CN101255120B - Novel technique for extracting glutaminic acid - Google Patents
Novel technique for extracting glutaminic acid Download PDFInfo
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- CN101255120B CN101255120B CN2008100235162A CN200810023516A CN101255120B CN 101255120 B CN101255120 B CN 101255120B CN 2008100235162 A CN2008100235162 A CN 2008100235162A CN 200810023516 A CN200810023516 A CN 200810023516A CN 101255120 B CN101255120 B CN 101255120B
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- glutamic acid
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- mother liquor
- isoelectric point
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Abstract
The invention relates to a novel process for abstracting glutamate which need less raw material and water, comprising: adding fermentation broth of glutamate into an isoelectric point crystallization can for isoelectric point crystallization; centrifugally separating after isoelectric point crystallization to obtaining glutamate crystallization and an isoelectric mother liquid; passing the isoelectric mother liquid through thallus for separating to obtain thallus albumen and an isoelectric clear mother liquid; vaporizing a part of the isoelectric clear mother liquid to obtain a concentrated clear mother liquid, and the other part is kept for solubilizing the secondary crystal of glutamate; secondarily crystallizing the concentrated clear mother liquid to obtain secondarily crystallized glutamate crystal, solubilizing the secondarily crystallized glutamate crystal by water, an isoelectric clear mother liquid, and sulfuric acid; returning dilute sulfuric acid with glutamate obtained by solubilization back to the after isoelectric point crystallization can, adjusting a next set of fermentation broth for after isoelectric point crystallization. The process can reduce the consumption of sulfuric acid and liquid ammonia, raising the abstraction yield of enhance by using secondary crystal process; and has a good quality for crystallization without compound crystal.
Description
Technical field
The present invention relates to the extracting glutamic acid novel process of the few waste water of a kind of low material consumption, specifically the fermented food industry technical field.
Background technology
The production technique of monosodium glutamate is a raw material with starch or waste molasses mainly, obtains intermediate product L-glutamic acid through sugaring, fermentation and extraction, and L-glutamic acid passes through operations such as neutralization, decolouring, deironing, Crystallization Separation and drying again, makes the finished product monosodium glutamate.
Wherein, the prior art of extraction L-glutamic acid mainly contains from glutami acid fermentation liquor: " isoelectric point crystallization+ion-exchange " technology and " concentrating isoelectric point crystallization+metacrystal " technology.
Domestic most glutamate production enterprise adopts " isoelectric point crystallization+ion-exchange " technology.Its technological process is the height stream part pH value of regulating fermented liquid that obtains with ion-exchange, makes it drop to iso-electric point 3.22, and is cooled to about 10 ℃, and most of glutamic acid crystallization is separated out; Remain in the L-glutamic acid spent ion exchange resin absorption in the crystalline mother solution, with ammoniacal liquor the L-glutamic acid wash-out of resin absorption is obtained high stream part again, high stream part is used for next batch fermented liquid isoelectric point crystallization.The advantage of this technology is the extract yield height, and general total recovery can reach 94%, but this technology has additionally produced 40% hc effluent, again additive decrementation 100% sulfuric acid and 45% liquefied ammonia.
" concentrating and wait electricity+metacrystal " technology is that glutami acid fermentation liquor is concentrated 3～4 times, make that aminoglutaric acid concentration reaches about 30% in the concentrated broth, enter the continuous electricity jar that waits then, stream adds acidic hydrolysis liquid simultaneously, the pH value of electricity such as control jar is 3.0～3.2, be cooled to simultaneously about 30 ℃, glutamic acid crystallization is separated out, separate obtaining glutamic acid crystal again with horizontal spiral centrifuge.Because it is of poor quality to separate the glutamic acid crystallization that obtains, and must cook monosodium glutamate by making with extra care after " metacrystal ".The advantage of this technology is that sulfuric acid, liquefied ammonia consumption are few, and the waste water of generation is also few.Its shortcoming is that the extracting glutamic acid yield is low, only 88%, there is not obvious competitive power economically, and only there are the indivedual production lines in a little enterprise on probation at home in the monosodium glutamate industry.
Thereby therefore reducing the novel extracting glutamic acid technology that material consumptions such as sulfuric acid, liquefied ammonia reduce production costs and reduce the waste water generation, is the key problem in technology that monosodium glutamate industry develops in a healthy way.
