CN1067376C - Method for extracting glutamic acid from fermentation liquor - Google Patents
Method for extracting glutamic acid from fermentation liquor Download PDFInfo
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- CN1067376C CN1067376C CN96116404A CN96116404A CN1067376C CN 1067376 C CN1067376 C CN 1067376C CN 96116404 A CN96116404 A CN 96116404A CN 96116404 A CN96116404 A CN 96116404A CN 1067376 C CN1067376 C CN 1067376C
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Abstract
The present invention discloses a method for extracting glutamic acid from fermentation liquor. The chief technology has the technical characteristics that bacteria in crystallized mother liquor are removed; the sterilization mother liquor is hydrolyzed after condensed and desalted; the hydrolyzed filtering liquor is recycled, and the next batch of fermentation liquor is crystallized. The main body of the process is the closed cycle. The present invention can reach the high extraction yield which is more than 95%, can also obtain by products, such as feed, fertilizers, etc. and solves the problem of serious contamination by effluent in gourmet powder industry from technology interior.
Description
The present invention relates to a kind of method of from fermented liquid, extracting L-glutamic acid.
The prior art of extracting L-glutamic acid from fermented liquid related to the present invention mainly contains following several:
" amino acid technology " (Tianjin Light Industry College etc. are write, the publication of light industry press) low temperature (3-5 ℃) the isoelectric point crystallizing method of introducing, CN 88106847.0 disclosed isoelectric point crystallization ion exchange methods, be on the basis of above-mentioned low temperature isoelectric point crystallization method, to carry out again once from friendship, with fermented liquid or the crystalline mother solution wash-out adjusted, to reclaim the most of L-glutamic acid in the crystalline mother solution.The disclosed concentrated isoelectric point crystallization method of Japanese Patent 59-14794.This method concentrates earlier and removes fermented liquid, adds acid again and transfers concentrated solution to pH3.2, and glutamic acid crystallization is separated.Ultrafiltration and resistates hydrolysis method that French Patent FR2574-790-A introduces are extracted L-glutamic acid from fermented liquid, with glutami acid fermentation liquor after ultrafiltration, obtain filtrate and residue, filtrate concentrates, the residue hydrolysed filtrate and with L-glutamic acid concentrated solution mixing post crystallization, these methods or extracting glutamic acid yield are not high, and economic benefit is not high, or contaminated wastewater is serious.
2.CN1099746A disclose a kind of extracting method of L-glutamic acid,, do not had contaminated wastewater again though yield is higher, but when making hydrolyst with hydrochloric acid, Cl-excessive concentration in the loop-body material, too big to common stainless steel corrodibility, then invest too big with special rolling-mill section.When making hydrolyst with sulfuric acid, sulfate radical accumulates in circulation easily, causes later stage technology operation difficult.Particularly, this technology is not considered the recovery of other material except that major product L-glutamic acid in the fermented liquid, influences overall economic efficiency.
The objective of the invention is to overcome the deficiency of above-mentioned prior art, provide a kind of and can improve major product extracting glutamic acid recovery rate by a relatively large margin, can obtain a large amount of high protein thalli feeds and by products such as high-quality chemical fertilizer and higher-grade fertilizer again; Overall economic efficiency can be increased substantially, a large amount of novel procesies of discharging the severe contamination that environment is caused of crystalline mother solution can be solved again.
Extracting method of the present invention is made up of the following step:
A: fermented liquid is isoelectric point crystallization below 30 ℃.
B: crystal separates with mother liquor and obtains glutamic acid crystallization and mother liquor.
C: from mother liquor, remove the glutamic acid fermentation bacterium.
D: remove mother bacterial liquid and concentrate, obtain concentrated solution and water of condensation.
E: the concentrated solution desalination obtains ammonium sulfate and desalination and concentration liquid.
F: but desalination and concentration liquid acid hydrolysis after-filtration obtains hydrolysed filtrate liquid and filter cake.
G: hydrolysed filtrate liquid can decolour, but also nondiscoloration.At least be partly recirculated to A, regulate the pH of next batch fermented liquid, isoelectric point crystallizing, the process main body realizes closed cycle.
Accompanying drawing 1 is a process flow sheet of the present invention.
The invention will be further described below in conjunction with relevant devices:
In crystallizing tank, with glutami acid fermentation liquor, be cooled to earlier below 30 ℃, acid adding (the A collection of) or add the hydrolysed filtrate liquid that the last consignment of circulation comes, make the zymotic fluid crystallization. PH3.0-3.2 Lower stirring educate brilliant after on centrifuge centrifugation go out crystal, and use the running water washing crystal, Mother liquor is heated to 80-120 ℃, temperature retention time 5-25 minute, the glutamate producing bacterium flocculation Rear interpolation cellulosic filter aid removes by filter. The clear mother liquor of degerming concentrates 3-8 doubly in inspissator, Deliver to and add liquefied ammonia or ammoniacal liquor (also can not adding) in the demineralizer, at 20-120 ℃, pH4.0-8.0 Lower desalination is also centrifugal, isolates ammonium sulfate (containing a small amount of sylvite) crystallization. Desalination and concentration liquid Send into the hydrolytic decomposition pot acid hydrolysis, so that the pyroglutamic acid that will produce will concentrate time hydrolysis reverts back to paddy Propylhomoserin is conducive to improve the extract yield of glutamic acid, simultaneously residual sugar is hydrolyzed into humus, Be not allowed to condition in the closed circuit circulatory system and accumulate, plate-frame filtering or suction filtration obtain filter cake and were hydrolyzed Filtrate. Filter cake is a kind of high-grade humic acid organic fertilizer material. Hydrolysed filtrate liquid is acidity also Be rich in glutamic acid, can add active carbon or other bleaching agent bleaching, but also nondiscoloration, this acidity The circulation of (decolouring) liquid is returned and is replaced sulfuric acid to regulate next group zymotic fluid pH, isoelectric point crystallizing.
