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• • C—CHEMISTRY; METALLURGY
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  • C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
  • C07H19/00—Compounds containing a hetero ring sharing one ring hetero atom with a saccharide radical; Nucleosides; Mononucleotides; Anhydro-derivatives thereof
  • C07H19/02—Compounds containing a hetero ring sharing one ring hetero atom with a saccharide radical; Nucleosides; Mononucleotides; Anhydro-derivatives thereof sharing nitrogen
  • C07H19/04—Heterocyclic radicals containing only nitrogen atoms as ring hetero atom
  • C07H19/06—Pyrimidine radicals
  • C07H19/067—Pyrimidine radicals with ribosyl as the saccharide radical
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D9/00—Crystallisation
  • B01D9/0063—Control or regulation
• • B—PERFORMING OPERATIONS; TRANSPORTING
  • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
  • B01D—SEPARATION
  • B01D9/00—Crystallisation
  • B01D9/02—Crystallisation from solutions
  • B01D9/04—Crystallisation from solutions concentrating solutions by removing frozen solvent therefrom
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  • C07D207/00—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
  • C07D207/02—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
  • C07D207/04—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members
  • C07D207/10—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
  • C07D207/16—Carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals
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  • C07D209/00—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom
  • C07D209/02—Heterocyclic compounds containing five-membered rings, condensed with other rings, with one nitrogen atom as the only ring hetero atom condensed with one carbocyclic ring
  • C07D209/04—Indoles; Hydrogenated indoles
  • C07D209/10—Indoles; Hydrogenated indoles with substituted hydrocarbon radicals attached to carbon atoms of the hetero ring
  • C07D209/18—Radicals substituted by carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals
  • C07D209/20—Radicals substituted by carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals substituted additionally by nitrogen atoms, e.g. tryptophane
• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
  • C07D—HETEROCYCLIC COMPOUNDS
  • C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
  • C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
  • C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
  • C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
  • C07D213/62—Oxygen or sulfur atoms
  • C07D213/63—One oxygen atom
  • C07D213/65—One oxygen atom attached in position 3 or 5
  • C07D213/66—One oxygen atom attached in position 3 or 5 having in position 3 an oxygen atom and in each of the positions 4 and 5 a carbon atom bound to an oxygen, sulphur, or nitrogen atom, e.g. pyridoxal
  • C07D213/67—2-Methyl-3-hydroxy-4,5-bis(hydroxy-methyl)pyridine, i.e. pyridoxine
• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
  • C07D—HETEROCYCLIC COMPOUNDS
  • C07D213/00—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members
  • C07D213/02—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members
  • C07D213/04—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom
  • C07D213/60—Heterocyclic compounds containing six-membered rings, not condensed with other rings, with one nitrogen atom as the only ring hetero atom and three or more double bonds between ring members or between ring members and non-ring members having three double bonds between ring members or between ring members and non-ring members having no bond between the ring nitrogen atom and a non-ring member or having only hydrogen or carbon atoms directly attached to the ring nitrogen atom with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
  • C07D213/78—Carbon atoms having three bonds to hetero atoms, with at the most one bond to halogen, e.g. ester or nitrile radicals
  • C07D213/79—Acids; Esters
  • C07D213/80—Acids; Esters in position 3
• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
  • C07D—HETEROCYCLIC COMPOUNDS
  • C07D239/00—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings
  • C07D239/02—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings
  • C07D239/24—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members
  • C07D239/28—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, directly attached to ring carbon atoms
  • C07D239/46—Two or more oxygen, sulphur or nitrogen atoms
  • C07D239/47—One nitrogen atom and one oxygen or sulfur atom, e.g. cytosine
• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
  • C07D—HETEROCYCLIC COMPOUNDS
  • C07D239/00—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings
  • C07D239/02—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings
  • C07D239/24—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members
  • C07D239/28—Heterocyclic compounds containing 1,3-diazine or hydrogenated 1,3-diazine rings not condensed with other rings having three or more double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, directly attached to ring carbon atoms
  • C07D239/46—Two or more oxygen, sulphur or nitrogen atoms
  • C07D239/52—Two oxygen atoms
