GB2170198A - Process for the preparation of glutamic acid or the monosodium salt thereof - Google Patents

Process for the preparation of glutamic acid or the monosodium salt thereof Download PDF

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GB2170198A
GB2170198A GB08530897A GB8530897A GB2170198A GB 2170198 A GB2170198 A GB 2170198A GB 08530897 A GB08530897 A GB 08530897A GB 8530897 A GB8530897 A GB 8530897A GB 2170198 A GB2170198 A GB 2170198A
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glutamic acid
obtaining
liquors
msg
mother
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Pierre Henri Cami
Claude Marcel Renaud
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SANTERRE ORSAN
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/14—Ultrafiltration; Microfiltration
    • C—CHEMISTRY; METALLURGY
    • C05—FERTILISERS; MANUFACTURE THEREOF
    • C05F—ORGANIC FERTILISERS NOT COVERED BY SUBCLASSES C05B, C05C, e.g. FERTILISERS FROM WASTE OR REFUSE
    • C05F11/00—Other organic fertilisers
    • C05F11/08—Organic fertilisers containing added bacterial cultures, mycelia or the like
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C1/00—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon
    • 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
    • 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
    • C07C227/14—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof
    • C07C227/18—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof by reactions involving amino or carboxyl groups, e.g. hydrolysis of esters or amides, by formation of halides, salts or esters
    • 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
    • C07C227/28—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from natural products
    • 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
    • C07C227/42—Crystallisation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C229/00—Compounds containing amino and carboxyl groups bound to the same carbon skeleton
    • C07C229/02—Compounds containing amino and carboxyl groups bound to the same carbon skeleton having amino and carboxyl groups bound to acyclic carbon atoms of the same carbon skeleton
    • C07C229/04—Compounds containing amino and carboxyl groups bound to the same carbon skeleton having amino and carboxyl groups bound to acyclic carbon atoms of the same carbon skeleton the carbon skeleton being acyclic and saturated
    • C07C229/24—Compounds containing amino and carboxyl groups bound to the same carbon skeleton having amino and carboxyl groups bound to acyclic carbon atoms of the same carbon skeleton the carbon skeleton being acyclic and saturated having more than one carboxyl group bound to the carbon skeleton, e.g. aspartic acid
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00—Preparation of carboxylic acid esters
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P13/00—Preparation of nitrogen-containing organic compounds
    • C12P13/04—Alpha- or beta- amino acids
    • C—CHEMISTRY; METALLURGY
    • C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P13/00—Preparation of nitrogen-containing organic compounds
    • C12P13/04—Alpha- or beta- amino acids
    • C12P13/14—Glutamic acid; Glutamine

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  • General Engineering & Computer Science (AREA)
  • General Health & Medical Sciences (AREA)
  • Genetics & Genomics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Preparation Of Compounds By Using Micro-Organisms (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)

Abstract

Glutamic acid, or its sodium salt, in crystalline form is prepared from a fermented must containing glutamic acid by the steps of: subjecting the must to ultrafiltration to provide a permeate and a retained product, hydrolysing the retained product with a concentrated acid, filtering the product obtained by hydrolysis to obtain an acidic juice as filtrate, and mixing at least a portion of the acidic juice with the permeate to effect crystallization of the glutamic acid therefrom. The resultant crystalline glutamic acid may be purified, and converted to its sodium salt, which may then itself be crystallized.