Summary of the invention
The objective of the invention is to overcome above-mentioned weak point, thereby the extracting glutamic acid novel process of the few waste water of a kind of low material consumption is provided, can reduce the consumption of sulfuric acid and liquefied ammonia; Adopt secondary crystallization process, can improve the extracting glutamic acid yield; Glutamic acid crystallization is best in quality, need not " metacrystal ".
Main solution of the present invention is achieved in that
The extracting glutamic acid novel process of the few waste water of a kind of low material consumption of the present invention, adopt following processing step:
1, glutami acid fermentation liquor enters isoelectric point crystallization jar isoelectric point crystallization, adds the dilution heat of sulfuric acid that contains 2～30% L-glutamic acid, and sulfuric acid concentration is 1～50%; Regulate the pH value 3.0～3.2 of fermented liquid, 5～25 ℃ of controlled temperature are separated out glutamic acid crystallization; The ratio of glutami acid fermentation liquor and dilution heat of sulfuric acid is controlled by pH.
2, isoelectric point crystallization after centrifugation obtain the product glutamic acid crystallization and etc. electric mother liquor;
3, will wait electric mother liquor by the thalline separating step obtain the by product tropina and etc. the clear mother liquor of electricity;
4, with the clear mother liquor separated into two parts of electricity such as above-mentioned, 80～100% of the clear mother liquor total amounts of electricity such as a part accounts for enter evaporator evaporation and obtain concentrating clear mother liquor, vacuum tightness-0.09～-0.01MPa, thickening temperature is 45～98 ℃, concentrates the back volume and is 1/2～1/8 of clear mother liquor volume before concentrating; 0～20% of the clear mother liquor total amounts of electricity such as another part accounts for do not concentrate, and use as dissolving secondary crystal L-glutamic acid in the step 7;
5, concentrate clear mother liquor by controlled temperature and pH and secondary crystal, make to remain in the L-glutamic acid continuation crystallization that waits in the electric mother liquor and separate out; The pH value 3.0～3.6 of secondary crystal, 5～85 ℃ of controlled temperature;
6, separation obtains L-glutamic acid secondary crystal and secondary crystal mother liquor behind the secondary crystal;
7, the glutamic acid crystal of secondary crystal enters dissolving vessel, in dissolving vessel, add retain in the step 4 of the water of 1～50 times of glutamic acid crystallization weight and/or 1～50 times wait the clear mother liquor of electricity, add 1～15 times sulfuric acid again, glutamic acid crystallization is dissolved;
8, the dilution heat of sulfuric acid that contains L-glutamic acid that obtains through dissolving is sent the isoelectric point crystallization jar back to, regulates next batch fermented liquid isoelectric point crystallization.
Isoelectric point crystallization technology of the present invention can adopt intermittently batch crystallization, or adopts various crystallization techniques such as continuous crystallisation.
Thalline of the present invention separates to adopt and adds flocculation agent flocculation after-filtration, or direct heating makes thalline solidify after-filtration, or adopts separation method such as membrane filtration.Used flocculation agent can be polyacrylamide, sodium polyacrylate, polyaluminium salts or polymeric ferric salt etc., and flocculant addition is 10～300ppm, and Heating temperature is 50～145 ℃.
Evaporation mode of the present invention can adopt single-effect evaporation, or adopts multiple-effect evaporation.
Regulate the dilution heat of sulfuric acid that pH value is adopted among the present invention during isoelectric point crystallization, be by sulfuric acid, water and/or etc. the glutamic acid crystal mixing of the clear mother liquor of electricity, the acquisition of secondary isoelectric point crystallization be made into.Aminoglutaric acid concentration 2～30%, sulfuric acid concentration: 1～50%.
The glutamic acid crystal of described secondary crystal enters the dissolving vessel dissolving, during the pH value of transferring fermented liquid that dilution heat of sulfuric acid is not enough, can directly add sulfuric acid in fermented liquid, drops to 3.0～3.2 until the pH of fermented liquid value.
Two inferior electric mother liquors among the present invention can freely be processed into various products such as ammonium sulfate, composite fertilizer.
Compared with the prior art the present invention has the following advantages:
1, got rid of ion exchange process, so the consumption of sulfuric acid and liquefied ammonia is minimum, its consumption is lower than existing " isoelectric point crystallization+ion-exchange " technology and " concentrating isoelectric point crystallization+metacrystal " technology.。
2, adopt secondary crystallization process, can improve the extracting glutamic acid yield.Extracting glutamic acid yield and " isoelectric point crystallization+ion-exchange " technology remain basically stable, and are higher than " concentrating isoelectric point crystallization+metacrystal " technology.
