CN101157625B - Glutamic acid closed cycle abstraction process combined with crystal transformation - Google Patents
Glutamic acid closed cycle abstraction process combined with crystal transformation Download PDFInfo
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- CN101157625B CN101157625B CN2007101903867A CN200710190386A CN101157625B CN 101157625 B CN101157625 B CN 101157625B CN 2007101903867 A CN2007101903867 A CN 2007101903867A CN 200710190386 A CN200710190386 A CN 200710190386A CN 101157625 B CN101157625 B CN 101157625B
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Abstract
The invention relates to a combined rotating crystal glutmic acid loop circulation extraction technique. Glutmic acid zymotic fluid is mainly mixed with monosodium glutamate mother solution, and the out-separation of the glutmic acid can be fulfilled through the adjustment of the isoelectric point. After two-stage separation, the Alpha crystal type glutmic acid crystal and the isoelectric mother solution can be respectively obtained, and the isoelectric mother solution enters an evaporator for compression and compression by desalting after the thallis recollection, the bacteria elemination and separation so as to separate the ammonium sulfate crystal out and then to obtain the ammonium sulfate crystal and the compressed mother solution. The Alpha crystal type glutmic acid crystal is added with the monosodium glutamate mother solution or water, and then is dissolved through heating. After the cooling, the Alpha crystal type glutmic acid crystal is changed into the Beta crystal type glutmic acid. The rotating crystal mother solution after the compression is mixed with the desalted compression mother solution, and then vitriol is added in for hydrolyzation. The hydrolyzed solution returns to the isoelectric crystal after the circulation. The invention has high the glutmic acid extraction, the quality of the obtained glutmic acid is good, meanwhile, the thalli albumen, ammonium sulfate, corrosion substances and other additional substances are obtained, thereby the pollution of the high-density sewage is prevented.
Description
Technical field
The present invention relates to a kind of L-glutamic acid closed cycle extraction process of combining rotation crystal, specifically belong to the fermented food industry field.
Background technology
L-glutamic acid is a kind of important amino acid, is mainly used to produce tasty agentss such as monosodium glutamate, chickens' extract.China is glutamate production and consumption big country, and China's glutamate production total amount reached more than 170 ten thousand tons in 2006.
The production technique of L-glutamic acid mainly is a fermentation method, is raw material with starch or molasses, obtains by fermentation, extraction.
The current technology of extracting L-glutamic acid from fermented liquid mainly contains: isoelectric point crystallization adds ion exchange process, concentrate isoelectric point crystallization add change brilliant technology and closed cycle extraction process (number of patent application: 96116404.2, title: a kind of method of from fermented liquid, extracting L-glutamic acid) etc.
It is the most widely used extraction process of domestic glutamate production enterprise that isoelectric point crystallization adds ion exchange process, and its advantage is the extract yield height of L-glutamic acid, reaches more than 95%, but shortcoming is also very big, because ion-exchange, the consumption of sulfuric acid, liquefied ammonia is bigger, and wastewater discharge increases more than 50%.Along with raw and auxiliary materials such as sulfuric acid, liquefied ammonia appreciate, and country is to the improving constantly of environmental requirement, and isoelectric point crystallization adds ion exchange process and not only lost economic advantages, also runs counter to Sustainable development.Therefore, getting rid of ion exchange process, will be the inexorable trend of extraction technology of glutamic acid development.
It is that the L-glutamic acid quality that extract to obtain is good that concentrated isoelectric point crystallization adds the great advantage of changeing brilliant technology.Shortcoming is that extract yield is low, generally only 88～90%, and secondly, wait electric mother liquor to adopt the thin pulp spraying drying, atmosphere polluting problem is very serious.
Closed cycle extraction process (number of patent application: 96116404.2 1 kinds of methods of from fermented liquid, extracting L-glutamic acid) successfully got rid of ion exchange process, thoroughly solved problem of environmental pollution, but the glutamic acid crystallization color and luster that obtains is laid particular stress on.
