CN1312245A - Glutamic acid extracting process from fermentation liquid - Google Patents
Glutamic acid extracting process from fermentation liquid Download PDFInfo
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- CN1312245A CN1312245A CN 01105327 CN01105327A CN1312245A CN 1312245 A CN1312245 A CN 1312245A CN 01105327 CN01105327 CN 01105327 CN 01105327 A CN01105327 A CN 01105327A CN 1312245 A CN1312245 A CN 1312245A
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Abstract
The method for extracting glutamic acid from fermenting liquor is characterized by adding glutamic acid fermenting liquor to glutamic acid high fraction whose pH value is less than isoelectric point of glutamic acid until the pH value is reached to isoelectric point of glutamic acid. The adoption of said method can prevent the protein and colloid matter being in fermenting liquor from precipitating in the course of downward-regulating pH value, and does not produce glutamic acid negative ion in the course of neutralization so as to inhibit formation of beta-glutamic acid. Said invention method also is suitable for extracting glutamic acid from fermenting liquor with high acid-forming rate.
Description
The present invention relates to from fermented liquid, extract the method for L-glutamic acid, more particularly, relate to the method for from fermented liquid, extracting L-glutamic acid by anti-accent iso-electric point.
It is most popular a kind of method both at home and abroad that fermentation method is made L-glutamic acid, and its manufacturing processed is divided into starch hydrolysis, seed culture, fermentation, extraction, several operations such as refining substantially.When domestic manufacturer extracts L-glutamic acid from fermented liquid, generally be subjected to the restriction of present existing device and technology, not first separating thallus, but directly from contain thalline and proteinic fermented liquid, extract L-glutamic acid.
Isoelectric point method is the simplest a kind of method in the glutamic acid extraction method.This method is easy and simple to handle, and equipment is simple, less investment.Extract yield of L-glutamic acid with this method and can reach 60-70%.At normal temperatures, also contain about 1.8% L-glutamic acid in the iso-electric point mother liquor.Present domestic most of factory all adopts this method.The principle of this method is, L-glutamic acid is when iso-electric point, and positive and negative charge equates that promptly, total static charge equals zero.The dipole ion that forms promptly can anode not move in DC electric field, can not move to negative electrode yet, at this moment, because the intermolecular mutual collision of L-glutamic acid, and the effect by electrostatic attraction, the L-glutamic acid molecule can be combined into bigger polymer and be easy to precipitation and separate out.Therefore, when iso-electric point, the solubleness minimum of L-glutamic acid.Isoelectric point method has utilized this character exactly.
Glutamic acid fermentation finishes, put jar after, generally about 6.5-7.0, at this moment, in this fermented liquid, L-glutamic acid exists with the form of monoammonium glutamate the pH of fermented liquid, this ammonium salt is by the NH in L-glutamic acid and the substratum
3Reaction and form.The solubleness of monoammonium glutamate is very big, therefore, must just can make the solubleness of L-glutamic acid in fermented liquid drop to minimum with pH regulator to iso-electric point.Extract in the operation of L-glutamic acid at isoelectric point method, along with the reduction that adds acid for adjusting pH value and temperature, when L-glutamic acid moved closer to iso-electric point, the L-glutamic acid in the solution can carry out the transition to hypersaturated state from undersaturated condition, and excessive solute (being L-glutamic acid) just can be separated out in crystallization.
