CN101156675A - Glutamic acid abstraction technics combining rotation crystal - Google Patents
Glutamic acid abstraction technics combining rotation crystal Download PDFInfo
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- CN101156675A CN101156675A CNA2007101354130A CN200710135413A CN101156675A CN 101156675 A CN101156675 A CN 101156675A CN A2007101354130 A CNA2007101354130 A CN A2007101354130A CN 200710135413 A CN200710135413 A CN 200710135413A CN 101156675 A CN101156675 A CN 101156675A
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Abstract
The invention relates to a glutamic acid extraction process combined with crystal dispersion, and belongs to the fermented food industry technical field. Firstly, fermentation liquid is evaporated and concentrated, and then is continuously crystallized after being cooled, the glutamic acid crystal and isoelectronic broth with Alpha-crystal type can be obtained through separation; the isoelectronic broth is heated and separated to recover tropina, and clean broth is put in an evaporation and desalination crystallizer, in order to obtain ammonium sulfate crystal through crystallization and separation, and a small amount of broth is remained to produce compound fertilizer; the Alpha-crystal type glutamic acid is rapidly crystallized after being crystallized and dissolved, in order to be converted into Beta-crystal type dispersed crystal, and then the finished glutamic acid product can be obtained through separation. Humic substance and hydrolyzed liquid are obtained through concentrating and separating the dispersed crystal by adding acid, and the hydrolyzed liquid is cycled to a continuous crystallizer, and is used as isoelectronic crystallization used acid; and the condensed water drained out is used as the raw material handling water. The glutamic acid crystal obtained by the invention has good crystallization quality, meanwhile, a plurality of by-products of the tropina, the ammonium sulfate and the compound organic fertilizer, etc. can be obtained, thereby not only improving the product quality, but also eliminating wastewater pollution of high concentration.
Description
Technical field
The present invention relates to a kind of extraction technology of glutamic acid of combining rotation crystal, belong to the fermented food industry technical field.
Background technology
Glutamic acid is a kind of important amino acid, is mainly used to produce tasty agents 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 technology of glutamic acid mainly is a fermentation method, is raw material with starch or molasses, obtains by fermentation, extraction.
In prior art, the current technology of extracting glutamic acid from zymotic fluid normally adopts following several method: isoelectric point crystallization adds ion-exchange process, concentrate isoelectric point crystallization adds and changes brilliant technology and closed cycle extraction process (Chinese patent application number: 96116404.2 1 kinds of methods of extracting glutamic acid from zymotic fluid) 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 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 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 spray-drying, atmosphere polluting problem is very serious.
Closed cycle extraction process (number of patent application: 96116404.2 1 kinds of methods of from zymotic fluid, extracting 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.
Obviously, optimum extraction technology of glutamic acid should be taken into account extract yield, crystalline product quality and pollutant discharge amount, reaches the consistent of business economic benefit and social benefit.
The key operation that influences the extracting glutamic acid yield is an isoelectric point crystallization.The waiting electricity or wait in the electricity operation continuously of routine in batches, wait electricity to finish the back and wait in the electric mother liquor residual 2~2.5% glutamic acid, and in concentrated isoelectric point crystallization, the concentration of residual glutamic acid is up to 2.5~4.0% in the mother liquor.Obviously, how effectively reduction waits that residual aminoglutaric acid concentration is the main path that improves extract yield in the electric mother liquor.
According to crystallization theory, have only the identical molecule of character in lattice, to grow up, therefore, impurity in the crystalline solid is mainly derived from containing between the occlusion of plane of crystal and crystal, by washing means such as crystalline substance, commentaries on classics crystalline substance, can effectively reduce impurity concentration, improve crystal mass.
Deng the solute that contains 6~12% in the electric mother liquor, mainly be mycoprotein, ammonium sulfate, glutamic acid, residual sugar and other amino acid.By rational technology, from wait electric mother liquor, reclaim above-mentioned substance, not only eliminated the problem of environmental pollution that direct discharging brings, also can turn waste into wealth, can further improve the business economic benefit.
Summary of the invention
The objective of the invention is to overcome above-mentioned weak point, thereby a kind of extraction technology of glutamic acid of combining rotation crystal is provided, electric extract yield such as can improve; Effectively mycoprotein is separated and reclaim; Accessory substances such as recyclable ammonium sulfate, composite fertilizer, and can thoroughly eliminate the pollution of high-concentration waste water.
