CN1048702A - A kind of method of extracting L-glutamic acid - Google Patents
A kind of method of extracting L-glutamic acid Download PDFInfo
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- CN1048702A CN1048702A CN 90102179 CN90102179A CN1048702A CN 1048702 A CN1048702 A CN 1048702A CN 90102179 CN90102179 CN 90102179 CN 90102179 A CN90102179 A CN 90102179A CN 1048702 A CN1048702 A CN 1048702A
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Abstract
The invention provides a kind of method of extracting L-glutamic acid.The inventive method is made up of following steps, employing has the flocculation agent of cationic characteristic and removes the fermented liquid colloid, isoelectric fractionation goes out crystallization L-glutamic acid and isoelectric point crystallizing mother liquor, concentrates isoelectric point crystallizing mother liquor at twice, and isoelectric fractionation goes out crystallization L-glutamic acid and final enriched material.The inventive method can obtain the high L-glutamic acid result of purity, and its L-glutamic acid total recovery can reach 90%, final enriched material with in the ammoniacal liquor and after directly become farming fertilizer with commodity value, realize no discharging of waste liquid, solved environmental pollution problem.
Description
The present invention relates to a kind of method of extracting L-glutamic acid, it comprises removes fermented liquid colloid, protein, thalline step, and iso-electric point is extracted L-glutamic acid and obtained the step of final enriched material.
The monosodium glutamate that is used as seasonings in the daily life is a L-Sodium Glutamate salt, and L-glutamic acid can be raw material by starch, molasses, carries out industrialness with biological culturing method and produces acquisition.
The method of extracting L-glutamic acid at present from fermented liquid has isoelectric point method, hydrochloride method, zincate process, ion-exchange-resin process, direct method of enrichment.L-glutamic acid is when isoelectric pH, and solubleness is minimum in solution.But in fermented liquid, owing to be subjected to impurity effects such as residual sugar, protein, pigment, hindered glutamic acid crystallization, so the glutamic acid crystallization purity that isoelectric point method extracts from fermented liquid is restricted, and its yield also has only 60%, can bring up to 70% if cooperation is freezing, carry out ion exchange resin absorption again, then can reach 80%.As the glutamic acid crystallization mother liquor of discharge of wastewater, its L-glutamic acid content still reaches 1.3 grams more than/100 milliliters.
In the method that includes several extraction L-glutamic acid of removing fermented liquid colloid, protein, thalline and these two steps of concentrated broth, separating out, improving the glutamic acid crystallization purity of impurity followed in minimizing when reducing foamy interference and iso-electric point sedimentation glutamic acid crystallization during concerning concentrated broth, and colloid, protein, the thalline at first removed in the fermented liquid are vital.
Having narrated a kind of technology in the Chinese patent application numbers 85109246 is to adopt commercially available mineral membrane to carry out super filtration, but its filtration time is long, and mineral membrane costs an arm and a leg, and super filtering operation is also pretty troublesome.Shanghai Gourmet Powder Factory writes, the direct method of enrichment of introducing in " glutamate production " book that nineteen eighty-two is published by light industry press is to adopt supercentrifuge separate fermentation liquogel, protein, the thalline of 6000～15000 rev/mins of turn ups, and its equipment price costliness, energy consumption are big.
Because aminoglutaminic acid thalline is little, the method removal colloid of common industrial economy, protein, thalline will have very big difficulty.
More existing glutamic acid extraction methods as isoelectric point method, ion exchange method, zincate process, ion-exchange membrane electrodialysis method, are not all removed the processing step of colloid in the fermented liquid, protein, thalline.
Chinese patent application is narrated by numbers 85109246 li, contains/100 milliliters of L-glutamic acid 11 grams in the fermented liquid that is concentrated, and its concentration ratio is 2.4: 1.
In the direct method of enrichment that " glutamate production " book is introduced, the fermented liquid L-glutamic acid content that is concentrated is/100 milliliters of 7～10 grams, and its concentration ratio is selected in 4～5: 1.
Should be noted that, the L-glutamic acid content of above-mentioned fermented liquid restrains more than/100 milliliters 7, if choose high concentration ratio, make the L-glutamic acid content of concentrated solution higher, then after concentrating, can produce β-type glutamic acid crystallization and be settled out colloid, protein, thalline, directly influence the purity of iso-electric point extraction glutamic acid crystallization.
