 48 to provide an enriched L-Lysin fermentation broth. The enriched L-Lysin fermentation broth can be spray granulated at 60; spray drying in 61; and spray drying, spray granulation, tunnel drying, and pan drying or drum drying at 62 to provide an L-Lysine forage supplement with a final L-Lysine purity in the theoretical range of between about 35 ° C. % and 80% L-Lysine, measured as one percent of the free base per kg, more preferably between about 50% and 80% L-Lysine.
Detailed Description of the Preferred Modes Although one aspect of this invention is the harvesting and processing of the L-Lysine base of a fermentation broth, the composition and nature of the fermentation medium may vary. For example, any suitable organism that produces high amounts of L-Lysine of the genus Coryneabacterium or Brevibacterium can be used to inoculate the fermentation medium. Before inoculation with the bacteria that produce L-Lysine, the fermentation medium can have the following composition: Material Quantity (g / 1) Soy hydrolyzate 20.0 Ammonium sulfate 20.0 Urea 3.0 Monopotassium phosphate 1.0 Magnesium sulfate heptahydrate 0.5 Manganese sulphate 0.002 Material Quantity (g / 1) Biotin 0.0001 Thiamin Hydrochloride 0.0001 Glucose 30.0 The pH was adjusted and maintained at approximately 7.2 with ammonium hydroxide. The temperature was maintained at approximately 32 ° C. The forage is glucose: (NH4) 2S0 with the glucose concentration maintained at approximately 10 g / 1.
The fermentation medium can be inoculated into the fermentation vessel using standard microbiological practices that are known to those skilled in the microbiological arts. The fermentation vessel should be equipped with an agitator, a ventilation system, and a temperature control device to maintain the fermentation broth at about 30 ° C and preferably at 32 ° C. The fermentation is carried out until the L-Lysine base concentration is about 92 g / l (grams per liter) and that of total dry solids is about 218 g / l. Aseptic techniques should be observed through the fermentation process to avoid contamination of the fermentation broth with organisms that do not produce L-Lysine.
Within one aspect of this invention, which will be understood with reference to FIGURE 1, the process produces granular L-lysine substantially free of dust, which flows freely, from a fermentation broth somewhat as described below: (i) A fermentation broth containing L-Lysine in the fermentor 20 is separated into two fractions by means of ultrafiltration at 24 to remove the cells to produce a L-Lysine broth substantially free of cells (shown at 28 as the Permeable Fraction "in the attached Figure. The L-lysine broth rich in cells (here treated as residual retained fraction) is eliminated in 32. The ultrafilter used to remove the cells, has a molecular weight cut of between 10,000 Daltons and 500,000 Daltons, preferably about 500,000 Daltons (ii) The substantially cell free L-Lysine broth is evaporated to remove the water at 36 to produce a L-Lysine broth with centered substantially cell-free 28. Preferably, the concentrated L-Lysine broth substantially free of cells (shown as 'Concentrate' at 40) has between about 30% and 70% solids by weight. The waste water is drained at 44. The evaporation is carried out in the approximate range of between 60 ° C and 101.11 ° C (140 ° F and 214 ° F), preferably between 62.77 ° C and 68.33 ° C (145 ° F and 155 ° F), and a pressure of between 20 KPa and 75.86 KPa (2.9 psia and 11 psia) (vacuum), preferably from 20 KPa to 27.58 KPa (2.9 psia to 4 psia). (iii) The purity of L-Lysine from the concentrated L-cellulose broth substantially cell-free is adjusted in a mixing tank 52. The adjustment is made by adding L-Lysine-containing material at 48 to a mixing tank 52 to provide a L-Lysine broth enriched substantially free of SCFELB cells at 54. The L-Lysine containing material is added in an amount which leads to a final L-Lysine forage supplement with a purity of L-Lysine in the range theoretical between approximately 35% and 80% L-Lysine, measured. as a percent of the free base per kg, and more preferably between about 50% and 80% of L-Lysine. (iv) L-Lysine broth enriched substantially cell-free is atomized by means of a nozzle 56 to provide an atomized spray of L-Lysine broth enriched substantially cell-free to produce a percolation bed of L-Lysine particles in a dew granulator 60. L-Lysine particles have particle sizes of less than about 177 microns (ie the particles can pass through an 80 mesh) and preferably in the size range of approximately 100 microns and 177 microns. The spray granulator bed is preferably a fluidized bed of L-Lysine particles and is operated at a temperature between about 30 ° C and 100 ° C. (v) The position of the nozzle 56 is adjusted until it is just above the fluidized bed of L-Lysine particles. (vi) L-Lysine broth enriched substantially cell-free is sprayed onto the fluidized bed of L-Lysine particles to initiate the agglomeration process. (vii) The agglomeration process is allowed to continue to produce the granular L-lysine product, substantially free of dust, flowing freely, in the size range of between about 177 microns and 1190 microns, and preferably in the size range of between about 177 microns to 420 microns. (viii) 'The product is removed from the dewatering granulator at 64, with the waste water flowing at 68 in the form of steam in the dryer exhaust system. (ix) The product is then selected and classified by size in the sieve 72 (preferably 80 mesh). (x) Granules in 76 that are too large (for example in the size range of more than about 1190 microns) are crushed in a mill at 80 to a smaller particle size (for example in the size range of less than about 177 microns) and combined with the material that is too small 84 (for example in the size range of less than about 177 microns) to produce recycled L-Lysine particles (shown at 88 as "Recharge" in Figure 1) and returned to the spray granulator 60 as starting material which it acts as seeds for the agglomeration process. (xi) The product of granular L-lysine substantially free of free flowing powder, in the size range from about 177 microns to 1190 microns (shown 92 as' Particles of 177-1190 microns ") passes through the sieving process and is acceptable as the final product at 96. However, the preferred range is from about 177 microns to 420 microns since it is better packaged and reduces transportation costs. The preferred L-Lysine concentration in the starting feed stream of the L-Lysin fermentation broth is about 90 g / 1 L-Lysine, measured as a percent of the free base per kg.
