Classifications

• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
  • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
  • C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
  • C07C227/38—Separation; Purification; Stabilisation; Use of additives
  • C07C227/40—Separation; Purification

Definitions

• the present invention relates to a method for separating a basic amino acid from a fermentation broth.
• Lysine and other basic amino acids are used extensively as animal feed supplements.
• lysine is produced by the fermentation of dextrose.
• the fermentation broth contains a variety of impurities, such as color bodies, residual sugars, salts, and other by-products.
• the primary step in the purification of lysine from fermentation broth is ion exchange chromatography (Tanaka, et al., U.S. Patent No. 4,714,767 (1985)).
• the chromatographic separation can be operated in batch or continuous mode using fixed bed or simulated moving bed technology (Nan Walsern, H.J., and
• SMB Simulated moving bed
• the present invention relates to a method for separating a basic amino acid from fermentation broth using simulated moving bed technology, comprising contacting the fermentation broth with strong acid cation exchange resins that have a low degree of cross-linkage, and eluting the amino acids from the exchange resins.
• Figure 1 shows the column configuration of amino acid separation in simulated moving bed operation.
• the present invention relates to method and apparatus of separating basic amino acids from a fermentation broth. Specifically, the invention relates to separating basic amino acids from fermentation broth, using simulated moving bed technology, comprising: (a) contacting the fermentation broth with strong acid cation exchange resins that have a low degree of cross-linkage; and
• the method of the current invention utilizes a simulated moving bed (SMB) apparatus.
• SMB apparatus comprise multiple columns containing ion exchange resins are connected in series as shown in Figure 1.
• the locations of entry ports for feed and eluent, as well as the exit ports for product and raffinate, are changed periodically in the direction of the fluid flow in order to simulate counter current movement of resins with respect to the fluids.
• a portion of the product stream is recycled (l ⁇ iown as enrichment stream) back to the apparatus at the port next to the product exit port.
• the ports divide the apparatus into multiple zones.
• the apparatus consists of three zones, namely, the adsorption zone, the enrichment zone, and the elution zone.
• the adsorption zone includes the columns between feed entry port and raff ⁇ nate exit port.
• the elution zone consists of columns between eluent entry port and product exit port.
• the columns between the enrichment entry port and feed entry port constitute the enrichment zone.
• a 4-th zone, known as reload zone, is often used in order to minimize the solvent usage.
• SMB apparatus commercially available. These apparatus can be divided into two categories, namely, moving port system and moving column system (Barker,
• a preferred embodiment of the present invention provides a method for separating basic amino acids from fermentation broth.
• fermentation broths include but are not limited to liquors, or broths derived from beet molasses, cane molasses, or hydrolysates of starch or soy protein. Any of the fermentation broths may be filtered, or unfiltered.
• the present invention relates to methods for separating basic amino acids from fermentation broth using strong acid cation exchange resins with low cross- linkage.
• the present invention relates to strong acid cation exchange resins that are cross-linked less than about 8%.
• the method of the present invention employs strong acid cation exchange resins that are cross- linked from about 2 to 7%.
• the method of the present invention employs strong acid cation exchange resins that are cross-linked from about 4 to 6.5%, preferably about 4% or about 6.5%.
• strong acid cation exchange resins with a low degree of cross-linkage include, but are not limited to, SKI 04 (Mitsubishi), 4% cross-linkage, and GC480 (Finex), 6.5% cross- linkage.
• the current invention provides a method for separating basic amino acids from fermentation broth using a simulated moving bed apparatus, comprising contacting the fermentation broth with strong acid cation exchange resins with a low degree of cross-linking and an elution step.
• the elution step of the present invention comprises using about 1 to 7% NH 4 OH, more preferably about 2 to 5.1%, most preferably about 2.2%.
• a preferred embodiment of the present invention provides an elution step comprising an elution volume of less than about 3 bed-volumes. More preferably, the elution step of the present invention comprises an elution volume of about 1 to 2 bed volumes. Most preferably, the elution step of the present invention comprises about 1.2 bed volumes.
• the method of the current invention using strong acid cation exchange resins with a low degree of cross-linkage in a simulated moving bed apparatus, does not increase time for elution of the basic amino acids, as compared to higher cross- linked resins.