First advantage of the present invention be the average extract yield of glutamic acid up to 95-97%, this is this The outstanding advantages of the close circulation technology of invention design. Loss is only from thalline, and ammonium sulfate is tied Carrying secretly on a small quantity glutamic acid when brilliant and humic acid filter cake leaves circulating ring. As fine to them The ground washing can be reduced the loss again, and then extract yield also can further improve.
Second advantage of the present invention is that the process main body forms closed cycle (Infinite Cyclic), realizes Non-pollution discharge. Leave a large amount of condensate water of circulating ring, its COD can be controlled in 400ppm About, can be used as process water. Leave the solid matter of circulating ring or for product or for by-product Product. Therefore, solved the long-term unsolved serious waste water pollution problem of monosodium glutamate industry.
The 3rd outstanding advantages of the present invention is a large amount of accessory substance of output-high protein thalli feed (protein＞50%, its amount account for msg output 12%); The crystalline sulfuric acid ammonium (accounts for monosodium glutamate Output 70%); (total content of humic acid 55%, its amount accounts for monosodium glutamate to the high-grade organic fertilizer Output 11%); Significant economic benefit is arranged.
The 4th advantage of the present invention is that this close circulation technology can adopt the normal temperature crystallization and do not reduce Extract yield is compared with freezing and crystallizing, can save the investment of a large amount of electric energy and refrigerating plant, Substantially remedied the thermal energy consumption expense when concentrated.
Embodiment one:
25 ℃ fermented liquid 3000ml adds the vitriol oil and transfers isoelectric point crystallization, removes by filter electric mother liquor 3050ml such as obtaining L-glutamic acid behind the crystal, mother liquor aminoglutaric acid concentration 2.0%.Mother liquor is heated to 110 ℃, keeps after 5 minutes and add flocculating aids 0.5%, B filter and washing leaching cake once, obtain clear filtrate 3010ml, wet cake 50g, normal pressure concentrates about 5 times in the pottery pot, add ammoniacal liquor and transfer pH5.5-7.5, temperature 10-80 ℃ of following desalination.Get ammonium sulfate 150g, desalination and concentration liquid 400ml after centrifugal.Can add vitriol oil 80ml in desalination and concentration liquid, hydrolysis is 5 hours under the 0.2MPa, and the evaporation about 100ml water, filter filter cake 120g, hydrolysed filtrate liquid 250ml.Add gac 2.5g in hydrolysed filtrate liquid, the 1 hour after-filtration that decolours is removed filter residue.Regulate next batch 3000ml with this hydrolysed filtrate liquid, aminoglutaric acid concentration is the pH of 8.0% fermented liquid, and isoelectric point crystallizing obtains crystallization L-glutamic acid 237.4g, and purity is 96.5%, mother liquor 3200ml, and concentration is 1.90%.
But infinite loop successively.
Embodiment two:
In crystallizer, with 1000ml, L-glutamic acid content is 8.2% fermented liquid, is cooled to 20 ℃ earlier, adds the hydrolysed filtrate liquid of last consignment of, makes the fermented liquid crystallization.After pH3.0-3.2 stirred down and educates crystalline substance, centrifugation on whizzer obtained the dried crystal of 81.2Kg, and purity is 96.5%; Mother liquor is heated to 100 ℃, 10 minutes, add 3Kg cellulosic flocculating aids after the thalline flocculation, Plate Filtration obtains thalline throw out 24kg (moisture 52%), the clear mother liquor of degerming concentrates 4 times in thickener after, deliver in the demineralizer, in 70 ℃ of following desalinations and centrifugal, isolate ammonium sulfate crystallization 73.2kg (moisture 10%), concentrated solution 121L after the desalination can send into hydrolytic decomposition pot and add the hydrolysis 4 hours under 0.2Mpa of the 24.2L vitriol oil, and at hydrolysis later stage evaporation 25L water, Plate Filtration obtains filter cake 22.3kg (moisture 48%) and hydrolysed filtrate liquid 103L.Hydrolysed filtrate liquid returns regulates next batch fermented liquid pH, isoelectric point crystallizing.But infinite loop successively.