However, the concentration of L-Lysine can vary from one fermentation trial to the next. Accordingly, the use of a fermentation broth containing approximately 90 g / l of L-Lysine means that other suitable concentrations of L-Lysine in the concentration broth are acceptable. However, the concentration of L-Lysine in the fermentation broth should not be less than about 30 g / 1.
As described in step (iii) above, the final concentration of desired L-Lysine can be achieved by adding a material containing L-Lysine. Although ultrafiltration is the preferred method for obtaining the L-Lysine broth substantially free of cells, it does not mean that other methods can not be used. The cells could also be removed by mechanical separation techniques, such as centrifugation. Other suitable methods include microfiltration and decanting. The invention contemplates the removal of cells from the fermentation broth containing L-Lysine by several other processes. For example, the fermentation broth 20 could be similarly separated and approximately 50% centrifuged and the remaining 50% ultrafiltered with the results of the broth cell removal process combined to produce a substantially cell-free L-Lysine broth. This flexibility will improve the practice of the invention in the industrial installation. Although the present invention contemplates the addition of a L-Lysine-containing material to the concentrated, cell-free L-lysine broth in the mixing tank 52, the addition of such material to the concentrated L-Lysine broth can be "" omitted if the desired concentration of L-Lysine (as the free base) in the concentrated L-Lysine broth substantially free of cells is such that the addition of the L-Lysine-containing material, as described in step (iii), it is unnecessary. For example, the step of adding the material containing L-Lysine can be omitted if the concentration of L-Lysine in the concentrated L-Lysine broth substantially free of cells substantially exceeds about 35% L-Lysine, as measured as a percent of the free base per kg. If the cell-free concentrated L-Lysine broth contains substantially more than about 35% L-Lysine, measured as a percent of the free base per kg, the L-Lysine broth is an enriched L-Lysine broth. substantially cell free. Experience has shown that there is a relationship between nozzle orifice size 56, flow velocity and anometric pressure. Although the preferred nozzle size is 0.156 cm (0.0615 pg), several other sizes can also be used to supply the spray. In particular, the nozzle designs distributed by Spraying Systems Co., PO Box 7900, Wheaton, IL 60189-7900, USA (tel: 630-665-5000) work well to produce a fine mist. The spray granulator can be obtained from Glatt Air Techniques, 20 Spear Road, Ramsey, NJ 07446-1288, USA (tel: 201-825-8700) .. Experience also suggests that manufacturing L-Lysine granules on a commercial scale will require several nozzles to atomize and spray the enriched * L-Lysine broth onto a proportionally larger bed of particles of percolation of L-Lysine. The particle percolation bed should comprise L-Lysine particles of small enough size to function as seeds for the agglomeration process. It is preferred that the L-Lysine particles be less than about 177 microns in size and preferably between about 100 microns and 177 microns. In the agglomeration process, the sown particles grow simultaneously in size and dry when sprayed with the permeable fraction of enriched L-Lysine. The agglomeration process is aided by binders that are inherently present in the broth • of enriched L-Lysine, namely: the fermentation broth of L-Lysine, L-Lysine hydrochloride, L-Lysine sulfate and water. A binder is defined as a substance that provides the adhesive component that allows the seeds the agglomeration process to grow in size. The L-Lysine particle source used for producing the seeds in the fluidized bed of L-Lysine in the spray granulator is not critical, although the preferred source is obtained by atomizing the enriched L-Lysine broth substantially free of cells as , < ? described in step (iv.) above or the particles L-Lysine recycled as described in step (x) above, and shown- in 88 in FIGURE 1. Alternatively, the fluidized bed of L-Lysine particles could be produced by atomizing or spray drying any of the following: the broth of fermentation containing L-Lysine from step (i), the permeable fraction of L-Lysine substantially free of cells from step (i), the L-Lysine broth substantially free of cells produced by the centrifugation of the fermentation broth containing L-Lysine from step (i), the broth from L-Lysine substantially free of cells from step (ii) or any combination thereof. In addition, L-Lysine hydrochloride and pure L-Lysine free base could be used as a source for the L-Lysine particles to produce the fluidized bed of L-Lysine particles and for act as seeds for the agglomeration process.