  • C07D239/54—Two oxygen atoms as doubly bound oxygen atoms or as unsubstituted hydroxy radicals
• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
  • C07D—HETEROCYCLIC COMPOUNDS
  • C07D307/00—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom
  • C07D307/02—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings
  • C07D307/34—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members
  • C07D307/56—Heterocyclic compounds containing five-membered rings having one oxygen atom as the only ring hetero atom not condensed with other rings having two or three double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
  • C07D307/62—Three oxygen atoms, e.g. ascorbic acid
• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
  • C07D—HETEROCYCLIC COMPOUNDS
  • C07D339/00—Heterocyclic compounds containing rings having two sulfur atoms as the only ring hetero atoms
  • C07D339/02—Five-membered rings
  • C07D339/04—Five-membered rings having the hetero atoms in positions 1 and 2, e.g. lipoic acid
• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
  • C07D—HETEROCYCLIC COMPOUNDS
  • C07D473/00—Heterocyclic compounds containing purine ring systems
  • C07D473/02—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6
  • C07D473/04—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6 two oxygen atoms
• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
  • C07D—HETEROCYCLIC COMPOUNDS
  • C07D473/00—Heterocyclic compounds containing purine ring systems
  • C07D473/02—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6
  • C07D473/18—Heterocyclic compounds containing purine ring systems with oxygen, sulphur, or nitrogen atoms directly attached in positions 2 and 6 one oxygen and one nitrogen atom, e.g. guanine
• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
  • C07D—HETEROCYCLIC COMPOUNDS
  • C07D473/00—Heterocyclic compounds containing purine ring systems
  • C07D473/26—Heterocyclic compounds containing purine ring systems with an oxygen, sulphur, or nitrogen atom directly attached in position 2 or 6, but not in both
  • C07D473/28—Oxygen atom
  • C07D473/30—Oxygen atom attached in position 6, e.g. hypoxanthine
• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
  • C07D—HETEROCYCLIC COMPOUNDS
  • C07D473/00—Heterocyclic compounds containing purine ring systems
  • C07D473/26—Heterocyclic compounds containing purine ring systems with an oxygen, sulphur, or nitrogen atom directly attached in position 2 or 6, but not in both
  • C07D473/32—Nitrogen atom
  • C07D473/34—Nitrogen atom attached in position 6, e.g. adenine
• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
  • C07D—HETEROCYCLIC COMPOUNDS
  • C07D475/00—Heterocyclic compounds containing pteridine ring systems
  • C07D475/02—Heterocyclic compounds containing pteridine ring systems with an oxygen atom directly attached in position 4
  • C07D475/04—Heterocyclic compounds containing pteridine ring systems with an oxygen atom directly attached in position 4 with a nitrogen atom directly attached in position 2
• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
  • C07D—HETEROCYCLIC COMPOUNDS
  • C07D487/00—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00
  • C07D487/02—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, not provided for by groups C07D451/00 - C07D477/00 in which the condensed system contains two hetero rings
  • C07D487/04—Ortho-condensed systems
• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
  • C07D—HETEROCYCLIC COMPOUNDS
  • C07D495/00—Heterocyclic compounds containing in the condensed system at least one hetero ring having sulfur atoms as the only ring hetero atoms
  • C07D495/02—Heterocyclic compounds containing in the condensed system at least one hetero ring having sulfur atoms as the only ring hetero atoms in which the condensed system contains two hetero rings
  • C07D495/04—Ortho-condensed systems
• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
  • C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
  • C07H3/00—Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
  • C07H3/02—Monosaccharides
• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
  • C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
  • C07H3/00—Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
  • C07H3/04—Disaccharides
• • C—CHEMISTRY; METALLURGY
  • C07—ORGANIC CHEMISTRY
  • C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
  • C07H3/00—Compounds containing only hydrogen atoms and saccharide radicals having only carbon, hydrogen, and oxygen atoms
  • C07H3/06—Oligosaccharides, i.e. having three to five saccharide radicals attached to each other by glycosidic linkages

Definitions

• the present invention relates to an apparatus and method for isolating and purifying natural products of amino acids, dipeptides, tripeptides, nucleobases, nucleosides, saccharides, or vitamins. More specifically, in the present invention, when a natural product is concentrated and crystallized from a solution containing the natural product, the total amount of salt supplied to the concentrating device is measured and controlled to an appropriate concentration, thereby achieving high purity. An apparatus and a method for isolating and purifying natural products of the present invention are provided.