Claims (4)
1. method of from fermented liquid, extracting L-glutamic acid, this method is made up of following steps:
A: fermented liquid is isoelectric point crystallization below 30 ℃,
B: crystal separates with mother liquor and obtains glutamic acid crystallization and mother liquor,
C: from mother liquor, remove the glutamic acid fermentation bacterium,
D: remove mother bacterial liquid and concentrate, obtain concentrated solution and water of condensation,
E: the concentrated solution desalination, obtain ammonium sulfate and desalination and concentration liquid,
F: desalination and concentration liquid acid hydrolysis after-filtration, obtain hydrolysed filtrate liquid and filter cake,
G: hydrolysed filtrate liquid can decolour, but also nondiscoloration is partly recirculated to A at least, regulates the pH of next batch fermented liquid, isoelectric point crystallizing, and the process main body realizes closed cycle.
2. by the described a kind of method of extracting L-glutamic acid from fermented liquid of claim 1, it is characterized in that removing thalline with heat flocculation-filtration method, that is: temperature 80-120 ℃, soaking time 5-25 minute flocculation thalline adds cellulosic flocculating aids sheet frame after-filtration and removes thalline.
3. by the described a kind of method of extracting L-glutamic acid from fermented liquid of claim 1, it is characterized in that: crystallization removes ammonium sulfate under 20-120 ℃, pH4.0-8.0.
4. by the described a kind of method of from fermented liquid, extracting L-glutamic acid of claim 1, it is characterized in that adding sulfuric acid and be hydrolyzed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96116404A CN1067376C (en) | 1996-06-25 | 1996-06-25 | Method for extracting glutamic acid from fermentation liquor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN96116404A CN1067376C (en) | 1996-06-25 | 1996-06-25 | Method for extracting glutamic acid from fermentation liquor |
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| CN1161324A CN1161324A (en) | 1997-10-08 |
| CN1067376C true CN1067376C (en) | 2001-06-20 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN96116404A Expired - Fee Related CN1067376C (en) | 1996-06-25 | 1996-06-25 | Method for extracting glutamic acid from fermentation liquor |
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Families Citing this family (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1072907C (en) * | 1997-12-03 | 2001-10-17 | 福建省沙县科丹生物工程研究所 | Producing technology for tasty additive of soy sauce or other seasonings |
| CN101120766B (en) * | 2007-07-30 | 2011-08-10 | 山东阜丰生物科技开发有限公司 | Monosodium glutamate green manufacturing technology |
| CN101103801B (en) * | 2007-07-30 | 2011-05-25 | 山东阜丰生物科技开发有限公司 | Intermittent type glutamic acid crystalloblastic technology |
| CN101255120B (en) * | 2008-04-02 | 2010-12-15 | 江南大学 | Novel technique for extracting glutaminic acid |
| CN102120722B (en) * | 2010-12-29 | 2013-11-27 | 菱花集团有限公司 | Method for recycling glutamic acid from desalting liquid |
| CN102583835A (en) * | 2012-03-13 | 2012-07-18 | 同济大学 | Closed-cycle circulating process for governing biogas slurry fermented through wastewater from pig farms |
| CN104262014B (en) * | 2014-10-07 | 2016-05-18 | 内蒙古阜丰生物科技有限公司 | A kind of bio-bacterial manure that utilizes glutamic acid fermentation discarded object to prepare |
| CN104256056B (en) * | 2014-10-14 | 2016-09-07 | 内蒙古阜丰生物科技有限公司 | Utilize animal feed prepared by glutamic acid fermentation waste material |
| CN104311337B (en) * | 2014-10-19 | 2016-05-25 | 内蒙古阜丰生物科技有限公司 | A kind of method of utilizing glutamic acid wastewater to produce liquid fertilizer |
| CN107043343B (en) * | 2017-06-20 | 2021-04-27 | 峨眉山市龙腾生物科技有限公司 | Preparation method of L-pyroglutamic acid |
| CN107500830B (en) * | 2017-09-27 | 2021-05-25 | 江苏省农业科学院 | Glutamic acid type special fertilizer for sweet potatoes and preparation method thereof |
| CN111534552B (en) * | 2017-12-15 | 2023-03-31 | 内蒙古伊品生物科技有限公司 | Fermentation production and post-treatment of glutamic acid |
| CN112694413A (en) * | 2021-03-24 | 2021-04-23 | 鲁东大学 | Method for extracting L-homoserine from fermentation liquor |
| CN113072457A (en) * | 2021-04-07 | 2021-07-06 | 华东理工大学 | Method for freezing, concentrating and isoelectric point crystallizing glutamic acid |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1048702A (en) * | 1990-04-13 | 1991-01-23 | 陈雪贞 | A kind of method of extracting L-glutamic acid |
| CN1099746A (en) * | 1993-08-30 | 1995-03-08 | 无锡轻工业学院 | Method for extracting glutaminic acid from fermentation liquor |
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1996
- 1996-06-25 CN CN96116404A patent/CN1067376C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1048702A (en) * | 1990-04-13 | 1991-01-23 | 陈雪贞 | A kind of method of extracting L-glutamic acid |
| CN1099746A (en) * | 1993-08-30 | 1995-03-08 | 无锡轻工业学院 | Method for extracting glutaminic acid from fermentation liquor |
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