Above-mentioned technology exists seriously pollutedly to some extent, or yield is low or problem such as poor product quality, for addressing the above problem, does not influence under the prerequisite of extracting glutamic acid yield guaranteeing, improves the crystalline product quality, and eliminates environmental pollution.
Summary of the invention
The objective of the invention is to overcome above-mentioned weak point, thereby a kind of L-glutamic acid closed cycle extraction process of combining rotation crystal is provided, but by products such as high efficiente callback tropina, ammonium sulfate, composite fertilizer are thoroughly eliminated the pollution of high-concentration waste water again.
Main solution of the present invention is achieved in that
The L-glutamic acid closed cycle extraction process of combining rotation crystal of the present invention adopts following processing step:
1, glutami acid fermentation liquor is put into the isoelectric point crystallization device, with below the water quench to 30 ℃, add the part sodium glutamate mother liquid simultaneously, the volume of sodium glutamate mother liquid is 0～60% of a fermentating liquid volume, transfer fermented liquid pH value with the hydrolyzed solution or the industrial vitriol oil: 3.0～3.2, temperature is reduced to 5～15 ℃, and L-glutamic acid is separated out with the alpha-crystal form crystallization;
2, after the crystallization etc. electric liquid through flash liberation, obtain the alpha-crystal form glutamic acid crystal of total amount 0～85%; Pass through secondary separation etc. electric liquid, remaining glutamic acid crystal is separated fully with the electric mother liquor such as grade;
3, secondary separation obtain etc. electric mother liquor separate by degerming and obtain tropina and clear mother liquor,
4, clear mother liquor heating evaporation is concentrated, control evaporator pressure :-0.01～0.1MPa, and temperature is: 45～121 ℃, clear mother liquid evaporation cycles of concentration (liquid volume ratio before and after the evaporation) is: 2～5 times;
5, the mother liquor after the evaporation is again by the evaporation concentration desalination, makes in the mother liquor ammonium sulfate crystallization separate out evaporator pressure :-0.01～0.1MPa, and temperature is: 45～121 ℃, mother liquid evaporation cycles of concentration (before and after the evaporation liquid volume than) is: 1～6 times; Separate and obtain ammonium sulfate and desalination and concentration mother liquor;
6, the water or the sodium glutamate mother liquid that in the alpha-crystal form glutamic acid crystal, add 2～5 times of mass ratioes, adjust the pH value with alkali lye: 4.0～6.0, while Heating temperature: 70～90 ℃, L-glutamic acid is partly or entirely dissolved, cool fast then 5～30 ℃, L-glutamic acid is separated out with the beta crystal crystallization; Be referred to as to change brilliant;
7, change the separation of brilliant back and obtain the beta crystal glutamic acid crystallization, promptly major product is discharged simultaneously and is changeed brilliant mother liquor;
8, change brilliant mother liquor heating evaporation and concentrate, control evaporator pressure :-0.01～0.1MPa, temperature is: 55～121 ℃, change brilliant mother liquor cycles of concentration (before and after the evaporation liquid volume than) and be: 2～8 times;
9, concentrated solution and the desalination and concentration mother liquor that changes brilliant mother liquor pressed the arbitrary proportion mixing, adds industrial vitriol oil hydrolysis, and the mass ratio that adds sulfuric acid quality and mixed concentrated liquid is 0.2～1: 1, and hydrolysis temperature is: 80～150 ℃, hydrolysis time is: 1～5 hour;
10, hydrolysis finishes postcooling to 30～80 ℃, separates obtaining solid filter residue and hydrolyzed solution, and hydrolyzed solution is circulated back to isoelectric point crystallization.
Separation method of the present invention can adopt centrifugal or filter.Centrifuge speed: 1400～6000rpm.
Alpha-crystal form glutamic acid crystal of the present invention is irregular prism or pyramidal morphology.
Evaporation operation of the present invention can adopt single-action or multiple-effect evaporation.
Evaporative desalination of the present invention can adopt single-action or multiple-effect evaporation.