3, the glutamic acid crystal that obtains of secondary crystal with sulfuric acid, water, etc. the clear mother liquor of electricity mix, or mix with sulfuric acid and water, or mix with electric mother liquor such as clear with sulfuric acid, dissolving is made and is returned isoelectric point crystallization workshop section after " dilution heat of sulfuric acid that contains L-glutamic acid " and be used for the fermented liquid isoelectric point crystallization, its effect is better than the direct accent of sulfuric acid etc., more be better than the electricity such as height stream part accent that ion-exchange obtains, therefore the glutamic acid crystallization that obtains is best in quality, need not " metacrystal ".
4, the wastewater volume of Chan Shenging reduces 30-80% than " isoelectric point crystallization+ion-exchange " technology, in conjunction with existing ammonium sulfate crystallization technology, composite fertilizer's production technology, by product such as reclaim(ed) sulfuric acid ammonium, composite fertilizer and decontamination smoothly, and because the waste water total amount is few, the steam and the electric energy that consume are also low, and production cost is low.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
Embodiment during following the present invention incites somebody to action in conjunction with the accompanying drawings is further described:
Embodiment one: the extracting glutamic acid novel process of the few waste water of a kind of low material consumption of the present invention adopts following processing step:
1, gets 100m
3Glutami acid fermentation liquor, aminoglutaric acid concentration are 10%, 36 ℃ of temperature, pH6.7.Glutami acid fermentation liquor enters the isoelectric point crystallization jar, adds 16m
3The sulfuric acid concentration that contains 6% L-glutamic acid is 25% dilution heat of sulfuric acid, slowly regulates the pH value to 3.1 of fermented liquid, cools 5 ℃, and glutamic acid crystallization is separated out.
2, separate with whizzer, the whizzer velocity of separation is 1200rpm, obtains 10.1 tons of product glutamic acid crystallizations and 110m
3Deng electric mother liquor;
3, separation obtain etc. add 5Kg sodium polyacrylate flocculation agent in the electric mother liquor, make thalline flocculation after-filtration, obtain 2.1 tons of tropinas and 108m
3In the clear mother liquor of electricity.
4, obtain in the step 3 etc. the clear mother liquor of electricity, 95m
3Enter quadruple effect evaporator and concentrate, residue 13m
3Be left to dissolving usefulness in the step 7.Quadruple effect evaporator is imitated quadruple effect vaporization temperature 45～78 ℃ from first, vacuum tightness-0.09～-0.04MPa, concentrating the back volume is 25m
3
5, after concentrating etc. the clear mother liquor of electricity cool to 20 ℃, make remain in etc. electricity clearly the L-glutamic acid secondary crystal in the mother liquor separate out, the pH value of secondary crystal is 3.2.
6, obtain glutamic acid crystallization and secondary crystal mother liquor with the whizzer separation behind the secondary crystal; The whizzer velocity of separation is 6000rpm.
7, separate 1.22 tons of glutamic acid crystallizations that obtain behind the above-mentioned secondary crystal, drop into dissolving vessel, in dissolving vessel, add 13m
3The clear electric mother liquor that waits adds 3700Kg concentration and is 93% industrial sulphuric acid again, makes the glutamic acid crystallization dissolving;
8, the dilution heat of sulfuric acid that contains L-glutamic acid that obtains in the step 7 is returned the isoelectric point crystallization jar, regulate next batch fermented liquid isoelectric point crystallization.
Embodiment two: the extracting glutamic acid novel process of the few waste water of a kind of low material consumption of the present invention adopts following processing step:
1, gets 10m
3Glutami acid fermentation liquor, aminoglutaric acid concentration are 9%, 35 ℃ of temperature, pH6.5.Glutami acid fermentation liquor enters the isoelectric point crystallization jar, adds 1.5m
3The sulfuric acid concentration that contains 7% L-glutamic acid is 20% dilution heat of sulfuric acid, and other adds 60Kg concentration is 93% industrial sulphuric acid, regulates the pH value 3.2 of fermented liquid, and 15 ℃ of controlled temperature are separated out glutamic acid crystallization;
2, separate with whizzer, the whizzer velocity of separation is 1200rpm, obtains 0.9 ton of product glutamic acid crystallization and 11m
3Deng electric mother liquor;
3, with separate in the step 2 obtain etc. electric mother liquor water steam heating to 120 ℃, filter then and obtain 0.22 ton of by product tropina and 10.7m
3In the clear mother liquor of electricity;
4, with in the step 3 etc. the clear mother liquor of electricity enter 2nd effect evaporator and concentrate, vaporization temperature is 65～75 ℃, vacuum tightness-0.04～-0.02MPa, concentrating the back volume is 2.2m
3
5, after concentrating etc. electricity clearly mother liquor cool to 25 ℃, the glutamic acid crystallization that remains in etc. in the electric mother liquor is separated out; The pH value of secondary crystal is 3.2.