The objective of the invention is to avoid above-mentioned weak point of the prior art and propose a kind of operating process simple, only need general device, can carry out the method for the high glutamic acid crystallization of the dna purity of suitability for industrialized production, no discharging of waste liquid contaminate environment.
Purpose of the present invention can reach by following steps, from L-glutamic acid cultivate the step of removing colloid, protein, thalline the sophisticated fermented liquid, iso-electric point is extracted L-glutamic acid step and crystalline mother solution enrichment step, it is characterized in that this method is made up of following steps:
A) carboxylic acid (any in formic acid, acetate, the lactic acid) that is dissolved in 0.2～2% concentration with chitosan is prepared into the flocculation agent with cationic characteristic of 0.5～3 gram/100 ml concns;
B) in fermented liquid, add 0.02～1 grams per liter (with respect to the fermented liquid volume) chitosan, at normal temperature, pH7～6.5 o'clock, colloid, protein, thalline cohesion, condensation product was deposited in appearance and carries a device bottom through 1～2 hour, and the acquisition clear liquid first time and the first time be turbid liquid down;
C) with turbid liquid accent pH7～7.5 under the first time, colloid, protein, thalline cohesion, condensation product was deposited in an appearance year device bottom through 1～2 hour, the acquisition clear liquid second time and turbid liquid under the second time;
D) will be heated to 60～90 ℃ by turbid liquid under the second time, drop into activated carbon 2～30 grams per liters, adjust pH5～3, obtain clear liquid for the third time after filtration;
Three clear liquids that e) will obtain merge transfers isoelectric fractionation to go out crystallization L-glutamic acid and isoelectric point crystallizing mother liquor;
F) concentrate isoelectric point crystallizing mother liquor, concentration ratio is 1.5～5: 1, and concentrated solution is heated to 60～90 ℃, drops into 2～30 grams per liter active carbon filtrations, and isoelectric fractionation goes out crystallization L-glutamic acid and secondary isoelectric point crystallizing mother liquor;
G) concentrate the secondary isoelectric point crystallizing mother liquor, concentration ratio is 1.5～4: 1, and concentrated solution is heated to 60～90 ℃, drops into 2～30 grams per liter active carbon filtrations, and isoelectric fractionation goes out crystallization L-glutamic acid and final enriched material.
Flocculant concentration is preferably/100 milliliters of 1～2 grams.Chitosan add-on in fermented liquid is preferably 0.03～0.5 grams per liter.
It is 2.7～3.3 that concentrated isoelectric point crystallizing mother liquor is preferably in concentration ratio: 1,60～80 ℃ of temperature vacuumize evaporation concentration.It is 1.85～2.1 that concentrated secondary isoelectric point crystallizing mother liquor is preferably in concentration ratio: 1,60～80 ℃ of temperature vacuumize evaporation concentration.
Final enriched material is neutralized to pH6.2～6.8 with strong aqua and obtains farming fertilizer.
The invention has the advantages that:
The present invention adopts based on colloid, protein, thalline in the flocculation agent removal fermented liquid with cationic characteristic of chitosan, and its operation steps simply, only needs general device, can carry out industrialized production.Above-mentioned impurity can make in the concentrated mother liquor process and can not produce a large amount of foams after removing from fermented liquid, and protein receptor heat evolution coagulum also significantly reduces.Because isoelectric point crystallizing mother liquor is subacidity, filter the glutamic acid crystallization purity height that is obtained easily when removing the impurity of concentrated solution with activated carbon.
The present invention adopts the secondary concentration isoelectric point crystallizing mother liquor, and each concentration ratio is little, but total concentration ratio is big, like this, has both avoided producing β-type crystallization when high density is collected L-glutamic acid, can improve the L-glutamic acid yield again.
Still contain residual sugar, residual urea, L-glutamic acid, mineral ion in the final enriched material that final step of the present invention obtained, its moisture content has reduced 80-90% than this step before concentrated, add in the strong aqua and after just to become farming with practical value fertile.Meanwhile, also solved the glutamic acid crystallization mother liquor as the discharge of wastewater problem of environment pollution caused.