Beta crystal glutamic acid crystallization body of the present invention is irregular needle-like or lamellar morphology.
Sodium glutamate mother liquid of the present invention can add before isoelectric point crystallization, also can add when changeing brilliant, or isoelectric point crystallization and commentaries on classics adds when brilliant simultaneously.
Isoelectric point crystallization of the present invention can adopt electricity or continuous isoelectric point crystallizations such as intermittence.
Degerming of the present invention separates can adopt air supporting degerming technology, maybe will wait electric mother liquor to be heated to 80～132 ℃, and tropina is solidified, and separates obtaining animal feeding-stuff containing somatic protein.
Alkali lye of the present invention is sodium hydroxide or sodium carbonate solution, and concentration is 40% (w/w)
Compared with the prior art the present invention has the following advantages:
The present invention improves the crystalline product quality under the prerequisite that does not influence the extracting glutamic acid yield, the extract yield height, but by products such as high efficiente callback tropina, ammonium sulfate, composite fertilizer can thoroughly be eliminated the pollution of high-concentration waste water again.
Description of drawings
Fig. 1 is a process flow sheet 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 L-glutamic acid closed cycle extraction process of combining rotation crystal of the present invention adopts following processing step:
Fermented liquid described in the present embodiment is meant with starchy material or molasses raw material, by fermentation the liquid that contains L-glutamic acid of Huo Deing.
Get the 1000ml glutami acid fermentation liquor, aminoglutaric acid concentration is 11.0%, pH6.7.Put into beaker, cool to 20 ℃ with cooling bath, add while stirring and go up batch hydrolyzed solution that experiment obtains, isoelectric point crystallization technological operation routinely, control solution final pH value is 3.1, temperature is 5 ℃, and L-glutamic acid is separated out with the alpha-crystal form crystallization, and described alpha-crystal form glutamic acid crystal is irregular prism or pyramidal morphology.Continue to stir after 4 hours with whizzer separate obtain alpha-crystal form L-glutamic acid 117.5 grams (wet purity 89%, yield 95%) and etc. electric mother liquor 110ml; To wait electric mother liquor to be heated to 121 ℃, keep 5 minutes postcooling to 60 ℃, vacuum filtration, vacuum tightness is-0.09MPa to obtain wet thallus 22 grams and clear mother liquor 1080ml; Clear mother liquor continues vacuum concentration makes ammonium sulfate crystallization, and evaporating pressure be-0.09MPa, and temperature is 50 ℃, and concentrating afterwards, final volume is 160ml; After being cooled to 30 ℃, obtain 72 gram ammonium sulfate and desalination mother liquor 95ml with the whizzer centrifugation.
117.5 gram alpha-crystal form L-glutamic acid with separation obtains are dissolved in the 100ml water, add the 100ml sodium glutamate mother liquid, and are heated to 85 ℃, make the L-glutamic acid dissolving, are cooled fast to 10 ℃ with ice-water bath then, and L-glutamic acid is separated out with the beta crystal crystallization; Vacuum filtration obtains beta crystal L-glutamic acid 114 grams (wet purity 92%, yield 95%) and changes brilliant mother liquor 200ml, changes brilliant mother liquor vacuum concentration, and it is the same to concentrate condition, final concentrated solution volume 40ml.With the desalination mother liquor with change brilliant concentrated mother liquor and mix, adding 30ml concentration is the vitriol oil of 95% (w/w), 121 ℃ of hydrolysis 3 hours, be cooled to 25 ℃ with water-bath after, suction filtration under-0.06MPa vacuum degree condition obtains 120ml hydrolyzed solution and 50g filter residue; Hydrolyzed solution returns the next batch isoelectric point crystallization and transfers pH to use.