6, behind the secondary crystal, obtain glutamic acid crystallization and secondary crystal mother liquor, whizzer velocity of separation 6000rpm with the whizzer separation.
7, the glutamic acid crystallization that obtains in the step 6 is entered dissolving vessel, the concentration of the water of adding 1000Kg and 300Kg is 93% industrial sulphuric acid in dissolving vessel, makes the glutamic acid crystallization dissolving.
8, the sulphuric acid soln that contains L-glutamic acid that obtains in the step 7 is returned the isoelectric point crystallization jar, regulate next batch fermented liquid isoelectric point crystallization.
Embodiment three: the extracting glutamic acid novel process of the few waste water of a kind of low material consumption of the present invention adopts following processing step:
1,100m
3Glutami acid fermentation liquor, aminoglutaric acid concentration are 10.5%, 35 ℃ of temperature, pH6.7.Glutami acid fermentation liquor enters continuous isoelectric point crystallization system.Continuously the isoelectric point crystallization system waits the electricity jar to be in series by four, adds 9m simultaneously in four isoelectric point crystallization jars
3, the sulfuric acid concentration that contains 10% L-glutamic acid is 47% dilution heat of sulfuric acid, the pH value of regulating fermented liquid in the electricity such as four jar is followed successively by 4.2,3.8,3.5,3.2, controls 10 ℃ of outlet temperatures, and glutamic acid crystallization is separated out;
2, obtain 10.6 tons of product glutamic acid crystallizations and 101m with the whizzer separation
3Deng electric mother liquor.The whizzer velocity of separation is 1440rpm.
3, with in the step 2 etc. the electric mother liquor membrane sepn, refilter after the thalline concentrated solution that obtains is heated to 80 ℃, obtain 2.2 tons of by product tropinas.Filtrate merging obtains 97m
3In the clear mother liquor of electricity;
4, with the 95m in the step 3
3Enter quadruple effect evaporator and concentrate in the clear mother liquor of electricity, vaporization temperature is 55～75 ℃, and cycles of concentration (the clear electric mother liquor volume ratio that waits before and after concentrating) is 6 times; Vacuum tightness-0.04～-0.015MPa: all the other 2m
3Give over to dissolving usefulness in the step 7 in the clear mother liquor of electricity.
5, after concentrating etc. the clear mother liquor of electricity cool to 20 ℃, make remain in wait electricity clearly the L-glutamic acid continuation crystallization in the mother liquor separate out; The pH value of secondary crystal is 3.2.
6, centrifugation obtains glutamic acid crystallization and secondary crystal mother liquor behind the secondary crystal;
7, the glutamic acid crystallization that obtains in the step 6 is entered dissolving vessel, in dissolving vessel, add 5m
3Water and 2m
3The wait clear mother liquor of electricity and 3 times of concentration to L-glutamic acid secondary crystal crystal weight be that 93% industrial sulphuric acid makes the glutamic acid crystallization dissolving;
8, the sulphuric acid soln that contains L-glutamic acid that obtains in the step 7 is returned the isoelectric point crystallization jar, regulate next batch fermented liquid isoelectric point crystallization.