Method of the present invention is compared from the friendship two step method with iso-electric point is freezing, and its L-glutamic acid yield is high by 10%, and ton starch produces L-glutamic acid increases by 10%, and product cost reduces by 10～20%.
Fig. 1 is a process flow sheet of the present invention.
By the following non-limiting examples that will narrate the present invention is further elaborated.
Embodiment one:
Getting 1100 liters is that the L-glutamic acid of raw material is cultivated sophisticated fermented liquid with starch, and its L-glutamic acid content is 6.28 grams/100 milliliters, pH7.5, OD1.2.
With being prepared into concentration in 4.4 liters of acetic acid that are dissolved in 1% concentration with chitosan is that the flocculation agent of/100 milliliters of 1 grams drops in the above-mentioned fermented liquid, and pH6.5～6.9 are transferred in acid, and through 5 minutes, visible coacervation took place.Through 2 hours, settlement separate 660 liters of clear liquids and the 440 liters of following turbid liquid of obtaining of 1100 liters fermented liquid.
440 liters of stirrings of turbid liquid for the first time down, with adjusting PH with base 7.1～7.5, visible coacervation takes place once more, settlement separate 220 liters of clear liquids and the 220 liters turbid liquid down that obtains through 2 hours.
With obtained 220 liters down turbid liquid be heated to 90 ℃, make proteins coagulation, then, be cooled to 60 ℃, pH4 is transferred in acid, drops into 2.2 kilograms of activated carbon, with pressure filter filter 210 liters of clear liquids.
Merge totally 1090 liters of above-mentioned three clear liquids that step obtained, iso-electric point is extracted L-glutamic acid.The L-glutamic acid content of check isoelectric point crystallizing mother liquor is/100 milliliters of 2.5 grams, and OD0.1, L-glutamic acid yield are 60%, gets 45.7 kilograms of rough rice propylhomoserins.
Getting 1000 liters of isoelectric point crystallizing mother liquors concentrates, under 60 ℃ of temperature, evaporate moisture content with vacuum continuous concentration pot, concentration ratio is 2.7: 1, obtain 370 liters of its concentrated solutions, be heated to 80 ℃ then, drop into 1.1 kilograms of activated carbon, filter, after iso-electric point, isolate L-glutamic acid and secondary isoelectric point crystallizing mother liquor with pressure filter.The L-glutamic acid content of check secondary isoelectric point crystallizing mother liquor is/100 milliliters of 2.5 grams, and this moment, the L-glutamic acid yield was 25.5%, got 17 kilograms of rough rice propylhomoserins.
Getting 300 liters of secondary isoelectric point crystallizing mother liquors concentrates, under 60 ℃ of temperature, evaporate moisture content with vacuum continuous concentration pot, concentration ratio is 1.85: 1, obtain 135 liters of its concentrated solutions, be heated to 80 ℃ then, drop into 0.76 kilogram of activated carbon, filter, after iso-electric point, isolate L-glutamic acid and final enriched material with pressure filter.Checking final enriched material L-glutamic acid content is/100 milliliters of 3.5 grams, and at this moment, the L-glutamic acid yield is 3.5%, gets 2 kilograms of rough rice propylhomoserins.Through above-mentioned steps, its L-glutamic acid total recovery is 89%.
With in the strong aqua and after transferring pH6.2, it is fertile to obtain canned farming with final enriched material.
Embodiment two:
Getting 1100 liters is that the L-glutamic acid of raw material is cultivated sophisticated fermented liquid with starch, and its L-glutamic acid content is/100 milliliters of 6.28 grams, pH7.5, OD1.2.
With being prepared into concentration in 22 liters of lactic acid that are dissolved in 2% concentration with chitosan is that the flocculation agents of/100 milliliters of 2 grams drop in the above-mentioned fermented liquid, and pH6.5～6.9 are transferred in acid, and through 5 minutes, visible coacervation took place.Through 1 hour, settlement separate 770 liters of clear liquids and the 330 liters of following turbid liquid of obtaining of 1100 liters fermented liquid.