Embodiment two: the L-glutamic acid closed cycle extraction process of combining rotation crystal of the present invention adopts following processing step:
160m
3Glutami acid fermentation liquor, aminoglutaric acid concentration are 10.5%, 36 ℃ of temperature, pH6.7.Enter continuous isoelectric point crystallization jar, stream adds sodium glutamate mother liquid and hydrolyzed solution simultaneously, and the isoelectric pH ladder is 4.2～3.0, and the temperature ladder is 25～10 ℃, and promptly final isoelectric pH value is 3.0, and temperature is 10 ℃; After the electricity end, earlier with the flash liberation of conic basket type whizzer, rotating speed 1700rpm separates obtaining 17.4 tons of L-glutamic acid, and centrifugate is used the horizontal spiral centrifuge centrifugation again, and rotating speed 6000rpm obtains 2.7 tons in L-glutamic acid, waits electric mother liquor 180m
3
Enter the air flotation slot degerming Deng electric mother liquor, and filter and to obtain 4.2 tons of wet thallus, to remove mother bacterial liquid and enter quadruple effect evaporator and concentrate, concentrated condition is: the first single-effect evaporator pressure is 0.1MPa, temperature is 121 ℃, the second single-effect evaporator pressure is 0.02MPa, and temperature is 105 ℃, and third effect evaporator pressure is-0.02MPa, temperature is 90 ℃, fourth evaporator pressure is-0.06MPa that temperature is 72 ℃, concentrated solution volume 40m
3Concentrated solution is sent into the evaporative desalination crystallizer, and vacuum tightness is-0.08MPa, and temperature is 65 ℃, and controlling final concentrated solution volume is 28m
3, evaporation concentration is cooled with circulating water 40 ℃ after finishing; Separate with horizontal spiral centrifuge then, obtain 10.4 tons of ammonium sulfate crystallizations and concentrated mother liquor 19m
3
2.7 tons of L-glutamic acid that secondary separation obtains are poured into to be changeed in brilliant jar, adds 3m
3Sodium glutamate mother liquid adds 3m again
3Tap water is heated to 90 ℃ while stirring, and L-glutamic acid is fully dissolved, and then with being pumped into the crystallisation by cooling jar, with water quench to 15 ℃, separates out beta crystal L-glutamic acid; Open crystallisation by cooling pot bottom bleeder valve, make crystal solution flow into belt vacuum filter, vacuum tightness is-0.08MPa to filter and obtain 2.9 tons in beta crystal L-glutamic acid and mother liquor 6m
3Mother liquor send quadruple effect evaporator to concentrate, and operational condition is the same, and final concentrated solution volume is 2m
3With 19m
3Desalination mother liquor and 2m
3Change brilliant concentrated solution and mix, add 5.2m
3Concentration is the vitriol oil of 95% (w/w), is heated to 135 ℃ of hydrolysis 2 hours, is cooled to 50 ℃ with cooling water jecket then, pumps into flame filter press and filters, and obtains hydrolyzed solution 22m
3With 8.2 tons of filter residues, hydrolyzed solution returns electricity accent pH usefulness such as next batch.