• Japanese Patent No. 2668956 discloses a high quality amino acid with a high recovery rate while solving the problem of wastewater treatment in a conventional method in which it is adsorbed on an ion exchange resin and eluted with an alkali for crystallization.
• a method that combines concentrated crystallization and cooling crystallization for isolation has been disclosed.
• Japanese Patent No. 3525126 discloses a concentrated crystallization method capable of obtaining amino acid crystals whose crystal polymorphism is controlled by utilizing a temperature difference.
• the concentrated product of natural products is usually used for additives when producing natural products by fermentation, and for acid treatment, alkali treatment or neutralization treatment when purifying natural products.
• Treatment agents used include strong electrolytes such as sodium sulfate, ammonium phosphate, and sodium chloride salt. For this reason, unless proper concentration control is performed, not only the target substance but also crystals of strong electrolytes are precipitated, and the purity of the target substance is lowered.
• Patent Document 1 Japanese Patent No. 2668956
• Patent Document 2 Japanese Patent No. 3525126
• An object of the present invention is to provide a method for isolating a natural product with stable quality at a high recovery rate by controlling an appropriate concentration even in continuous or feed batch type concentrated crystallization.
• the present invention relates to the following (1) to (14).
• Means for receiving the liquid to be concentrated, means for supplying the liquid to the means for receiving the liquid to be concentrated, and evaporation for performing the concentration process by evaporating the solvent of the liquid to be concentrated A concentrating device comprising means,
• the concentrating device according to (2) further comprising means having a function capable of monitoring the electrical conductivity, the supply flow rate, and the integrated value of the product of the electrical conductivity and the supply flow rate.
• the concentration method according to (4), wherein the liquid to be concentrated is a solution in which a nonelectrolyte or a weak electrolyte and a strong electrolyte coexist, and the nonelectrolyte or the weak electrolyte is concentrated and crystallized.
• the group of neutral amino acids is selected from serine, gnoretamine, alanine, leucine, norine, isoleucine, glycine, phenylalanin, proline, tyrosine, threonine, tryptophan, methionine, cystine, cystine and asparagine.
• concentration method described in (6) The concentration method described in (6).
• nucleobase is selected from the group power consisting of adenine, cytosine, guanine, hypoxanthine, thymine, uracil and xanthine.
• Nucleoside force The method according to (6), which is selected from the group consisting of adenosine, cytidine, guanosine, inosine and uridine.
• Vitamins include vitamin Bl, vitamin B2, vitamin B6, nicotinic acid, pantothenic acid, folic acid, piotin, inosole, kogin, vitamin B12, vitamin. (6).
• the concentration method according to (6) which is selected from the group consisting of vitamin Ll, vitamin P, paraaminobenzoic acid, lipoic acid, orotic acid, carcin and methylmethionine.
• the concentration apparatus of the present invention is a concentration can as a means for receiving a liquid to be concentrated. Further, a concentrated liquid supply pipe is provided as means for supplying the concentrated liquid to the means for receiving the concentrated liquid, and a heating apparatus and a vacuum apparatus are provided as evaporation means for performing a concentration process by evaporating the solvent of the concentrated liquid.
• concentrated crystallization of the liquid to be concentrated is performed by evaporating the solvent by heating, reduced pressure or reduced pressure heating.
• the concentrating device of the present invention comprises an electric conductivity meter for measuring the electric conductivity of the liquid to be concentrated and a flow meter for measuring the supply flow rate of the liquid to be concentrated to the means for receiving the liquid to be concentrated.
• the concentration of the liquid to be supplied be set to such a level that no crystals are present, so that the measurement of electrical conductivity does not occur abnormally for a long time. Can be measured. For this reason, the sensor of the electric conductivity meter is inaccurate due to the inaccuracy of the measurement value and the high concentration solution caused by the solid matter such as crystals generated in the concentration can as seen in the device having the electric conductivity meter inside the concentration can. Measurement anomalies caused by scaling that occurs in the unit and the problem does not occur!
• the electrical conductivity and the supply flow rate of the liquid to be concentrated are continuously measured.
• the product of the electrical conductivity and the supply flow rate indirectly represents the amount of salt supplied to the concentrate can per unit time. From the integrated value obtained by integrating this product from the concentration start time to a certain time, the total amount of salt supplied to the concentration can by that time can be determined.