Description

SPECIFICATION Process for the preparation of glutamic acid or the monosodium salt thereof The present invention concerns a process for the preparation of glutamic acid under the crystallized state (G.A.), preferably under the form of the sodium salt thereof or MSG; the G.A., MSG, the salts and organic concentrate obtained by said process.
The glutamic acid under the crystallized state, preferably under the form of the sodium salt thereof, or MSG is usually prepared through salification of glutamic acid, obtained, for instance, by industrial fermentation of several carbon sources. The purity of MSG is dependent among others from the purity obtained for the obtained acid extracted from the fermentation broth. Also, it is very important to have in a first step a process for extracting glutamic acid allowing to obtain a glutamic acid the purest possible in view of the preparation of a MSG of excellent quality.
Several different processes for the separation of glutamic acid from the fermentation broth have been proposed, including processes consisting in converting the glutamic acid into the hydrochlorate thereof or into the zinc salt thereof, processes using ion exchange resins or membranes, processes including extracting with the aid of solvents, etc. All these processes are little used at the industrial scale since they are complicated and need thereafter important refining steps of the final product.
A process known for its great simplicity and its economy lies in the concentration of the fermentation broth, then in the adding of hydrochloride or sulfuric acid, with the purpose to set the pH at a value near to the isoelectric point of the glutamic acid, performing thereby the neutralization thereof, which causes the crystallization of glutamic acid, and finally the separation of the crystals. Such a basic process is described in the Japanese patent application published after examination under number 59-14794 on January 25, 1984, filed under number 57-124260 on July 1982. This process comprises an ultrafiltration of the concentrated solution and gives an example of application to a lysine fermentation broth obtained by fermentation of sugar-beet molasses.
According to another process described in the Japanese patent application published under N 14795 on January 1984, based on Japanese patent application N" 125529 of July 19, 1982, it is performed a preliminary adjustment of the amino acid-containing fermentation broth to a pH ranging between 2 and 5 before performing a filtration. This process is applied to a glutamic acid fermentation must adjusted at a pH equal to 4.8 before the filtration as well as to a lysine-containing fermentation broth set to pH 4. It is set forth that this process improves the elimination of impurities.
According to a further other process described in Japanese patent application published under N" 12720 on January 1984, based on Japanese patent application N" 122450 of July 13, 1982, is is performed at first a preheating of the fermentation solution containing the amino acid at a temperature of 50-100 C, preferably 70-80"C to perform a denaturation and coagulation of the proteins contained in the solution before performing an ultrafiltration with an ultrafiltration membrane, which avoids the clogging of the ultrafiltration membrane.
According to a further other process described in Japanese patent application published under N" 12719 on January 1984, based on Japanese application 122449 of July 1982, it is described a process comprising the obtention of a highly concentrated amino-acid solution or highly concentrated monosodium glutamate also called MSG, the dilution of said solution to perform a maximal filtration and a filtration of the resulting diluted solution with an ultrafiltration membrane with the purpose to improve the efficiency of the filtration. It is given a filtration example of a solution of MSG at 20 gramsldecilitre. All these described processes do not allow to obtain a glutamic acid of an excellent purity.
It must be noted in this respect that the problems which are encountered to separate the glutamic acid are coming from the fact that the fermentation broth contains, aside the glutamic acid, important amounts of several impurities which must be discarded if it is wished to crystallize the glutamic acid in good conditions with the best possible purity.
The average composition of a broth obtained by fermentation of sugar-beet molasses is given in table I below.
TABLE I Broth 9000 1 Glutamicacid 1000kg Other soluble organic materials 740 kg Soluble inorganic materials 380 kg including K+ 130 kg NH4+ 100kg Ca++ 24 kg Mg++ 16kg Na+ 10kg Cl 60 kg S04 24 kg Others 6 kg Bacterial dry materials and other 180 kg insoluble materials 7600 kg Water Thus, the essential difficulties encountered during the crystallization of glutamic acid are coming from the presence: 1. of the bacterial cells which become pseudonucleus of crystals of glutamic acid, and which are lowering the crystallinity and cause a lowering of the purity of the crystallized glutamic acid.
If this type of impurities is not eliminated from the broth (as for instance in French patents N" 1 248 655 and 1 282773 of AJINOMOTO or even in GB-986738 AJINOMOTO where the cells are only separated after a first crystallization), it can be reached the formation of impure crystals of any size which can therefore be separated with great difficulties by the usual industrial economical processes.
When it is wished to separate the cells therefrom, the most usual means are: - The separation through centrifugation (as for instance in FR-A-1 335 193 ASAHI) but the use of a battery of centrifugation apparatuses is costly in energy; and/or - the filtration (as for instance in FR-A-1 250 507 AJINOMOTO) but the filtration of the fermentation broth is very difficult due to the fine bacterial cells and the materials in suspension within the broth, and this is necessarily costly in filtration adjuvent or aid.
In any way, irrespective of the used technique, namely the filtration and/or centrifugation, with the purpose of limiting the losses in glutamic acid within the filtration cake or the concentrate containing the cells, these must be washed, and it is therefore compulsory to introduce washing water which must be recycled and which will be necessarily evaporated during the concentration operation preceding the crystallization of glutamic acid, which causes a high energetic consumption.
2. The colloids which constitute another impurity which is particularly difficult to eliminate. These substances of a bad known nature are organic compounds insoluble or becoming insoluble during the extraction chain of glutamic acid or of preparation of MSG, particularly during the acidification or salification steps. They are perturbing the extracting steps and are polluting the glutamic acid or the obtained crystallized MSG. It is therefore necessary to try to eliminate them by filtration but this operation is difficult (filtration rates very low) and therefore very costly in filtration adjuvent or aid.