Embodiment three: the L-glutamic acid closed cycle extraction process of combining rotation crystal of the present invention adopts following processing step:
100m
3Glutami acid fermentation liquor, aminoglutaric acid concentration are 10%, 36 ℃ of temperature, pH6.5.Enter continuous isoelectric point crystallization jar, stream adds sodium glutamate mother liquid and hydrolyzed solution simultaneously, and the isoelectric pH ladder is 4.2～3.0, and the temperature ladder is 25～10 ℃, and promptly final isoelectric pH value is 3.0, and temperature is 10 ℃; After the electricity end, use the horizontal spiral centrifuge centrifugation, rotating speed 6000rpm obtains 10.8 tons in L-glutamic acid, waits electric mother liquor 114m
3
Enter the air flotation slot degerming Deng electric mother liquor, and filter and to obtain 2.7 tons of wet thallus, to remove mother bacterial liquid and enter quadruple effect evaporator and concentrate, concentrated condition is: the first single-effect evaporator pressure is 0.1MPa, temperature is 121 ℃, the second single-effect evaporator pressure is 0.02MPa, and temperature is 105 ℃, and third effect evaporator pressure is-0.02MPa, temperature is 90 ℃, fourth evaporator pressure is-0.06MPa that temperature is 72 ℃, concentrated solution volume 30m
3Concentrated solution is sent into the evaporative desalination crystallizer, and vacuum tightness is-0.08MPa, and temperature is 65 ℃, and controlling final concentrated solution volume is 15m
3, evaporation concentration is cooled with circulating water 40 ℃ after finishing; Separate with horizontal spiral centrifuge then, obtain 6.6 tons of ammonium sulfate crystallizations and concentrated mother liquor 9.2m
3
Separate 10.8 tons of L-glutamic acid that obtain and pour in the brilliant jar of commentaries on classics, add 20m
3Sodium glutamate mother liquid, stream adds the liquid caustic soda of 20% (w/w) again, and control pH value is 4.2, is heated to 85 ℃ while stirring, and L-glutamic acid is fully dissolved, and then with being pumped into the crystallisation by cooling jar, with water quench to 15 ℃, separates out beta crystal L-glutamic acid; Open crystallisation by cooling pot bottom bleeder valve, make crystal solution flow into belt vacuum filter, vacuum tightness is-0.08MPa to filter and obtain 9.4 tons in beta crystal L-glutamic acid and mother liquor 22m
3Mother liquor send quadruple effect evaporator to concentrate, and operational condition is the same, and final concentrated solution volume is 6m
3With 9.2m
3Desalination mother liquor and 6m
3Change brilliant concentrated solution and mix, add 6m
3Concentration is the vitriol oil of 95% (w/w), is heated to 145 ℃ of hydrolysis 2 hours, is cooled to 50 ℃ with cooling water jecket then, pumps into flame filter press and filters, and obtains hydrolyzed solution 17m
3With 5.1 tons of filter residues, hydrolyzed solution returns electricity accent pH usefulness such as next batch.
Claims (10)
1. the L-glutamic acid closed cycle extracting method of a combining rotation crystal is characterized in that: adopt following processing step:
(1), glutami acid fermentation liquor is put into the isoelectric point crystallization device, with below the water quench to 30 ℃, add sodium glutamate mother liquid simultaneously, the volume of sodium glutamate mother liquid is 0～60% of a fermentating liquid volume, pH value with hydrolyzed solution or industrial vitriol oil accent fermented liquid: 3.0～3.2, temperature is reduced to 5～15 ℃, and L-glutamic acid is separated out with the alpha-crystal form crystallization;
(2), after the crystallization etc. electric mother liquor through flash liberation, obtain the alpha-crystal form glutamic acid crystal of total amount 85%; Pass through secondary separation, remaining glutamic acid crystal is separated fully with the electric mother liquor such as grade;
(3), secondary separation obtain etc. electric mother liquor separate by degerming and obtain tropina and clear mother liquor,
(4), clear mother liquor heating evaporation concentrates, control evaporator pressure :-0.01～0.1MPa, temperature is: 45～121 ℃, clear mother liquid evaporation concentrates 2～5 times;
(5), the concentrated mother liquor after the evaporation is again by the evaporation concentration desalination, makes in the concentrated mother liquor ammonium sulfate crystallization separate out evaporator pressure :-0.01～0.1MPa, temperature is: 45～121 ℃, 1～6 times of mother liquid evaporation concentrating and desalinating; Separate and obtain ammonium sulfate and desalination and concentration mother liquor;
(6), the water or the sodium glutamate mother liquid that in the residue glutamic acid crystal that obtains through secondary separation, add 2～5 times of mass ratioes, adjust the pH value with alkali lye: 4.0～6.0, while Heating temperature: 70～90 ℃, make the L-glutamic acid dissolving, temperature cools 5～30 ℃, and L-glutamic acid is separated out with the beta crystal crystallization; Be referred to as to change brilliant;
(7), commentaries on classics brilliant back separation obtains the beta crystal glutamic acid crystallization, the brilliant mother liquor of discharge commentaries on classics simultaneously;
(8), change brilliant mother liquor heating evaporation and concentrate, control evaporator pressure :-0.01～0.1MPa, temperature is: 55～121 ℃, change brilliant mother liquor and concentrate 2～8 times;
(9), the concentrated solution and the desalination and concentration mother liquor that change brilliant mother liquor mix, and adds industrial vitriol oil hydrolysis, the mass ratio that adds sulfuric acid quality and mixed concentrated liquid is 0.2～1: 1, hydrolysis temperature is: 80～150 ℃, hydrolysis time is: 1～5 hour;
(10), hydrolysis finishes postcooling to 30～80 ℃, separates obtaining solid filter residue and hydrolyzed solution, hydrolyzed solution is circulated back to isoelectric point crystallization.