• the integrated value force can determine the salt concentration of the liquid to be concentrated in the concentrating can at that time.
• the salt concentration of the liquid to be concentrated in the concentration can determined by measuring the electric conductivity is the concentration of the salt that is an impurity, that is, the strong electrolyte. Will represent. For this reason, it is possible to concentrate with stable quality by always keeping the salt concentration constant at the end of concentration crystallization. Further, the total amount of the maximum salt is determined in advance so that the salt does not precipitate as impurities and the purity of the obtained crystal does not decrease, and a predetermined value corresponding to the maximum amount of salt is set.
• the concentration process is terminated, so that the concentration is performed at a high concentration, and crystals with high purity can be produced with a high recovery rate.
• the target substance obtained by concentration is a substance that ionizes into an aqueous solution
• the salt concentration of the liquid to be concentrated in the concentration can determined by the measurement of the degree represents the concentration of the salt that is an impurity, that is, the strong electrolyte as it is.
• the target substance obtained by concentration is not weakly ionized, that is, less ionized in the liquid to be concentrated.
• the electrical conductivity resulting from the ionization of a part of the substance has almost no effect on the measurement of the electrical conductivity, so the inside of the concentration can determined by the measurement of the electrical conductivity.
• the concentration of the liquid to be concentrated in can be regarded as the concentration of the salt that is an impurity, that is, the concentration of the strong electrolyte. Therefore, as described above, high-concentration concentration is possible, and high-purity crystals can be produced with a high recovery rate.
• Examples of the weak electrolyte include substances having an ionization degree of not more than 0.05, preferably not more than 0.01 when dissolved in a concentrated solution at a concentration of ImolZL.
• the ionization degree when dissolved at a concentration of ImolZL in the liquid to be concentrated is 0.05 or less, preferably examples include the following substances: neutral amino acids, peptides, nucleobases, nucleosides, saccharides, or vitamins, preferably neutral amino acids, peptides, or saccharides. .
• neutral amino acid examples include serine, gnoretamine, alanine, leucine, parin, isomouth isine, glycine, phenylalanin, proline, tyrosine, threonine, tryptophan, methionine, cysteine, cystine, and asparagine.
• Examples of the peptide include dipeptides and tripeptides.
• Examples of the dipeptide include ara-glutglutamine, and examples of the tripeptide include dalthathion.
• nucleobase examples include adenine, cytosine, guanine, hypoxanthine, thymine, uracil, and xanthine.
• nucleosides examples include adenosine, cytidine, guanosine, inosine, and uridine. Is mentioned.
• saccharide examples include monosaccharides, oligosaccharides of 2 to 5 sugars, and oligosaccharides of 6 or more sugars.
• Vitamins include, for example, vitamin Bl, vitamin B2, vitamin B6, nicotinic acid, pantothenic acid, folic acid, piotin, inositol, choline, vitamin B12, vitamin C, vitamin Ll, vitamin P, paraaminobenzoic acid, lipoic acid, Examples include orotic acid, carcin, and methylmethionine.
• the strong electrolyte contained in the liquid to be concentrated has an ionization degree of 0.1 or higher, preferably 0.5 or higher when dissolved in the liquid to be concentrated at a concentration of 1 mol / L. More preferred is a substance of 0.7 or more, and most preferred is 0.9 or more, and examples thereof include inorganic and organic salts.
• sodium salt, ammonium salt, potassium salt, calcium salt and the like can be mentioned. Specific examples include sodium sulfate, sodium chloride salt, ammonium phosphate, ammonium sulfate, Examples thereof include inorganic salts such as ammonium chloride, ammonium phosphate, potassium sulfate, potassium chloride, and potassium phosphate.
• the liquid to be concentrated supplied by the method of the present invention may be any solution containing a non-electrolyte or a weak electrolyte and a strong electrolyte, but produces a non-electrolyte or a weak electrolyte.
• FIG. 1 is a schematic view of a concentrating device in the present invention.
• FIG. 2 is a block diagram of a concentration procedure in the present invention.
• FIG. 3 is a graph showing the relationship between the integrated value Q at the time of concentrated crystallization with L-neck Ishin in the present invention and the electrical conductivity of the concentrated treatment liquid. Explanation of symbols
• FIG. 1 shows a specific example of the concentrating device of the present invention.