Claims (7)
1. extraction technology of glutamic acid is characterized in that adopting following processing step:
(1), glutami acid fermentation liquor enters isoelectric point crystallization jar isoelectric point crystallization, adds the dilution heat of sulfuric acid that contains 2～30% L-glutamic acid, sulphuric acid soln concentration is 1～50%; Regulate the pH value 3.0～3.2 of fermented liquid, 5～25 ℃ of controlled temperature are separated out glutamic acid crystallization;
(2), isoelectric point crystallization after centrifugation obtain the product glutamic acid crystallization and etc. electric mother liquor;
(3), will wait electric mother liquor by thalline separate obtain the by product tropina and etc. the clear mother liquor of electricity;
(4), with the clear mother liquor separated into two parts of electricity such as above-mentioned, a part accounts for and waits electricity 80～100% the entering evaporator evaporation and obtain concentrated clear mother liquor of mother liquor total amount clearly, vacuum tightness-0.09～-0.01MPa, thickening temperature is 45～98 ℃; 0～20% of the clear mother liquor total amounts of electricity such as another part accounts for do not concentrate, and retain to be secondary crystal L-glutamic acid dissolving usefulness;
(5), concentrate clear mother liquor by secondary crystal, make to remain in the L-glutamic acid continuation crystallization that waits in the electric mother liquor and separate out; The pH value 3.0～3.6 of secondary crystal, 5～85 ℃ of controlled temperature;
(6), separate glutamic acid crystal and the secondary crystal mother liquor that obtains secondary crystal behind the secondary crystal;
(7), the glutamic acid crystal of secondary crystal enters dissolving vessel, in dissolving vessel, add the water of 1～50 times of glutamic acid crystallization weight and/or 1～50 times above-mentioned retention wait the clear mother liquor of electricity, add 1～15 times dilution heat of sulfuric acid again, glutamic acid crystallization is dissolved; Sulfuric acid concentration is 1～50% in the solution;
(8), the dilution heat of sulfuric acid that contains L-glutamic acid that obtains through dissolving is sent the isoelectric point crystallization jar back to, adjusting next batch fermented liquid isoelectric point crystallization.
2. a kind of extraction technology of glutamic acid according to claim 1 is characterized in that described isoelectric point crystallization adopts intermittently batch crystallization or employing continuous crystallisation.
3. a kind of extraction technology of glutamic acid according to claim 1 is characterized in that described thalline separates to adopt and adds flocculation agent flocculation after-filtration, or direct heating makes thalline solidify after-filtration, or adopts membrane filtration to separate.
4. a kind of extraction technology of glutamic acid according to claim 3 is characterized in that described flocculation agent is polyacrylamide, sodium polyacrylate, polyaluminium salts or polymeric ferric salt, and flocculant addition is 10～300ppm, and temperature is 50～145 ℃.
5. a kind of extraction technology of glutamic acid according to claim 3 is characterized in that described heating is solidified thalline, and Heating temperature is 50～145 ℃.
6. a kind of extraction technology of glutamic acid according to claim 1 is characterized in that described evaporation employing single-effect evaporation or adopts multiple-effect evaporation.
7. a kind of extraction technology of glutamic acid according to claim 1, it is characterized in that entering the dissolving vessel dissolving when the glutamic acid crystal of described secondary crystal, during the pH value of transferring fermented liquid that dilution heat of sulfuric acid is not enough, can in fermented liquid, directly add sulfuric acid, drop to 3.0～3.2 until the pH of fermented liquid value.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113072457A (en) * | 2021-04-07 | 2021-07-06 | 华东理工大学 | Method for freezing, concentrating and isoelectric point crystallizing glutamic acid |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101993280A (en) * | 2009-08-10 | 2011-03-30 | 江南大学 | Method for producing compound fertilizer by using fermentation glutamate extraction waste liquor |
| CN106748871B (en) * | 2016-11-29 | 2019-03-05 | 岳阳科罗德联合化学工业有限公司 | A kind of green circulatory industrial production process of amino acid surfactant |
| CN114433294B (en) * | 2022-02-18 | 2023-08-22 | 郇玉芝 | Preparation process of biological amino acid |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1161324A (en) * | 1996-06-25 | 1997-10-08 | 无锡轻工大学 | Method for extracting glutamic acid from fermentation liquor |
| CN1597661A (en) * | 2004-07-22 | 2005-03-23 | 徐昌洪 | Glutamic acid extraction technology in production of glutamic acid by fermentation method |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1161324A (en) * | 1996-06-25 | 1997-10-08 | 无锡轻工大学 | Method for extracting glutamic acid from fermentation liquor |
| CN1597661A (en) * | 2004-07-22 | 2005-03-23 | 徐昌洪 | Glutamic acid extraction technology in production of glutamic acid by fermentation method |
Non-Patent Citations (3)
| Title |
|---|
| 周涛，等.谷氨酸母液的二次等电结晶.中国调味品.2003,(12),24-26，31. |
| 周涛.谷氨酸提取无污染工艺研究.江南大学硕士学位论文.2005,9-26. * |
| 周涛等.谷氨酸母液的二次等电结晶.中国调味品.2003,(12),24-26,31. * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113072457A (en) * | 2021-04-07 | 2021-07-06 | 华东理工大学 | Method for freezing, concentrating and isoelectric point crystallizing glutamic acid |
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