2. the L-glutamic acid closed cycle extracting method of combining rotation crystal according to claim 1 is characterized in that described separation method adopts centrifugal or filtration, centrifuge speed: 1400～6000rpm.
3. the L-glutamic acid closed cycle extracting method of combining rotation crystal according to claim 1 is characterized in that described alpha-crystal form glutamic acid crystal is irregular prism or pyramidal morphology.
4. the L-glutamic acid closed cycle extracting method of combining rotation crystal according to claim 1 is characterized in that described evaporation operation adopts single-action or multiple-effect evaporation.
5. the L-glutamic acid closed cycle extracting method of combining rotation crystal according to claim 1 is characterized in that described evaporative desalination adopts single-action or multiple-effect evaporation.
6. the L-glutamic acid closed cycle extracting method of combining rotation crystal according to claim 1 is characterized in that described beta crystal glutamic acid crystallization body is irregular needle-like or lamellar morphology.
7. the L-glutamic acid closed cycle extracting method of combining rotation crystal according to claim 1 is characterized in that described sodium glutamate mother liquid adds before isoelectric point crystallization, also can add when changeing brilliant, or isoelectric point crystallization and commentaries on classics adds when brilliant simultaneously.
8. the L-glutamic acid closed cycle extracting method of combining rotation crystal according to claim 1 is characterized in that described isoelectric point crystallization adopts electricity or continuous isoelectric point crystallizations such as intermittence.
9. the L-glutamic acid closed cycle extracting method of combining rotation crystal according to claim 1, it is characterized in that described degerming separates employing air supporting degerming technology, maybe will wait electric mother liquor to be heated to 80～132 ℃, tropina is solidified, separate obtaining animal feeding-stuff containing somatic protein.
10. the L-glutamic acid closed cycle extracting method of combining rotation crystal according to claim 1 is characterized in that described alkali lye is sodium hydroxide or sodium carbonate solution.
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| CN2007101903867A CN101157625B (en) | 2007-11-27 | 2007-11-27 | Glutamic acid closed cycle abstraction process combined with crystal transformation |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101717343B (en) * | 2009-11-25 | 2012-07-18 | 李平凡 | Glutamic acid crystallization method for preventing and controlling Beta-type crystal from occurring and application thereof |
| CN101735088B (en) * | 2009-11-30 | 2013-02-27 | 北京坡华生物科技有限公司 | Production process of glutamic acid and monosodium glutamate |
| CN101973901B (en) * | 2010-09-20 | 2013-10-30 | 江南大学 | Glutamic acid continuous isoelectric crystallization method |
| CN102120722B (en) * | 2010-12-29 | 2013-11-27 | 菱花集团有限公司 | Method for recycling glutamic acid from desalting liquid |
| CN109987614A (en) * | 2017-12-30 | 2019-07-09 | 许传高 | A method of extracting ammonium sulfate from glutamic acid fermentation tail washings |
| CN113072457A (en) * | 2021-04-07 | 2021-07-06 | 华东理工大学 | Method for freezing, concentrating and isoelectric point crystallizing glutamic acid |
| CN114433294B (en) * | 2022-02-18 | 2023-08-22 | 郇玉芝 | Preparation process of biological amino acid |
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