Although the exact source of the L-Lysine particles to produce the fluidized bed of L-Lysine particles and the seeds for the agglomeration process is not critical, it is preferred that the L-Lysine particles be less than about 177 microns in size and preferably between about 100 microns and 177 microns. In summary, suitable sources for producing the L-Lysine particles include: the substantially cell-free L-Lysine broth obtained from the centrifugation of the fermentation broth containing L-Lysine from step (i), the permeable fraction from L -Lysine substantially free of cells from step (i), the concentrated L-Lysine broth substantially free of cells from step (ii), and the enriched L-Lysine broth substantially free of cells from step (iii). Each of these sources, or any combination of those sources, can be atomized by the nozzle 56 in the spray granulator 60 to generate the L-Lysine particles. Alternatively, the L-Lysine particles can be made separately by spray-drying, and possibly storing for later use, any of the following: the substantially cell-free L-Lysine broth obtained from the centrifugation of the fermentation broth that contains L-Lysine from step (i), the permeable fraction of L-Lysine substantially free of cells from step (i), the concentrated L-Lysine broth substantially free of cells from step (ii) and the L-Lysine broth enriched substantially free of cells of step (iii). Before using as L-Lysine particles, the spray-dried products can be screened to remove lumps and to obtain particles in the size range of less than about 177 microns (preferably between about 100 microns and 177 microns). For example, the concentrated L-Lysine broth substantially free of cells from step (ii) can be used to produce the bed of percolation seed particles at 60. The concentrated L-Lysine broth substantially free of cells can be atomized by the nozzle 56 in the spray granulator 60 to generate the percolation bed of seed particles. Alternatively, the concentrated L-Lysine broth substantially cell free can be spray-dried separately. Before using as L-Lysine particles, the concentrated, spray dried L-Lysine broth can be screened to remove lumps and to obtain particles in the size range of less than about 177 microns (preferably from about 100 microns and 177 microns).
Another example of a suitable source of L-Lysine particles would be the purified L-Lysine hydrochloride powder which can be obtained by the processes known in the state of the art. This dry powder can be used as a source of L-Lysine particles or the powder can be screened to remove the lumps and classify the particles of less than about 177 microns (preferably in the range of about 100 microns to 177 microns) . Experience has shown that once the agglomeration process becomes self-sustaining, the particles for the fluidized bed 60 come from the particles recycled at 88 in the bed of the fluidized spray granulator 60 by the use of the particles in 84, which They are too small or the granules that are too large and have been crushed in 80 to a smaller size. Experience has also shown that the agglomeration process can operate in batches or semi-continuously. Batch process is preferred. Although the preferred L-Lysine concentration in the initial feed stream, measured as one percent of the free base per kg, in the fermentation broth is about 90 g / L L-Lysine, those skilled in the art will understand that the concentration of L-Lysine can vary from one fermentation trial to the next. Accordingly, the use of a fermentation broth containing approximately 90g / L L-Lysine should not be taken to mean that other suitable concentrations of L-Lysine in the fermentation broth are impeded. The desired final concentration of L-Lysine can be achieved by adding a material containing L-Lysine, such as L-Lysine HCl or the free base of L-Lysine, at 48, and as described in step (iii) above. However, the concentration of L-Lysine in the fermentation broth should not be less than 30 g / l. A second embodiment of this invention for producing an L-Lysine forage supplement is shown in FIGURE 2. (i) A fermentation broth containing L-Lysine in a fermenter at 20 is separated into two fractions at 24 to produce a L-Lysine broth substantially free of CSCFLB cells ") and a cell-rich L-lysine broth CCRLB ") 32. The cell-rich L-Lysin broth (shown as E2 in FIGURE 2) can be processed as described in the third