330 liters of stirrings of turbid liquid for the first time down, with adjusting PH with base 7.1～7.4, settlement separate 220 liters of clear liquids and the 110 liters turbid liquid down that obtains through 1 hour.
With obtained 110 liters down turbid liquid be heated to 60 ℃, drops into 0.22 kilogram of activated carbon, acid accent pH4, with pressure filter filter 105 liters of clear liquids.
Merge totally 1095 liters of above-mentioned three clear liquids that step obtained.Iso-electric point is extracted L-glutamic acid.The L-glutamic acid content of check isoelectric point crystallizing mother liquor is/100 milliliters of 2.5 grams, and OD0.08, L-glutamic acid yield are 60%, gets 46 kilograms of rough rice propylhomoserins.
Getting 1000 liters of isoelectric point crystallizing mother liquors concentrates, under 60 ℃ of temperature, evaporate moisture content with vacuum continuous concentration pot, getting concentration ratio is 3.3: 1, obtain 300 liters of its concentrated solutions, be heated to 70 ℃ then, drop into 6 kilograms of active carbon filtrations, after iso-electric point, isolate L-glutamic acid and secondary isoelectric point crystallizing mother liquor.The L-glutamic acid content of check secondary isoelectric point crystallizing mother liquor is/100 milliliters of 2.5 grams, and at this moment, the L-glutamic acid yield is 27.8%, gets 19 kilograms of rough rice propylhomoserins.
Get 300 liters of secondary isoelectric point crystallizing mother liquors and concentrate, with vacuum continuous concentration pot evaporation moisture content, getting concentration ratio is 2.1: 1 under 60 ℃ of temperature, obtain 142 liters of its concentrated solutions, be heated to 70 ℃ then, drop into 3.5 kilograms of active carbon filtrations, after iso-electric point, isolate L-glutamic acid and final enriched material.The L-glutamic acid content of checking final enriched material is/100 milliliters of 3.5 grams, and at this moment, the L-glutamic acid yield is 3.9%, gets 2.8 kilograms of rough rice propylhomoserins.Through above-mentioned steps, its L-glutamic acid total recovery is 91.7%.
With in the strong aqua and after transferring pH6.5, it is fertile to obtain canned farming with final enriched material.
Can find out that method of the present invention has significant technological progress, it is fairly obvious comparing with former process.
Claims (6)
1, cultivate the method for sophisticated broth extraction crystallization L-glutamic acid by L-glutamic acid, comprise step, iso-electric point extraction L-glutamic acid step and the crystalline mother solution enrichment step of removing fermented liquid colloid, protein, thalline, it is characterized in that:
A) to be prepared into concentration be/100 milliliters of flocculation agents with cationic characteristic of 0.5～3 gram to the carboxylic acid (any in formic acid, acetate, the lactic acid) that is dissolved in 0.2～2% concentration with chitosan;
B) in fermented liquid, add 0.02～1 grams per liter (with respect to the fermented liquid volume) chitosan, at normal temperature, pH value is 7～6.5 o'clock, colloid, protein, thalline cohesion, condensation product was deposited in appearance and carries a device bottom through 1～2 hour, and the acquisition clear liquid first time and the first time be turbid liquid down;
C) will turbid liquid adjust pH be 7～7.5 under the first time, colloid, protein, thalline cohesion, condensation product was deposited in appearance and carries the device bottom through 1～2 hour, and the acquisition clear liquid second time and the second time be turbid liquid down;
D) will be heated to 60～90 ℃ by turbid liquid under the second time, drop into activated carbon 2～30 grams per liters, adjust PH5～3, obtain clear liquid for the third time after filtration;
Three clear liquids that e) will obtain merge transfers isoelectric fractionation to go out crystallization L-glutamic acid and isoelectric point crystallizing mother liquor;
F) concentrate isoelectric point crystallizing mother liquor, concentration ratio is 1.5～5: 1, and concentrated solution is heated to 60～90 ℃, drops into 2～30 grams per liter active carbon filtrations, and isoelectric fractionation goes out crystallization L-glutamic acid and secondary isoelectric point crystallizing mother liquor;
G) concentrate the secondary isoelectric point crystallizing mother liquor, concentration ratio is 1.5～4: 1, and concentrated solution is heated to 60～90 ℃, drops into 2～30 grams per liter active carbon filtrations, and isoelectric fractionation goes out crystallization L-glutamic acid and final enriched material.