3. The soluble inorganic materials, including a particularly hindering ion: Ca.
Indeed, when the concentrated must is acidified, to cause the crystallization of glutamic acid, the acidification can be performed by HCI or H2SO4. H2SOA being of a well lower cost than HCI, it will be preferably used, but calcium is then precipitated under the form of a sulfate and this provides a pollution of the obtained glutamic acid crystals.
The main object of the present invention is therefore to solve the new technical problem lying in the preparation of glutamic acid underthe crystallized state, preferably under the form of the monosodic salt thereof also called MSG with an excellent purity with a relatively simple process usable at the industrial scale and with a reasonable energetic consumption.
Another main object of the present invention is also to solve the new technical problem lying in the recovery of the substances present aside the glutamic acid under a more reliable form which can be directly commercialized, thereby lowering sharply the cost of the process.
Said technical problems, as well as any other technical problem which will be apparent to one skilled in the art from the following description, are solved for the first time by the present invention. Thus, the present invention provides a process of preparation of glutamic acid under the crystallized state, preferably under the form of the sodium salt thereof also called MSG, from a fermented must containing said glutamic acid, comprising an ultrafiltration step of the fermented must, thereby obtaining a permeated product and a retained product, and an acidification step of the retained product, characterized in that it comprises, after the step of ultrafiltration of the fermented must, the following steps:: a) The permeated product is concentrated, preferably through evaporation, thereby obtaining a concentrated juice of glutamic acid as well as condensates; b) hydrolyzing the retained product by adding acid, preferably sulfuric acid, under concentrated state, thereby obtaining a hydrolyzed retained product; c) filtering the hydrolyzed retained product, thereby obtaining a filtration cake and a filtered acid juice; d) mixing at least a portion of said filtered acidic juice with said glutamic acid concentrated juice so as to crystallize the glutamic acid; and e) performing a filtration of the mixture obtaining thereby crystallization mother-liquors and a crude glutamic acid cake which is preferably purified.
Preferably, it is performed the purification of the glutamic acid by putting in suspension the crude glutamic acid in a washing water under stirring, at a temperature from 40 to 80"C during a sufficient period of time, preferably from 1 hour to 2 hours, then filtering the suspension thereby obtaining purified glutamic acid and washings.
Advantageously, it is performed the salification of glutamic acid, preferably under purified form, through addition thereto of saline water, then performing a further filtration thereby obtaining a monosodium glutamic acid mother-solution of MSG and finally performing the crystallization of MSG and preferably by concentrating, advantageously by evaporating.
Also, advantaueously, the crystals of MSG are separated from the crystallization mother-liquors and the MSG crystals are dried. The MSG crystals are obtained with an excellent purity, higher than that which was possible to be obtained according to the processes of the prior art.
According to a preferred feature of the invention process, the washings are recycled by adding them to the hydrolyzed retained product.
According to a preferred feature of the process according to the invention, the crystallization mother-liquors are in part recycled by using at least a portion thereof as a washing serving to the purification of the crude glutamic acid; advantageously, another portion of the crystallization mother-liquors is added to the saline water.
According to a further preferred feature of the invention process, the glutamic acid mother-liquors are neutralized with ammoniac, until obtaining a pH of about 6. Preferably, the mother-liquors neutralized with ammoniac are concentrated, advantageously by evaporating, to crystallize the sulfates which are separated therefrom, preferably by centrifugal drying, more preferably it is performed a further washing to obtain an organic concentrate commercializable in animal feed and salts commercializable as fertilizers or manures.
It can therefore be understood that with the invention process, it is obtained a MSG of an excellent purity, in good conditions of process, namely with a relatively low production cost, with simultaneously the recovery of products of a great commercial importance including an organic concentrate commercializable in animal feed and salts commercializable as fertilizers.
The present invention will be now described with respect to the actually preferred best mode of the production process of MSG according to the invention given merely by way of example and which cannot be construed as restricting the invention scope.
This example is given further with respect to the general scheme of the invention process set forth in table II by the end of the description.
Example At first, the fermented must obtained after fermentation of several carbon sources, for instance sugar-beet molasses, with a microorganism appropriate for the production of glutamic acid, for instance CORYNEBAC TERIUM MELASSECOLA, is, according to the invention process, directly submitted to an ultrafiltration step, performed with the aid of an inorganic membrane available on the market, set forth by the reference number 1 in table II, thereby obtaining on the one hand a permeate and, on the other hand, a retained product which contains the insoluble products under a concentrated state.
Thus, for 9000 litres of must, it is obtained: a) 7500 litres of permeate containing 850 kg of glutamic acid and 20 kg of calcium under the dissolved state; b) 1500 litres of retained product containing the bacterial bodies and other insoluble products, including the products under the colloidal state, kg of glutamic acid and 4 kg of calcium.
The process according to the invention is now performed as follows: a) The permeate is concentrated (in 2) by evaporation, thereby obtaining a glutamic acid concentrated juice as well as condensates.
At this evaporation step 2, 4600 kg of water are evaporated to obtain 3700 kg of concentrated juice not containing any insoluble particle, containing in major portion glutamic acid.