embodiment of FIGURE 3. Any suitable means, such as ultrafiltration or centrifugation, in 24 to separate the amino acid fermentation broth. (ii) The purity of the L-Lysine of the substantially cell-free L-Lysine broth is adjusted by adding an effective amount of the L-Lysine-containing material at 48 (FIGURE 2) to the L-Lysine broth substantially free of a mixing tank at 52 to provide an L-lysine broth enriched substantially cell-free ('SCFELB'). The amount of L-Lysine-containing material added at 48 depends on the concentration of L-Lysine in the L-broth. -Lysine substantially cell free, measured as a percent of the free base per kg, however, the amount of L-Lysine should be sufficient to ensure that the final concentration of L-Lysine in the final product is in the range of between about 35% and 80% of L-Lysine, measured as a percent of the free base per kg (iii) The L-Lysine broth, enriched substantially cell free is optionally atomized by a 56 nozzle for provide an atomized spray of L-Lysine broth enriched substantially cell-free to produce a percolation bed of L-Lysine particles in a dew granulator 60. The L-Lysine particles have a particle size of less than about 177 microns (i.e. which can pass through a 80 mesh) and preferably in the range of about 100 microns and 177 microns. The bed of the spray granulator is preferably a fluidized bed of L-Lysine particles and is operated at a temperature between about 30 ° C and 100 ° C. Alternatively, the L-Lysine broth enriched substantially cell free of step (ii) in FIGURE 2 can be spray dried to provide a forage supplement of L-Lysine. An L-Lysine forage supplement can also be produced by tunnel drying, drum drying, rotary drying, or tray drying of enriched, substantially cell-free L-Lysine broth (62 in FIGURE 2A). Excess water is removed (63 in FIGURE 2A), preferably by evaporation. (iv) The position of the nozzle 56 (FIGURE 2) is adjusted to just above the fluidised bed of L-Lysine particles of the spray granulator. (v) L-Lysine broth enriched substantially cell-free is sprayed onto the fluidized bed of L-Lysine particles from the spray granulator to initiate the agglomeration process. (vi) The agglomeration process is allowed to continue to produce the granular L-lysine product, substantially free of dust, which flows freely, in the size range of approximately 177 microns and 1190 microns, preferably in the range of approximately 177 microns to 420 microns. (vii) The product is removed from the dewatering granulator at 64, with the waste water flowing at 68 in the form of steam in the exhaust system of the spray granulator. (viii) The product is then sieved and sized by sieve 72 (preferably 80 mesh). (ix) Granules in 76 that are too large (for example in the size range of more than about 1190 microns) are crushed in a mill at 80 to a smaller particle size (for example in the size range of less than about 177 microns) and combined with the material what is too much 'small 84 (for example in the size range of less than about 177 microns) to produce recycled L-Lysine particles in 88 (FIGURE 2) and return to the spray granulator 60 as starting material to act as seeds for the agglomeration process. (x) The product of granular L-lysine substantially free of dust, free flowing, of 'Particles of 177-1190 microns ", with a purity of L-Lysine in the range of between about 35% and 80% of L - Lysine, measured as a percent of the free base per kg, and a size range of approximately 177 microns to 1190 microns in 92 passes through the sieving process and are acceptable as the final product in 96. However, since the bulk density viewpoint, the preferred product size is in the range of between about 177 microns and 420 microns.A third embodiment (FIGURE 3) of this invention produces a forage supplement of L-Lysine. A fermentation broth of L-Lysine in a fermentor 20 is separated into two fractions in 24 to produce a L-Lysine broth substantially free of CSCFLB cells ") and a cell-rich L-Lysine broth.
('CRLB ") 32. The L-Lysine broth substantially free of cells (shown as El) can be processed as described in the second embodiment of FIGURE 2. Any means for separating the fermentation broth from L can be used. -Lisine such as ultrafiltration or centrifugation Before separating the L-Lysin fermentation broth, an L-Lysine-containing material can be added optionally directly to the fermentation of L-Lysine.