But can contain various impurity such as residual sugar, other amino acid, polypeptide class, thalline and colloidalmaterial in the fermented liquid, wherein, as contained isoelectric point of protein in the corn of fermentation raw material, the rice all between pH4.2-4.8.Impurity such as many colloidalmaterials and tropina also can precipitate during adding acid is adjusted to fermented liquid pH L-glutamic acid from pH6.5-7.0 the process of iso-electric point about 3.22, thereby produce problems such as neutralization is difficult, filtration is difficult, L-glutamic acid separates difficulty with thalline, yield is low, even may cause that feed liquid sends out paste, can't separate.And the glutamic acid crystallization of producing often accompanies impurity and colloidalmaterial, becomes " light bran acid " or " slurry ".In addition, when from about pH6.5-7.0, being reduced to glutamic acid solution near the L-glutamic acid iso-electric point with existing method, also form β-type crystallization easily, and β-type crystallization is needle-like or lepidiod grain, its light weight, particle is little, purity is low, often be suspended in after the crystallization in the fermented liquid, difficult sedimentation, difficult precipitation is separated out.In addition, since nineteen ninety-five, the acid production rate of glutamic acid fermentation method has had further raising, brings up to about 12-15% from the past about 8-10%.But along with the raising of acid production rate, existing method adopted adds sour neutralization operation and exists that degree of supersaturation is too high, graining is put unmanageable problem.
Contamination precipitation and β-problems such as L-glutamic acid generation such as protein, colloid in the process of the downward modulation fermented liquid pH that exists in the method in view of present iso-electric point extraction L-glutamic acid, the present inventor has carried out deep research, found that the anti-iso-electric point of transferring can solve the above-mentioned problems in the prior art.
The object of the present invention is to provide a kind of by anti-method of transferring iso-electric point from fermented liquid, to extract L-glutamic acid.Can avoid protein in the fermented liquid and colloidalmaterial etc. in pH downward modulation process, to precipitate in this way, and, in N-process, can not produce the L-glutamic acid negative ion, generate thereby can suppress β-L-glutamic acid.
The present invention also aims to provide a kind of method that is fit to from the fermented liquid of high acid rate, extract L-glutamic acid.
The invention provides a kind of iso-electric point and extract the method for L-glutamic acid, it is characterized in that, glutami acid fermentation liquor is joined pH be lower than in the high flow point of L-glutamic acid of L-glutamic acid iso-electric point, reach the iso-electric point of L-glutamic acid until whole pH.
In the method for the invention, the high flow point of above-mentioned L-glutamic acid is the mother liquor through the glutami acid fermentation liquor of ion exchange method processing.
In the method for the invention, reduce the pH value of the high flow point of above-mentioned L-glutamic acid in advance with acid.
In the method for the invention, be reduced to below 1.0 with the pH value of acid in advance the high flow point of above-mentioned L-glutamic acid.
In the method for the invention, be reduced to 0.8-1.0 with sour pH value in advance with the high flow point of above-mentioned L-glutamic acid.
Fig. 1 shows that existing iso-electric point extracts the schematic flow sheet of key step of the method for L-glutamic acid.
Fig. 2 shows that anti-accent iso-electric point of the present invention extracts the schematic flow sheet of key step of the method for L-glutamic acid.
As shown in Figure 1, extract in the method for glutamic acid in existing isoelectric point, after glutamic acid fermentation is complete, by the centrifugal thalline etc. (also can without this step) of removing in advance, then zymotic fluid is entered in the isoelectric point tank (pond) its temperature of sampling and measuring, pH value and content of glutamic acid. Then stir and cool off, add an amount of high flow point of glutamic acid. When treating that temperature is down to below 30 ℃, use acid for adjusting pH value. When mash is in saturation state (what decide according to producing acid, generally produce acid 6% when above, and pH is between 4.0-4.5), input crystal seed (amount of charging seed be content of glutamic acid about 2%). Then stop acid and educated brilliant 1-2 hour, make the nucleus growth. Follow slow acid adding, until pH be adjusted to the isoelectric point (between about 3.0-3.2) of glutamic acid constant till. Continue to stir about 20 hours, then stop to stir, left standstill 4-6 hour, make the glutamic acid crystallization sedimentation. After taking out glutamic acid crystallization, mother liquor is sent to the ion exchange resin column upper prop, allows glutamic acid absorption, then with alkali lye with the glutamic acid wash-out. According to the variation of elution process pH and Baume degrees, understand the amount of glutamic acid in the efflux, Fractional Collections. About the pH of efflux reaches 2.5, when Baume degrees is 1 ° of B é, content of glutamic acid is higher, begins to collect peak liquid (high flow point) this moment. The average content of glutamic acid of high flow point is about 5-7%. A certain amount of high flow point of collecting is incorporated in another batch fermentation liquid, is used for next time isoelectric point extraction glutamic acid. Before going in being incorporated into zymotic fluid, acid adding is adjusted to pH1.5 with high flow point so that high flow point can play the effect of pickle simultaneously usually, thereby the pH slow decreasing of energy controlled fermentation liquid also reaches isoelectric point exactly.