• the concentrated liquid is supplied from the concentrated liquid tank 2 to the concentrated can 1 by the pump 3 through the concentrated liquid supply pipe 4.
• a flow meter 5 and an electrical conductivity meter 6 are attached to the concentrated liquid supply pipe 4, and the supply flow rate F and the electrical conductivity C of the concentrated liquid can be continuously measured.
• a vacuum device not shown
• the inside of the concentration can 1 can be decompressed via the vacuum pipe 10, and the solvent of the liquid to be concentrated can be evaporated at a low temperature. It is also possible to evaporate the solvent of the liquid to be concentrated by heating in a reduced pressure state.
• the amount of the liquid to be concentrated in the concentration can 1 is controlled by a liquid level gauge 11 attached to the side of the concentration can 1 so as to always maintain a constant liquid level.
• FIG. 2 shows the concentration procedure of the present invention.
• concentrate can 1 is depressurized and heated.
• the predetermined value V depends on the target substance for obtaining crystals and the components of the liquid to be concentrated containing the target substance.
• the predetermined value V the total amount of salt in the liquid to be concentrated to be placed in the concentration can 1 can be used directly.
• the product of the electrical conductivity and the total supply amount represents the total amount of salt indirectly supplied to the concentration can. Therefore, the product of electrical conductivity and total supply can be used as the predetermined value V.
• L-leucine was concentrated and crystallized by the Fuedbatch method using the method of the present invention.
• the electrical conductivity C of the L-necked Ishin solution was measured with an electrical conductivity meter (Smarter C CLD130, manufactured by Sakura Yendres Co., Ltd.).
• the electrical conductivity C of the concentrated treatment liquid in the concentration can 1 was measured.
• Figure 3 shows the relationship between the electrical conductivity C of the concentrated liquid and the integrated value Q. From this figure, concentration There is a correlation between the electrical conductivity C of the treatment liquid and the integrated value Q.
• Example 2 For comparison with Example 1, a conventional L-isoleucine concentration crystallization method will be described. Using the concentrator shown in Fig. 1, concentrated crystallization was performed by the Fuedbatch method. Under the measurement conditions, the maximum concentration at which L-isoleucine crystals do not precipitate is about 40 gZL, so the concentration of the supplied L-isoleucine solution was 35 g / L. In addition, this L-isoleucine solution contains sodium sulfate formed with sulfuric acid (36 mol / L) and sodium hydroxide (19 mol / L) added in the process up to obtaining the solution. .
• the concentration crystallization method of L-isoleucine by the method according to the present invention will be described.
• concentrated crystallization was performed using the Fuedbach method.
• the maximum concentration at which L-isoleucine crystals do not precipitate is about 40 gZL. Therefore, the concentration of the supplied L-isoloicine solution was set to 35 g / L.
• this L-isoleucine solution contains sodium sulfate formed by sulfuric acid (36 molZL) and sodium hydroxide (19 molZL) added in the process of obtaining the solution.
• the electrical conductivity of the L-isoleucine solution was measured with an electrical conductivity meter (Smarter C CLD130 manufactured by Sakura Endless Co., Ltd.).
• the product P of the electrical conductivity C (mS / cm) and the supply flow rate F (kLZh) was calculated every second, and the integrated value Q (kL'mSZcm) of the product P was calculated.
• the predetermined value V (kL'mSZcm) that was preliminarily input, the supply of the L-isoleucine solution was stopped and the concentration was completed.
• the preferred predetermined value for L-isoleucine The range of V is 700-800 kL'mSZcm In this example The predetermined value V was set to 750kL'mSZcm.
• the concentration of the L-norin solution to be supplied is set to 50 gZL. Since the maximum concentration at which L leucine crystals do not precipitate is about 25 gZL, the concentration of the supplied L leucine solution was 23 gZL.
• a preferable predetermined value V range for L-parin is 350 to 450 kL'mSZcm. In this example, the predetermined value V was set to 400 kL'mSZcm. Also, a preferable predetermined value V range for L leucine is 650 to 750 kL'mSZcm. In this example, the predetermined value V was set to 700 kL'mSZcm.

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• 2006
  • 2006-10-27 WO PCT/JP2006/321476 patent/WO2007049736A1/ja active Application Filing
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