The agitation provided by the fermenting vessel CSTR ") of the reactor in the tank with suitable agitation could provide the necessary degree of mixing to ensure a concentration of L-Lysine in the fermentation broth of L-Lysine. (Ii) The purity of L-Lysine from the L-broth. -Lysine rich in cells is adjusted by adding an effective amount of the L-Lysine-containing material to the cell-rich L-Lysin broth in a mixing tank at 52 to provide a broth enriched in enriched cells ('ECRB') 55. The amount of L-Lysine-containing material added at 48 depends on the concentration of L-Lysine in the cell-rich L-Lysin broth, measured as a percent of the free base per kg. However, the amount should be sufficient to ensure that the final concentration of L-Lysine in the final product is in the range of between about 35% and 80% L-Lysine, measured as one percent of the free base. per kg. (iii) The water is removed from the cell-rich broth enriched by evaporation at 36 to produce a concentrated cell-rich broth ('CCRB')., the broth rich in concentrating cells has between about 20% and 70% solids by weight. (iv) The concentrated cell-rich broth is dried at 62 'to provide a forage supplement of L-Lysine 96 with a purity of L-Lysine in the range of between about 35% and 80% L-Lysine, measured as a percent of the free base per kg. Alternatively, the concentrated cell-rich broth is mixed with more L-Lysine-containing material in a second mixing tank at 104 and then dried in 62. If this mode is practiced batchwise or in an iconic form, it would be more It is desirable to use only one mixing tank 52 simply by recycling the cell-rich stock again concentrated in 108 to the mixing tank 52 as described in FIGURE 3a. A fourth embodiment of this invention (FIGURE 4) includes a process for producing a forage supplement of L-Lysine with a purity of L-Lysine in the range of between about 35% and 80% L-Lysine, measured as one percent of the free base per kg. (i) The purity of the L-Lysine from a fermentation broth of L-Lysine in the fermentor 20 is adjusted by adding an effective amount of a material containing L-Lysine in 48 to a mixing tank at 52 to provide a broth fermentation of enriched L-Lysine('ELFB') The amount of L-Lysine-containing material added to 48 depends on the concentration of L-Lysine in the L-Lysine fermentation broth, measured as • one percent of the free base per kg. However, the amount should be sufficient to ensure that the final concentration of L-Lysine in the final product is in the range of between about 35% and 80% L-Lysine, measured as a percent of the free base by Theoretically, it would be beneficial to add L-Lysine-free base at 48 to take advantage of the natural aqueous anions present in the fermentation broth of L-Lysine Sulfate, chloride and hydroxyl anions in the fermentation broth of L-Lysine they could theoretically neutralize the free base of L-Lysine (ii) Depending on the position of the flow valve 112, the enriched L-Lysine fermentation broth is converted into a forage supplement of granular L-Lysine by means of a dew granulator 60 (it is say agglomerate) or converted into a forage supplement of L-Lysine by means of a spray dryer 61. The water is removed at 63, preferably by evaporation. The present invention contemplates the addition of a L-Lysine-containing material to, for example, the fermentation broth containing L-Lysine or the concentrated L-Lysine broth. However, the addition of the L-Lysine-containing material can be omitted if the desired concentration of L-Lysine (measured as free base) in the fermentation broth containing L-Lysine from the concentrated L-Lysine broth is such that the addition of the material containing L-Lysine is unnecessary, as when the concentration exceeds about 35% L-Lysine, measured as one percent of the free base per kg. If the fermentation broth containing L-Lysine or the concentrated L-Lysine broth contains substantially more than about 35% L-Lysine, measured as a percent of the free base per kg, then both the broth and the concentrate they count as enriched L-Lysine broth. A fifth embodiment of this invention (FIGURE 5) includes a process for producing a forage supplement of L-Lysine, which is essentially the same as described in the fourth embodiment with the optional step of removing the water, preferably by evaporation, from the fermentation broth of L-Lysine at 36 to provide a broth of L-Lysine concentrate with between approximately 30% and 70% solids by weight. A L-Lysine-containing material is added to the concentrated L-Lysine broth at 48 to provide an enriched L-Lysin fermentation broth. The enriched L-Lysin fermentation broth can be spray granulated at 60; spray drying in 61; and spray drying, spray granulation, tunnel drying, pan drying, or drum drying at 62 to provide a forage supplement of L-Lysine with a purity of L-Lysine in the range of between about 35% and 80% L-Lysine, measured as one percent of the free base per kg. The following examples represent specific but not limiting embodiments of the present invention: EXAMPLE 1 - Comparative Example 400 liters of fermentation broth were harvested with an L-Lysine concentration of 92 g / l (grams per liter) of the L-Lysine base and 218 g / l of total dry solids were harvested from a L-Lysine fermentation test. This material was ultrafiltered and evaporated at a concentration of 235 g / 1 in the form of L-Lysine sulfate (measured as the free base) and 493 g / 1 of dry solids. 5150 ml (milliliters) of this concentrate were dried on a Glatt WSG 5 spray granulator. The inlet temperature of the Glatt unit was maintained between 93 ° C and 124 ° C, preferably 120 ° C. The outlet temperature was maintained between about 40 ° C and 80 ° C, preferably between 60 ° C and 65 ° C. The bed temperature was maintained between 70 ° C and 92 ° C, preferably between 71 ° C and 74 ° C. The air flow was maintained between 1, 300 and 4,000 feet per minute (390 and 1,200 meters per minute), preferably between 1,300 and 1,500 feet per minute (390 and 450 meters per minute). The nozzle atomization air was at a gauge pressure of between 50 to 70 pounds per square inch (3.5 to 4.9 kilograms per square centimeter). Approximately 2,500 ml of the concentrate was sprayed into the dryer with the nozzle at the highest setting to form a bed of material on which it agglomerated. The nozzle was lowered to a position above the percolation material in the bed and the agglomeration was completed with the remaining 2.650 ml of the concentrate. This produced a granulated product having the composition indicated in Table 1.
* The purity is measured as the percent free base of L-Lysine per kg.