As previously mentioned, extract in the method for glutamic acid in existing isoelectric point, after being incorporated into a certain amount of high flow point (pH1.5) that is obtained by ion-exchange in the zymotic fluid (pH6.5-7.0), need with acid the gained material liquid pH value to be reduced to the isoelectric point (about 3.2) of glutamic acid, when the pH of feed liquid value is between 4.2-4.8, the contamination precipitations such as protein and colloidal substance can appear, be easy to generate β type glutamic acid, and, when the aminoglutaric acid concentration in the feed liquid reaches 10% when above, can't normal operating with existing isoelectric point extracting method.
Method of the present invention is to extract glutamic acid by anti-accent isoelectric point. That is, glutami acid fermentation liquor (its pH value is usually between 6.5-7.0) is joined in the high flow point of glutamic acid that the pH value is lower than the glutamic acid isoelectric point, until the pH value of mixed liquor reaches the glutamic acid isoelectric point gradually. Be preferably, before mixing zymotic fluid, be reduced to below 1.0 with the pH value of acid with high flow point in advance, be more preferably, be reduced in advance pH0.8-1.0.
In the method for the invention, owing to be glutami acid fermentation liquor (pH6.5-7.0) to be joined in the high flow point of glutamic acid that pH value is lower than the glutamic acid isoelectric point (preferably being adjusted in advance below the pH0.8-1.0) gradually go, extract in the operating process of glutamic acid in isoelectric point, the pH value of glutamic acid solution rises gradually from pH0.8-1.0, reach at last the isoelectric point (about pH3.0-3.2) of glutamic acid, thereby avoided dexterously the easily scope of the pH4.2-4.8 of precipitation of the impurity such as the protein in the zymotic fluid, colloidal substance, overcome the problems referred to above that exist in the existing method.
In the present invention, above-mentioned glutami acid fermentation liquor is particularly limited without any, for example, can be that the starch materials such as cornstarch, potato starch, rice starch and wild plant starch undergo microbial fermentation and the zymotic fluid that obtains, also can be the zymotic fluid that molasses, brown granulated sugar etc. contain the glycogen material.
Above-mentioned " the high flow point of glutamic acid " word is the general term in this area, has the known implication of those of ordinary skill in the art, refer to contain the flow point of high concentration of glutamate, more particularly, refer to extract behind the glutamic acid in the zymotic fluid flow point that contains high concentration of glutamate of mother liquor being processed through ion-exchange and obtaining with isoelectric point method. According to design of the present invention and purpose, the overall ph value of the collected high flow point of glutamic acid should be lower than the isoelectric point of glutamic acid, usually should can optionally adjust below pH4.0, preferably should be adjusted to pH0.8-1.0 by high flow point with acid in advance. In the present invention, the high flow point of described glutamic acid also can be any contain high concentration of glutamate, the pH value is lower than other solution of glutamic acid isoelectric point (or at least below pH4.0). Described high concentration is generally between the 5-7%, but also can a little more than or be lower than this scope.
In the present invention, the acid that is used for regulator solution pH value can be fermentation industry any acid commonly used, for example, can be the inorganic acids such as hydrochloric acid, sulfuric acid, phosphoric acid, also can be the organic acids such as acetic acid, propionic acid. But because the factors such as acid intensity and price are used the inorganic acids such as hydrochloric acid, sulfuric acid usually, wherein, sulfuric acid is because it is cheap and buy easily and the most frequently used. The consumption of acid is decided according to the acid production rate of zymotic fluid, and during with the sulfuric acid neutralise broth, its use amount is equivalent to about 1.35-1.54% (volume) of zymotic fluid usually.