b) The retained product is hydrolyzed (in 3) by adding thereto sulfuric acid concentrated at 97% by adding 560 kg of sulfuric acid for 1500 kg of retained product. To perform the hydrolysis, the mixture of the insoluble materials is treated at the boiling temperature of the mixture, at the atmospheric pressure, and by the end of the hydrolysis, namely 3 to 5 hours after the beginning of the hydrolysis,925 of or water are evaporated.
It is thus obtained a hydrolysed retained product. The hydrolysis has rendered possible to free 13 kg of glutamic acid. It is thus obtained 1535 kg of hydrolysed retained product or hydrolysate containing 163 kg of glutamic acid and 4 kg of calcium.
c) According to the best mode of the invention process, as shown in table II, it is now added to the hydrolysate the solution having served to the washing of glutamic acid in 8, which will be described later, and which has been obtained at a preceding cycle, in a ratio of 1700 kg of solution for 1235 of hydrolysate.
The 1700 kg of solution contain 300 kg of glutamic acid and 19.5 kg of calcium under the dissolved state.
30 kg of filtration aid or adjuvent are added to the mixture which is then filtered in 4 at a temperature ranging between 20 and 30"C.
The filtration allows to discard the humic substances formed during hydrolysis, the calcium which has been precipitated by crystallizing of the dihydrated calcium sulfate, as well as the other insoluble materials.
constituting the filtration cake, and it is also obtained a filtered acidic juice or acidic filtrate.
The filtration cake is washed with 365 kg of water to obtain: i) 3000 kg of acidicfiltrate containing 457 kg of glutamic acid under the sulfate state and 1 kg of calcium; ii) 3000 kg of filtration cake containing 5kg of glutamic acid and 22.5 kg of calcium under the sulfate state.
d) It is mixed in 5 at least one portion of the filtered acidic juice obtained in 4 with the concentrated juice of glutamic acid obtained in 2 so as to crystallize the glutamic acid. Thus, it is mixed 3700 kg of concentrated juice for 3000 kg of acidic juice.
e) After crystallization of glutamic acid in 5, it is filtered in 6 the suspension of the mixture, thereby obtaining crystallization mother-liquors and a crude glutamic acid cake.
During this step, it is preferably performed a first purification by adding washing water.
For 6700 kg of suspension, it is added 300 kg of washing water to obtain: a) 1500 kg of crude glutamic acid cake containing 1157 kg of glutamic acid and 19.5 kg of calcium; b) 5500 kg of crystallization mother-liquors containing 150 kg of glutamic acid and 1.5 kg of calcium.
According to the preferred embodiment of the invention process, shown in table II, it is performed a purification of glutamic acid by putting in suspension the crude glutamic acid in a washing water. This washing water comprises at least a portion of the crystallization mother-liquors which are at least in part recycled from step 11 which will be described later.
Thus, it is performed a resuspension of the crude glutamic acid, this resuspension being maintained under stirring at a temperature ranging between 40 and 80"C during 1 hour to 2 hours to purify the crude glutamic acid.
For 1500 kg of glutamic acid cake obtained in 6, it is added 700 kg of softened water and 600 kg of crystallization mother-liquors of sodium glutamate containing 200 kg of glutamic acid.
The treatment causes dissolution of the calcium sulfate present in the crude glutamic acid cake, dissolution of 100 kg of glutamic acid and dissolution of the major portion of the dyeing products.
The suspension is then filtered in 8 and the cake is washed by softened water.
For 2800 kg of suspension obtained in 7, containing 1357 kg of glutamic acid and 19.5 kg of calcium, the purified glutamic acid cake is washed with 300 kg of softened water.
It is obtained: i) 1400 kg of purified glutamic acid cake containing 1057 kg of glutamic acid and less than 100 kg of calcium. On the basis of 100 parts of total dried materials, it is now obtained 98 parts of glutamic acid; ii) 1700 kg of washing solution of glutamic acid containing 19.5 kg of calcium under the dissolved state and 300 kg of glutamic acid.
This washing solution is preferably recycled in 4 for the filtration of the hydrolysate; g) now, the glutamic acid more preferably purified, is salified in 9 by adding thereto saline water.
Preferably, the mother-solution is discolored by adding thereto active carbon.
It is then performed a new filtration thereby obtaining a monosodium glutamic acid mother-solution of MSG mother-solution.
h) It is now performed a crystallization of monosodium glutamate or MSG through concentration, here through evaporation.
i) The crystals of MSG are separated from the crystallisation mother-liquors in 11, these mother-liquors being preferably recycled at least in portion to the purification step in 7 as washing water and in portion to the salification step in 9; it is further performed a drying of the crystals as usual.
Thus, for 1400 kg of purified glutamic acid cake in 9, containing 1057 kg of glutamic acid, it is obtained 1062 kg of dried MSG (i.e. for 1000 kg of glutamic acid in the must). This MSG has a purity equal to 99.7-99.8% and it is produced an excess of crystallization mother liquors of MSG of 600 kg containing 100 kg of glutamic acid.
It has been seen that these mother-liquors are in portion recycled in 7 and in portion in 9.
j) On the other hand, according to the invention process, the glutamic acid crystallization mother-liquors obtained in 6 are neutralized to a pH equal to about 6 by adding ammoniac, in 12.
k) It is thus performed in 13 a concentration, preferably by evaporation, of the neutralized mother-liquors.
For 5500 kg of crystallization mother-liquors, 3400 of water are evaporated.
I) It is then separated in 14 the crystallized salts, preferably by centrifugal drying and it is obtained after washing the salts with water: i) an organic concentrate directly commercializable in animal feed; ii) salts commercializable as fertilizer.
For 5500 kg of mother-liquors obtained in 6, it is obtained: a) 1600 kg of organic concentrate containing 72% of dried materials, 8.4% of total nitrogen, 4.9% of organic nitrogen and 3.5% of ammoniacal nitrogen; 720 kg of salts containing under the form of sulfates, 20.7% of K2O, 10.7% of nitrogen, 3.7% of Na2O.
It can therefore be seen that the invention process provides an unexpected remarkable technical progress, fully unobvious for one skilled in the art with respect to the prior known processes.
,RAZZLE
Fermented must 1 7 Permeate Retained product N2S9 97% Condensates 3 < CDndensates Eva orat2ion 3 H drol sis Condensates 2 1 ' 11 KM- at n Water ' B , liquors > < liquor) Crude glutamic > (lutamic acid mother liquors acid -Water NH3 NH3 > 7 + * , | 12 Water Filtration 8 J8 g )) Condensates l I CrvstalizationJ 13 ( purified glutamic acid) Water + Later+ soda Water Salification Se aration 14 4 Discoloration 9 ~ 4 l Filtrjation MSG | MSG Mother solution 5 1 L < %acennitcrate < Salts > lCrvstallizatio 10 concentrates/ 1 Mother liquors 2A < M.S.G.)