EXAMPLE 2 The Lysine fermentation broth / ultrafiltrate and concentrate as described above in Example 1, was mixed 4 to 1 (based on lysine) with purified L-Lysine sulfate (produced as a free base and pH adjusted to 6 with sulfuric acid to give L-Lysine sulfate). The mixture was spray granulated as described in Example 1. The process was repeated with a mixture 3 to 2, a mixture 2 to 3, a mixture 1 to 4, and with L-Lysine sulfate only. The granulated products had the compositions indicated in Table 2.
TABLE 2 * The purity is measured as the percent free base of L-Lysine per kg.
EXAMPLE 3 The Lysine fermentation broth, ultrafiltered and concentrated as described above in Example 1, was mixed 4 to 1 (based on lysine) with pure L-Lysine hydrochloride. The mixture was spray granulated as set forth in Example 1 above. The process was repeated with a 3 to 2 mixture, a 2 to 3 mixture, a 4 to 1 mixture, and with L-Lysine hydrochloride alone. The granulated product had the compositions indicated in Table 3.
TABLE 3 * the purity is measured as the percent free base of L-Lysine per kg. It can be observed that when mixing the fermentation broth of concentrated L-Lysine and ultrafiltrate of the Example 1 with L-Lysine sulfate or L-Lysine hydrochloride, as described in Examples 2 and 3 respectively, produces a granular product with higher L-Lysine content.
Also, a preferred embodiment of the disclosed invention allows the L-Lysine content in the L-Lysin fermentation broth to be easily adjusted prior to the agglomeration step. Thus, natural variations in L-Lysine concentration, which often occur from a fermentation of L-Lysine to the next L-Lysine fermentation, do not require exhaustive ion exchange to obtain a final product of the necessary purity. to be used (for example with a forage additive). The preferred level of purity in the final granular L-Lysine product is in the range of between about 35% and 80% L-Lysine, measured as a percent of the free base per kg.
EXAMPLE 4 Lysine fermentation broth was mixed, having a solids content of 193.8 g / kg and a lysine content of 74.3 g / kg with the neutralized L-lysine produced as a free base to give a concentration of 508 g / kg of lysine and 977.1 g / kg of solids.
Approximately 3100 ml of this mixture were dried in a Glatt WSG 5 spray granulator. The inlet temperature was maintained between 136 ° C and 146 ° C. The outlet temperature was maintained between 42 ° C and 74 ° C, preferably between 60 ° C and 65 ° C. The bed temperature was maintained between 63 ° C and 79 ° C, preferably between 71 ° C and 74 ° C. The air flow was maintained between 4.44 and 5.91 cubic meters per minute (157 and 209 cubic feet per minute) (real), preferably between 36.69 and 42.45 cubic meters per minute (300 and 1500 cubic feet per minute). The nozzle atomization air was between a gauge pressure of 324.67 to 482.75 kilopascals (50 to 70 pounds per square inch). Approximately .2250 ml was sprayed into the dryer with the nozzle at the highest setting to form a bed of material on which to agglomerate. The nozzle was lowered just above the percolation material in the bed and the agglomeration was completed with the remaining 850 ml of the feed. This produced a granulated product having a purity of 52% 'on a dry basis. The granulated product had the composition indicated in Table 4.
TABLE 4 * purity was measured as percent free base per kg EXAMPLE 5 Five kilograms of ultrafiltered permeable fraction of lysine broth, having a purity of 44.9% on dry basis and total solids of 69.9 g / kg, were mixed, with 182 g of neutralized L-Lysine, which has a purity of 56.3% on dry basis and total solids of 716 g / kg, and was spray-dried on a Niro Atomizer spray dryer equipped with a spray nozzle type nozzle . The inlet temperature was 230 ° C, the outlet temperature was 80 ° C, and the atomizing disk pressure was 3.3 kp / cm2. The feed rate was 34 ml / mm. This produced a product that had a purity of 51.2% lysine on a dry basis.
EXAMPLE 6 Five kilograms of the ultrafiltered permeable fraction of the lysine broth, which had a purity of 44.9% on dry basis "and total solids of 69.9 g / kg, were mixed with 182 grams of neutralized L-lysine, which had a purity of 56.3% on dry basis and total solids of 716 g / kg, and evaporated to 25.4% solids This evaporated mixture was dried in a drum dryer The drum dryer had two drums rotating in the opposite direction, 22.22 cm (8.75 in) in length and 12.7 cm (5 in) in diameter rotating at a speed of 2.5 RPM Steam was supplied to the drum at a pressure of 275.86 KPa (40 psi) .The feed rate was 20 to 40 ml This produced a product having a purity of 48.9% lysine on a dry basis The invention was described above in connection with the preferred or illustrative embodiments, those embodiments are not intended to be exhaustive or to limit the invention. invention intends to cover all the alter native, modifications and equivalents included within the spirit and scope of the invention, as defined by the appended claims.