In the present invention, the alkali that is used for regulator solution pH value can be mineral alkali, also can be organic bases, but because factors such as alkaline intensity and price, usually use mineral alkalis such as liquefied ammonia, ammoniacal liquor, sodium hydroxide, potassium hydroxide, wherein, the most frequently used is liquefied ammonia, ammoniacal liquor and sodium hydroxide.
The volume ratio of fermented liquid and high flow point can be decided according to the pH value of fermented liquid and high flow point and aminoglutaric acid concentration separately by those skilled in the art, but usually between 2: 1 to 3: 2.
In the method for anti-accent iso-electric point of the present invention, because the pH value being adjusted in advance in the fermented liquid that 1.5 the high flow point of L-glutamic acid is incorporated into pH6.5-7.0 and adding method that pH value that acid makes the gained feed liquid is reduced to the L-glutamic acid iso-electric point gradually of just will using always at present changes fermented liquid with pH6.5-7.0 into and is incorporated into the iso-electric point of the pH value of anti-flavouring liquid in the high flow point of L-glutamic acid that the pH value is adjusted to 0.8-1.0 in advance to L-glutamic acid, and all the other operations are identical with existing method, therefore, add sour speed when in the present invention, adjusting pH, cooling rate, whole pH value, warm eventually, stirring state, educate brilliant situation and crystal seed play that crystalline form etc. influences the operational condition of glutamic acid crystallization and recovery rate and existing method is identical or those of ordinary skill in the art can easily make corresponding selection or determined according to purpose of the present invention.
Great advantage of the present invention is to have improved the purity and the generation of having avoided β-glutamic acid crystallization of glutamic acid crystallization.In the present invention, owing to be that fermented liquid is incorporated into pH value anti-iso-electric point of transferring in the high flow point of L-glutamic acid of (especially below pH1.0) below the iso-electric point, therefore, avoided the scope of the easy sedimentary pH4.2-4.8 of impurity such as the protein in the fermented liquid, colloidalmaterial dexterously, eliminated of the influence of above-mentioned impurity glutamic acid crystallization.In addition, those skilled in the art knows that the generation of β-glutamic acid crystallization is relevant with the L-glutamic acid negative ion concentration, and the concentration of L-glutamic acid negative ion depends on the pH value of solution.In the table 1 below, listed the β-L-glutamic acid negative ion concentration in the various pH value solution.In existing method, owing to be the iso-electric point (about pH3.22) that the solution of L-glutamic acid is reduced to L-glutamic acid from pH6.5-7.0, in the process of turning down the pH value, L-glutamic acid in the solution can carry out the transition to hypersaturated state from undersaturated condition, from about pH5.0, excessive solute (that is, L-glutamic acid) just can be separated out by graining, but when pH4.0-5.0, L-glutamic acid major part in the solution exists with the form of negative ion, thereby cause the generation of β-glutamic acid crystallization, and as previously mentioned, β-type crystallization is needle-like or lepidiod grain, its light weight, particle is little, purity is low, often be suspended in after the crystallization in the fermented liquid, difficult sedimentation, difficult precipitation is separated out.Method of the present invention is the anti-iso-electric point of transferring, and the pH value of feed liquid is adjusted to gradually the iso-electric point (pH3.0-3.2) of L-glutamic acid from pH0.8-1.0.As shown in table 1, below pH3.0, do not exist or only have the β-type L-glutamic acid of trace to exist in the solution.