2, method according to claim 1 is characterized in that said flocculant concentration is preferably/100 milliliters of 1～2 grams.
3, method according to claim 1 is characterized in that chitosan add-on in fermented liquid is preferably 0.03～0.5 grams per liter.
4, method according to claim 1, it is characterized in that it is 2.7～3.3 that concentrated isoelectric point crystallizing mother liquor is preferably in concentration ratio: 1,60～80 ℃ of temperature vacuumize evaporation concentration.
5, method according to claim 1, it is characterized in that it is 1.85～2.1 that concentrated secondary isoelectric point crystallizing mother liquor is preferably in concentration ratio: 1,60～80 ℃ of temperature vacuumize evaporation concentration.
6, method according to claim 1 is characterized in that final enriched material is neutralized to pH value 6.2～6.8 with strong aqua and obtains farming fertilizer.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90102179 CN1021704C (en) | 1990-04-13 | 1990-04-13 | Process for extracting amino glutaric acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 90102179 CN1021704C (en) | 1990-04-13 | 1990-04-13 | Process for extracting amino glutaric acid |
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| CN1048702A true CN1048702A (en) | 1991-01-23 |
| CN1021704C CN1021704C (en) | 1993-07-28 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 90102179 Expired - Fee Related CN1021704C (en) | 1990-04-13 | 1990-04-13 | Process for extracting amino glutaric acid |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1046267C (en) * | 1994-01-20 | 1999-11-10 | 华南理工大学 | Pretreatment method for isoelectric point extraction of extraction glutaminic acid from fermentation liquor |
| CN1067376C (en) * | 1996-06-25 | 2001-06-20 | 无锡轻工大学 | Method for extracting glutamic acid from fermentation liquor |
| CN1318599C (en) * | 2001-02-20 | 2007-05-30 | 味之素株式会社 | Composition containing organic nitrogen and its fertilizer containing said composition |
| CN101293849B (en) * | 2007-04-29 | 2013-02-13 | 长春大成实业集团有限公司 | Process for preparing glutamic acid crystallization |
| CN103058716A (en) * | 2013-01-14 | 2013-04-24 | 广西穗宁化工集团有限公司 | Organic matter liquid suitable for being used as leaf fertilizer raw material |
| CN103224454A (en) * | 2013-03-18 | 2013-07-31 | 内蒙古阜丰生物科技有限公司 | Glutamic acid separating and extracting technology |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100343180C (en) * | 2004-12-31 | 2007-10-17 | 西北大学 | Chitin/chitosan water processing flocculating agent and its preparing method |
-
1990
- 1990-04-13 CN CN 90102179 patent/CN1021704C/en not_active Expired - Fee Related
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1046267C (en) * | 1994-01-20 | 1999-11-10 | 华南理工大学 | Pretreatment method for isoelectric point extraction of extraction glutaminic acid from fermentation liquor |
| CN1067376C (en) * | 1996-06-25 | 2001-06-20 | 无锡轻工大学 | Method for extracting glutamic acid from fermentation liquor |
| CN1318599C (en) * | 2001-02-20 | 2007-05-30 | 味之素株式会社 | Composition containing organic nitrogen and its fertilizer containing said composition |
| CN101293849B (en) * | 2007-04-29 | 2013-02-13 | 长春大成实业集团有限公司 | Process for preparing glutamic acid crystallization |
| CN103058716A (en) * | 2013-01-14 | 2013-04-24 | 广西穗宁化工集团有限公司 | Organic matter liquid suitable for being used as leaf fertilizer raw material |
| CN103224454A (en) * | 2013-03-18 | 2013-07-31 | 内蒙古阜丰生物科技有限公司 | Glutamic acid separating and extracting technology |
| CN103224454B (en) * | 2013-03-18 | 2014-07-09 | 内蒙古阜丰生物科技有限公司 | Glutamic acid separating and extracting technology |
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| Publication number | Publication date |
|---|---|
| CN1021704C (en) | 1993-07-28 |
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