Claims (24)

CHAPTER CLAIMEDICATORÍO Having described the invention, it is considered as a novelty and, therefore, what is claimed in the following claims is claimed:
1. A process to produce an L-Lysine forage supplement with an adjustable amount of L-Lysine purity in a range between approximately 35% and 80% L-Lysine, measured as the percent of the base free per kg, the process is characterized by comprising the steps of: (a) adding: - a material containing L-Lysine to a fermentation broth of L-Lysine to provide a fermentation broth of enriched L-Lysine, the material aggregate is in an amount, which leads to a final L-Lysine forage supplement with a purity of L-Lysine within a range of between about 35% and 80% L-Lysine, measured as a percent of the free base per kg; and (b) substantially drying the L-Lysine fermentation broth enriched from step (a) to provide the final L-Lysine forage supplement.
2. The process according to claim 1, characterized in that the forage supplement of L-Lysine in step (b) has between about 50% and 80% of L-Lysine, measured as a percent of the base free per kg.
3. The process according to claim 1, characterized in that the L-Lysine-containing material of step (a) is selected from the group consisting of L-Lysine hydrochloride, L-Lysine sulfate and L-neutralized Lysine.
4. The process according to claim 1, characterized in that the L-Lysine-containing material of step (a) is the free base of L-Lysine.
The process according to claim 1, characterized in that the substantial drying of step (b) is carried out in a dryer selected from the group consisting essentially of: drum drying, spray drying, rotary drying, tray drying , tunnel drying and spray granulation.
6. A process for producing an L-Lysine forage supplement with an adjustable amount of the L-Lysine purity in a range of between about 35% and 80% L-Lysine, measured as a percent of the free base per kg, characterized in that it comprises the steps of: (a) removing water from a fermentation broth of L-Lysine to provide a concentrated L-Lysine broth; (b) adding a material containing L-Lysine to the concentrated L-Lysine broth from step (a) to provide an enriched L-Lysin fermentation broth, the added material being in an amount which leads to a forage supplement of final L-Lysine with a purity of L-Lysine in a range between about 35% and 80% L-Lysine, measured as a percent of the free base per kg; and '(c) substantially drying the L-Lysine fermentation broth enriched from step (b) to provide the final L-Lysine forage supplement.
The process according to claim 6, characterized in that the L-Lysine broth concentrated in step (a) has between about 30% and 70% solids by weight.
8. The process according to claim 6, characterized in that the L-Lysine-containing material "from step (b) is selected from the group consisting of L-Lysine hydrochloride, L-Lysine sulfate and neutralized L-Lysine.
The process according to claim 6, characterized in that step (a) comprises evaporating the fermentation broth of L-Lysine to remove water to provide the concentrated L-Lysine broth.
10. The process according to claim 7, characterized in that the evaporation step (a) is carried out between approximately 60 ° C and 101 ° C (140 ° F and 214 ° F).
11. The process according to claim 7, characterized in that the evaporation of step (a) is carried out between about 62.7 ° C and 68.3 ° C (145 ° F and 155 ° F).
12. The process according to claim 7, characterized in that the evaporation step (a) is carried out in a vacuum of between about 20 KPa and 75.86 KPa (2.9 psia and 11 psia).
13. The process according to claim 7, characterized in that the evaporation of step (a) is carried out in a vacuum of between about 20 KPa to 27.58 KPa (2.9 psia to 4 psia).
The process according to claim 6, characterized in that the L-Eisin fermentation broth enriched from step (b) has between about 50% and 80% L-Lysine, measured as a percent of the base free per kg.
15. The process according to claim 6, characterized in that the substantial drying of step (c) is selected from the group consisting essentially of: drum drying, spray drying, tray drying, tunnel drying, rotary drying and granulation by dew. ,
16. A process for producing an L-Lysine forage supplement with an adjustable amount of L-Lysine purity in a range of between about 35% and 80% L-Lysine, measured as a percent of the free base per kg, characterized in that it comprises the steps of: (a) separating a fermentation broth from L-Lysine in a L-Lysine broth substantially free of cells and a cell-rich L-Lysine broth; (b) adding a material containing L-Lysine to the L-lysine broth rich in cells of step (a) to provide a broth rich in enriched cells, the added material is in an amount which leads to a forage supplement of final L-Lysine with a purity of L-Lysine in a range of between about 35% and 80% L-Lysine, measured as a percent of the free base per kg; (c) removing water from the rich broth in cells enriched from step (b) to provide a broth rich in concentrated cells; and (d) drying the concentrated cell-rich broth from step (c) to provide the final L-Lysine forage supplement.