Table 1
| Existing method | ???pH4.0 | ????4.25 | ????4.5 | ????4.75 | ????5.0 |
| L-glutamic acid negative ion % | ???35.63 | ????49.78 | ????63.99 | ????77.90 | ????84.87 |
| Method of the present invention | ???pH1.0 | ????1.5 | ????2.0 | ????2.5 | ????3.0 |
| L-glutamic acid negative ion % | ???- | ????- | ????0.43 | ????1.17 | ????4.64 |
In addition, another advantage of the inventive method is to be suitable for the high fermented liquid of acid production rate.In the past, when the L-glutamic acid that reclaims with ion exchange method in the mother liquor, the L-glutamic acid content in the elutriant was about 5%, and volume is about 50% of fermented liquid.Use acid (as H as high flow point above-mentioned elutriant
2SO
4) transfer to pH1.5 after, with 1: 2 volume ratio high flow point being joined L-glutamic acid content is that the aminoglutaric acid concentration of gained feed liquid correspondingly drops to (10 * 2+5 * 1)/3=8.33% when waiting charge neutrality in 10% the fermented liquid.At this moment, can operate with existing method.And at present the fermentation and acid rate of L-glutamic acid has been brought up to 12-14% from the past 8-10%, during with charge neutrality such as existing methods, the aminoglutaric acid concentration of feed liquid correspondingly increases to (12 * 2+5 * 1)/3=9.67% to (14 * 2+5 * 1)/3=11%, add in the acid and the time exist that degree of supersaturation is too high, graining is put unmanageable problem.Therefore, can't normal running with existing method.The present invention adopts the method for anti-accent iso-electric point, is adjusted to from tart pH1.0 about the pH3.0 of L-glutamic acid iso-electric point, thereby does not have the existing existing problem of method, can successfully operate.
Under room temperature naturally cooling condition, along with the rising of L-glutamic acid content, β-type crystallization increases, and L-glutamic acid contains moisture and also can increase, and causes crystal and feed liquid to be difficult to separate, and the purity of L-glutamic acid also can descend.Shown in following table 2, when using existing iso-electric point extracting method, when aminoglutaric acid concentration increases gradually, β-crystallization also correspondingly increases, and use the method for anti-accent iso-electric point of the present invention, even then under the situation of the L-glutamic acid that contains high density, do not have yet or only have the β-L-glutamic acid of trace to exist.
Table 2
| Existing method | L-glutamic acid | ????8％ | ????10％ | ????15％ |
| β-L-glutamic acid | ????20％ | ????58％ | ????100％ | |
| Method of the present invention | L-glutamic acid | ????10％ | ????12％ | |
| β-L-glutamic acid | Do not have | Trace |
In addition, method of the present invention is applicable to the existing employed equipment of method, do not need to renovate, and the operating time shorten more than 1/3, thereby improved equipment capacity.
Embodiment 1
The past high flow point 200mL of L-glutamic acid (L-glutamic acid content is 5%, pH1.5) the middle sulfuric acid 7mL that adds, and (L-glutamic acid content is 9.3%, and pH6.7) 519mL is 3.2 until whole pH value, and this moment, temperature rose to 23 ℃ to add glutami acid fermentation liquor more gradually.Feed temperature is cooled to 7 ℃, and the glutamic acid crystallization that leaching is separated out all is the crystallization of α type.L-glutamic acid content in the mother liquor is 2.08%.
Embodiment 2
The past high flow point 200mL of L-glutamic acid (L-glutamic acid content is 5%, pH1.5) the middle sulfuric acid 6.2mL that adds, and (L-glutamic acid content is 9.8%, and pH6.7) 445mL is 3.2 until whole pH value, and this moment, temperature rose to 22 ℃ to add glutami acid fermentation liquor more gradually.Feed temperature is cooled to 7 ℃, and the glutamic acid crystallization that leaching is separated out all is the crystallization of α type.L-glutamic acid content in the mother liquor is 1.81%.