Claims (13)

1. Process of preparation of glutamic acid under the crystallized state, preferably under the form of the monosodium salt thereof or MSG, from a fermented must containing said glutamic acid, comprising an ultrafiltration step of the fermented must thereby obtaining a permeate and a retained product, and an acidification step, characterized in that it comprises, following the ultrafiltration step, the following steps:: a) Concentrating the permeate preferably by evaporation, thereby obtaining a glutamic acid concentrated juice as well as condensates; b) hydrolysing the retained product by adding thereto a concentrated acid, preferably sulfuric acid, thereby obtaining a hydrolysed retained product; c) filtering the hydrolysed retained product thereby obtaining a filtration cake and a filtered acidic juice; d) mixing at least a portion of said filtered acidic juice to said glutamic acid concentrated juice so as to crystallize the glutamic acid; and e) performing a filtration of the mixture thereby obtaining crystallization mother-liquors and a crude glutamic acid cake which is preferably purified.
2. The process of claim 1, characterized in that the purification of glutamic acid is performed by putting in suspension the crude glutamic acid in a washing water under stirring, at temperature ranging from 40 to 80"C during a sufficient period of time, preferably from 1 to 2 hours; then by filtering the suspension thereby obtaining purified glutamic acid and water washings.
3. The process of claim 1 or 2, characterized in that glutamic acid, preferably purified, is salified by adding thereto saline water, then it is performed a further filtration thereby obtaining a monosodium glutamic acid or MSG mother-solution and finally it is performed the crystallization of MSG, preferably by concentration, advantageously by evaporation.
4. The process of claim 3, characterized in that the crystals of MSG are separated from the crystallization mother-liquors and the MSG crystals are dried.
5. The process according to any one of claims 2 to 4, characterized in that the water washings are recycled by adding them to the hydrolyzed retained products.
6. The process according to claim 3,4 or 5, characterized in that the crystallization mother liquors are in portion recycled by using them at least in part as a washing serving for the purification of crude glutamic acid; advantageously another portion of the crystallization mother-liquors is added to the saline water.
7. The process according to any one of claims 1 to 6, characterized in that the g lutamic acid mother liquors are neutralized with ammonia, until obtaining a pH equal to about 6.
8. The process of claim 7, characterized in that the neutralized mother-liquors are concentrated, preferably by evaporation, to crystallize the sulfates which are separated therefrom, preferably by centrifugal drying, and it is preferably performed a washing to obtain an organic concentrate directly commercializable as well as salts also commercializable.
9. Monosodium glutamate or glutamic acid, characterized in that it is obtained from the process according to any one of claims 1 to 8.
10. The process substantially as described herein.
11. Monosodium glutamate substantially as described herein.
12. An organic concentrate suitable for use in animal feed whenever prepared by the process of claim 7 or8.
13. A fertilizer comprising salts prepared by the process of claim 7 or 8.
GB08530897A 1984-12-18 1985-12-16 Process for the preparation of glutamic acid or the monosodium salt thereof Expired GB2170198B (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
FR8419365A FR2574790B1 (en) 1984-12-18 1984-12-18 PROCESS FOR THE PREPARATION OF GLUTAMIC ACID IN THE PREFERRED CRYSTALLIZED CONDITION IN THE FORM OF ITS SODIUM SALT OR MSG; GLUTAMIC ACID, MSG, SALTS AND ORGANIC CONCENTRATE OBTAINED BY THIS PROCESS