17. The process according to claim 16, characterized in that step (c) further comprises adding an additional amount of the L-Lysine-containing material to the concentrated cell-rich broth.
18. The process according to claim 16, characterized in that the drying means of step (b) are selected from the group consisting essentially of a tunnel dryer, drum dryer, rotary dryer and tray dryer.
19. A process for producing an L-Lysine forage supplement with an adjustable amount of L-Lysine purity in a range of between about 35% and 80% L-Lysine, measured as a percent of the free base per kg, characterized in that it comprises the steps of: (a) separating a fermentation broth of L-Lysine in a L-Lysine broth substantially free of cells and a cell-rich L-Lysin broth; (b) adding a material containing L-Lysine to the L-Lysine broth substantially free of passage cells (a) to provide a L-lysine broth enriched substantially cell free, the aggregate material is in an amount which leads to a final L-Lysine forage supplement having a purity of L-Lysine in a range of between about 35% and 80% of L-Lysine, measured as a percent of the free base per kg; and (c) drying the enriched L-Lysine broth substantially free of cells from step (b) to provide the final L-Lysine forage supplement.
The process * according to claim 19, characterized in that the drying means of step (c) are selected from the group consisting essentially of: a spray granulator, spray dryer, tunnel dryer, drum dryer, dryer rotary and a tray dryer.
21. The process according to claim 19, characterized in that step (c) further comprises a screening step for selecting the particles in the size range of between about 177 microns and 1190 microns.
22. A process for producing an L-Lysine forage supplement with an adjustable amount of L-Lysine purity "in a range of between about 35% and 80% L-Lysine, measured as a percent of the free base per kg, characterized in that it comprises the steps of: (a) removing water from the fermentation broth containing L-Lysine to provide a concentrated L-Lysine broth; (b) determining the concentration of L-Lysine, measured as a percent of the free base per kg, in the concentrated L-Lysine broth; (c) adding a material containing L-Lysine to the concentrated L-Lysine broth to provide a broth of L-Lysine enriched if the concentration of L-Lysine in the concentrated L-Lysine broth, measured as a percent of the free base per kg, is less than about 35%, the aggregate material is in an amount, which leads to a final L-Lysine forage supplement with a purity of L-Lysine in a range of between about 35% and 80% L-Lysine, measured as a percent of the free base per kg; and (d) substantially drying the enriched L-Lysine broth to provide the final L-Lysine forage supplement.
23. A process for producing an L-Lysine forage supplement with an adjustable amount of the L-Lysine purity in a range of between about 35% and 80% L-Lysine, measured as a percent of the free base per kg, characterized in that it comprises the steps of: (a) removing water from a fermentation broth containing L-Lysine by evaporating the fermentation broth containing L-Lysine in a temperature range of approximately 140 ° F and 214 ° F (60 ° C and 101 ° C) and in a vacuum between approximately 20 KPa and 75.86 KPa (2.9 psia and 11 psia) to provide a concentrated L-Lysine broth, which contains approximately 30% and 70% solids by weight; (b) determining the concentration of L-Lysine, measured as a percent of the free base per kg, in the concentrated L-Lysine broth; (c) adding a sufficient amount of L-Lysine-containing material to the concentrated L-Lysine broth to provide an enriched fermentation broth if the concentration of L-Lysine in the concentrated L-Lysine broth, measured as a percent of the free base per kg is less than about 35%, the added material containing L-Lysine is selected from the group consisting of L-Lysine hydrochloride, L-Lysine sulfate and neutralized L-Lysine, the aggregate material being found in an amount which leads to a final L-Lysine forage supplement with a purity of L-Lysine in a range between approximately 35% and 80% L-Lysine, measured as a percent of the base free per kg; and (d) substantially drying the enriched L-Lysine broth to provide the final L-Lysine forage supplement with a purity of L-Lysine in a range of between about 35% and 80% L-Lysine, as measured as a percent of the free base per kg.
24. A process for producing an L-Lysine forage supplement, characterized in that it comprises: (a) determining the concentration of L-Lysine, measured as a percent of the free base per kg, in a fermentation broth containing L -Lisina; (b) adding a material containing L-Lysine to the fermentation broth containing L-Lysine to provide an enriched L-Lysine broth, the added material being in an amount, which leads to a forage supplement of L- Final Lysine with a purity of L-Lysine in a range of between about 35% and 80% L-Lysine, measured as a percent of the free base per kg, the added material containing L-Lysine is selected from group consisting essentially of L-Lysine hydrochloride, L-Lysine sulfate and neutralized L-Lysine; Y (c) substantially drying the enriched L-Lysine broth to provide the final L-Lysine forage supplement.
MXPA/A/1998/010678A 1997-12-16 1998-12-15 Process to manufacture granu l-lysine forage supplements MXPA98010678A (en)

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US08991145 1997-12-16
US09098948 1998-06-17

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