Embodiment 3
The past high flow point 200mL of L-glutamic acid (L-glutamic acid content is 5%, pH1.5) the middle sulfuric acid 7mL that adds, and (L-glutamic acid content is 12.06%, and pH6.7) 460mL is 3.2 until whole pH value, and this moment, temperature rose to 23 ℃ to add glutami acid fermentation liquor more gradually.Feed temperature is cooled to 7 ℃, and the glutamic acid crystallization that leaching is separated out all is the crystallization of α type.L-glutamic acid content in the mother liquor is 2.25%.
Embodiment 4
The past high flow point 200mL of L-glutamic acid (L-glutamic acid content is 5%, pH1.5) the middle sulfuric acid 7.4mL that adds, and (L-glutamic acid content is 13.1%, and pH6.4) 480mL is 3.2 until whole pH value, and this moment, temperature rose to 25 ℃ to add glutami acid fermentation liquor more gradually.Feed temperature is cooled to 7 ℃, and the glutamic acid crystallization that leaching is separated out all is the crystallization of α type.L-glutamic acid content in the mother liquor is 2.34%.
Claims (5)
1. extract the method for L-glutamic acid, it is characterized in that, glutami acid fermentation liquor is joined the pH value be lower than in the high flow point of L-glutamic acid of L-glutamic acid iso-electric point, reach the iso-electric point of L-glutamic acid until whole pH.
2. the method for claim 1 is characterized in that, the high flow point of above-mentioned L-glutamic acid is the mother liquor through the glutami acid fermentation liquor of ion exchange method processing.
3. method as claimed in claim 1 or 2 is characterized in that, reduces the pH value of the high flow point of above-mentioned L-glutamic acid in advance with acid.
4. method as claimed in claim 3 is characterized in that, is reduced to below 1.0 with the pH value of acid with the high flow point of above-mentioned L-glutamic acid in advance.
5. method as claimed in claim 4 is characterized in that, is reduced to 0.8-1.0 with sour pH value with the high flow point of above-mentioned L-glutamic acid in advance.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008140023A1 (en) * | 2007-05-14 | 2008-11-20 | Ajinomoto Co., Inc. | METHOD FOR PRECIPITATING α-CRYSTALS OF GLUTAMIC ACID |
| CN101367744B (en) * | 2008-08-30 | 2012-01-11 | 宝鸡阜丰生物科技有限公司 | Method for extracting glutamic acid |
| CN103045670A (en) * | 2012-12-23 | 2013-04-17 | 菱花集团有限公司 | Recycling process for monosodium glutamate fermentation water sample |
| CN113121376A (en) * | 2021-04-12 | 2021-07-16 | 梁山菱花生物科技有限公司 | Preparation method of glutamic acid |
-
2001
- 2001-02-13 CN CN 01105327 patent/CN1312245A/en active Pending
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2008140023A1 (en) * | 2007-05-14 | 2008-11-20 | Ajinomoto Co., Inc. | METHOD FOR PRECIPITATING α-CRYSTALS OF GLUTAMIC ACID |
| US20100094048A1 (en) * | 2007-05-14 | 2010-04-15 | Hidetada Nagai | Method of producing alpha-form glutamic acid crystals |
| US8198478B2 (en) | 2007-05-14 | 2012-06-12 | Ajinomoto Co., Inc. | Method of producing alpha-form glutamic acid crystals |
| CN101679212B (en) * | 2007-05-14 | 2014-10-22 | 味之素株式会社 | Method for precipitating a-crystals of glutamic acid |
| CN101367744B (en) * | 2008-08-30 | 2012-01-11 | 宝鸡阜丰生物科技有限公司 | Method for extracting glutamic acid |
| CN103045670A (en) * | 2012-12-23 | 2013-04-17 | 菱花集团有限公司 | Recycling process for monosodium glutamate fermentation water sample |
| CN103045670B (en) * | 2012-12-23 | 2014-04-09 | 菱花集团有限公司 | Recycling process for monosodium glutamate fermentation water sample |
| CN113121376A (en) * | 2021-04-12 | 2021-07-16 | 梁山菱花生物科技有限公司 | Preparation method of glutamic acid |
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