• Another preferred embodiment of the present invention provides a method for separating basic amino acids from fermentation broth.
• basic amino acid is used to mean any amino acid (natural, synthetic or modified) that has a positive charge at a neutral pH.
• the basic amino acids of the current invention that are separated from the fermentation broth are selected from the group comprising arginine, histidine and lysine. More preferably, the present invention provides for separating lysine from fermentation broth.
• strong acid cation exchange resins with a low degree of cross linkage When utilized in conjunction with SMB technology, strong acid cation exchange resins with a low degree of cross linkage have advantageous properties of higher dynamic capacity, faster exchange reaction rates and higher peak separation than the conventional basic amino acid separation resins with high cross-linkage.
• the combined effect of the unique properties of the strong acid cation exchange resins with a low degree of cross-linkage enable these resins to separate basic amino acids, specifically lysine, more effectively from fermentation broth. Operations using a simulated moving bed apparatus utilizing strong acid cation exchange resins with a low degree of cross-linkage result in higher throughput and higher concentration ratios as compared to operations using resins with a higher degree of cross-linkage.
• a preferred embodiment of the present invention provides a method for lysine separation from a fermentation broth resulting in the basic amino acid being about 85% or greater pure. More preferably, the purity of the basic amino acid from the separation method is about 86 to 100%, most preferably about 85%>, 93% or 95%.
• a preferred embodiment of the present invention provides a method for lysine separation from a fermentation broth resulting in a product yield of about 94%> or greater of the basic amino acid. More preferably, the basic amino acid product yield is about 98%> or greater, most preferably about 98% or 100%.
• a preferred embodiment of the present invention provides a method for separation of a basic amino acid from a fermentation broth resulting in a concentration ratio of the basic amino acid being about 0.8 to 2.0. More preferably, the concentration ratio of the basic amino acid from is about 1.0 to 1.8. As used herein, the term concentration ratio is defined as the concentration of the basic amino acid in the product, divided by the concentration of the basic amino acid in the feed.
• the resins used in this work were divided into two categories based on the degree of cross-linkage. Included in the first category were resins with a level of cross-linkage 8%> and higher, termed HX (high cross-linkage) resins. These resins are traditionally used in conventional lysine separation processes. Examples of HX resins are C100/1633 (Purolite) and T311 (Thermax). In the second category were resins with a level of cross-linkage lower than 8%, termed LX (low cross-linkage) resins. Examples of LX resins are SKI 04 (Mitsubishi) and GC480 (Finex).
• Simulated Moving Bed Operation Simulated Moving bed (SMB) experiments were conducted in 12 columns loaded with 300 ml of strong cation exchange resins and arranged in series with the configuration as shown in Figure 1. The flow rates of water and 14.5% of NH 4 OH were 6cc/min and
• HX and LX resins were evaluated in the SMB system at two levels of processing capacity.
• the higher level (HL) of processing refers to 8.0-8.4 gal/day of feed.
• the lower level (LL) of processing refers to 5.4-6.1 gal/day of feed.
• Table I compares the effectiveness of HX and LX resins in separating lysine from fermentation broths when the SMB was operated at HL level.
• Concentration Ratio (Concentration of lysine in product)/(Concentration of lysine in feed).
• Table I shows that LX resins produced significantly higher yields than HX resins.
• concentration ratios attained with LX resins were also higher than those with HX resins, and the lysine concentration in the product, obtained from LX resins, was higher than the feed stream. This is a significant benefit since it will reduce the cost of subsequent evaporation.
• Concentration Ratio (Concentration of lysine in product)/(Concentration of lysine in feed).
• Table II shows that the LX resins produced lysine product with higher yield and higher purity as compared to the HX resins. Most significantly, the values of concentration ratio attained with LX resins were considerably higher than those values attained with HX resins.
• Traditional SMB processes always result in a decreasing lysine concentration in the product stream, however, using resins with a low degree of cross-linldng, the concentration ratios are increased in the product stream.
• the higher dynamic capacity and faster uptake rate of the LX resins allowed higher fluid velocities in the adsorption zone of the SMB system with minimal loss of lysine in the waste stream.

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• Chemical & Material Sciences (AREA)
• Organic Chemistry (AREA)
• Preparation Of Compounds By Using Micro-Organisms (AREA)
• Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
• Fodder In General (AREA)

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• 2001
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