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GB8530897D0 GB8530897D0 (en) 1986-01-29
GB2170198A true GB2170198A (en) 1986-07-30
GB2170198B GB2170198B (en) 1988-10-26

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JP (1) JPS61145150A (en)
KR (1) KR940000810B1 (en)
CN (1) CN1006067B (en)
BG (1) BG44028A3 (en)
BR (1) BR8506325A (en)
ES (1) ES8606249A1 (en)
FR (1) FR2574790B1 (en)
GB (1) GB2170198B (en)
HU (1) HU198675B (en)
IT (1) IT1190434B (en)
MX (1) MX7614E (en)
MY (1) MY102704A (en)
PH (1) PH22374A (en)

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FR2670090B1 (en) * 1990-12-10 1994-01-21 Orsan PROCESS FOR THE PREPARATION OF PROTEIN BASES FOR THE MANUFACTURE OF FLAVORS.
KR970027315A (en) * 1995-11-13 1997-06-24 손경식 Method for preparing sodium glutamate
CN1331922A (en) * 2001-02-22 2002-01-23 唐祯 Non-protein nitrogen feed additive
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CN1006067B (en) 1989-12-13
IT8523187A0 (en) 1985-12-13
CN85109246A (en) 1986-08-13
GB8530897D0 (en) 1986-01-29
GB2170198B (en) 1988-10-26
HU198675B (en) 1989-11-28
ES549907A0 (en) 1986-04-16
KR940000810B1 (en) 1994-02-02
BR8506325A (en) 1986-08-26
BG44028A3 (en) 1988-09-15
PH22374A (en) 1988-08-12
IT1190434B (en) 1988-02-16
ES8606249A1 (en) 1986-04-16
MX7614E (en) 1990-03-27
FR2574790A1 (en) 1986-06-20
HUT41375A (en) 1987-04-28
KR860004838A (en) 1986-07-14
FR2574790B1 (en) 1987-03-06
JPS61145150A (en) 1986-07-02
MY102704A (en) 1992-09-30

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