Main solution of the present invention is achieved in that
The extraction technology of glutamic acid of combining rotation crystal of the present invention adopts following processing step:
1, adopt starchy material or molasses raw material to obtain to contain the zymotic fluid of glutamic acid by fermentation;
2, zymotic fluid concentrates through heating evaporation, evaporator pressure :-0.01~0.1MPa, and temperature is 45~121 ℃, glutami acid fermentation liquor evaporation and concentration (liquid volume ratio before and after the evaporation) is: 2~5 times;
3, evaporation and concentration after fermentation liquid is cooled to 25~50 ℃, enters continuous isoelectric point crystallization device, with hydrolyzate or the concentrated sulfuric acid (concentration is greater than 90%) adjust pH: 3.0~3.2, be cooled to 5~15 ℃ again, glutamic acid is separated out with the alpha-crystal form crystallization;
4, the zymotic fluid after the crystallization separate obtain the alpha-crystal form glutamic acid crystal and etc. electric mother liquor;
5, etc. electric mother liquor is heated to 80~132 ℃, separates obtaining mycoprotein and clear mother liquor;
6, clear mother liquor is by evaporative desalination workshop section evaporation and concentration, and ammonium sulfate crystallization is separated out; Evaporator pressure :-0.01~0.1MPa, temperature is: 45~121 ℃, it is 2~6 times that clear mother liquid evaporation concentrates (liquid volume ratio before and after the evaporation); Separate and obtain ammonium sulfate and concentrated mother liquor;
7, concentrated mother liquor can partly or entirely continue evaporation and concentration, or after adding potassium chloride or calcium superphosphate or phosphoric acid ammonia salt element, drying is made composite fertilizer;
8, in alpha-crystal form glutamic acid, add the water of 2~5 times of mass ratioes or from the monosodium glutamate crystalline mother solution of glutamate production refining step, adjust the pH value of solution value with alkali lye: 4.0~6.0, temperature is heated to 70~90 ℃, make the dissolving of alpha-crystal form glutamic acid, cool fast then to 5~30 ℃, glutamic acid is separated out with the beta crystal crystallization, be referred to as to change brilliant;
9, 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;
10, the brilliant mother liquor heating evaporation of commentaries on classics is concentrated, control evaporator pressure :-0.01~0.1MPa, and temperature is: 55~121 ℃, changeing brilliant mother liquid evaporation concentrated (evaporation front and back liquid volume ratio) is 2~8 times;
11, change brilliant concentrate and add sulphuric acid hydrolysis, adding sulfuric acid quality is 0.2~1 times of concentrate quality, and hydrolysis temperature is: 80~150 ℃, hydrolysis time is: 1~5 hour;
12, hydrolysis finishes the back and separates that to obtain the solid filter residue be humus and hydrolyzate, and the solid filter residue can be used as fertilizer, and hydrolyzate loops back continuous isoelectric point crystallization.
Heating evaporation of the present invention concentrates, and evaporation operation can adopt single-action or multiple-effect evaporations such as triple effect, quadruple effect.
Alpha-crystal form glutamic acid crystal of the present invention has irregular prism or pyramidal morphology.
Sylvite of the present invention is potassium chloride, and addition is 0.2~3% (w/w) of concentrate, and phosphate is calcium superphosphate or phosphoric acid ammonia salt element, and addition is 0.1 (w/w) of concentrate.
Can add alkali in the alpha-crystal form glutamic acid of the present invention, glutamic acid is separated out with the beta crystal crystallization.Used alkali lye is sodium carbonate or sodium hydroxide solution, and concentration is 10~40% (w/w), and addition is 0~20% (w/w) of alpha-crystal form glutamic acid.
Beta crystal glutamic acid crystal of the present invention has irregular needle-like or lamellar morphology.
The zymotic fluid concentration of glutamic acid of the present invention is 9.8~10.5%, pH value: 6.5~6.7.
Starchy material of the present invention is: corn, rice, wheat.
Molasses raw material of the present invention is: sugarcane, beet molasses.
Compared with the prior art the present invention has the following advantages:
1, extract yield height: the present invention optimizes crystalline environment by means such as thin brilliant elimination, thereby effective residual acid concentration≤2.0% in the electric mother liquor such as control such as has improved at electric extract yield.
But 2 high efficiente callback mycoproteins: since zymotic fluid through concentrating, etc. operations such as electricity, solution viscosity is big, and thalline itself is a kind of plasticity particle, adopts traditional methods such as air supporting to be difficult to effectively mycoprotein be separated recovery.The present invention adopts heating that mycoprotein is solidified, and improves its strainability, by separation equipment such as flame filter press, band filters, can reclaim mycoprotein smoothly, has also created good condition for next step evaporative desalination operation.
3, accessory substances such as recyclable ammonium sulfate, composite fertilizer are thoroughly eliminated the pollution of high-concentration waste water again.
4, good product quality: by changeing brilliant, removed most of impurity of crystal occlusion, crystallization purity improves greatly; Change brilliant mother liquor and concentrate posthydrolysis, and the hydrolyzate reuse is waited electricity continuously, avoided changeing brilliant influence yield.
Description of drawings
Fig. 1 is a process chart of the present invention.
The specific embodiment
Embodiment during following the present invention incites somebody to action in conjunction with the accompanying drawings is further described:
Embodiment one:
The extraction technology of glutamic acid of combining rotation crystal of the present invention adopts following processing step:
Zymotic fluid of the present invention is meant with starchy material or molasses raw material, by fermentation the liquid that contains glutamic acid of Huo Deing.
1000ml glutami acid fermentation liquor, aminoglutaric acid concentration are 10.0%, and the pH value is: 6.7.In cold boiler, concentrate earlier, fermentating liquid volume is dwindled.Evaporation operation adopts single-action to concentrate: evaporating pressure is :-0.09MPa, and temperature is: 50 ℃, cycles of concentration is about 3 times, concentrates back concentrate volume to be: 350ml; The limit slowly drips the stirring of hydrolyzate limit in concentrate, makes the final pH value be: 3.1, and cool 10 ℃, glutamic acid is separated out with the alpha-crystal form crystallization; After isoelectric point crystallization finishes, pour liquid into tripod pendulum type batch centrifugal, with the rotating speed centrifugation that per minute 1400 changes, obtain alpha-crystal form glutamic acid 112 grams and etc. electric mother liquor 310ml; Described alpha-crystal form glutamic acid crystal has irregular prism or pyramidal morphology.To wait electric mother liquor to be heated to 121 ℃, and keep after 5 minutes and be cooled to 60 ℃, and use the Buchner funnel vacuum filtration, vacuum is :-0.09MPa obtains wet thallus (mycoprotein) 22 grams and clear mother liquor 240ml; Clear mother liquor continuation vacuum concentrates and makes ammonium sulfate crystallization, and evaporating pressure is :-0.09MPa, and temperature is: 50 ℃, concentrating the back final volume is 100ml; After being cooled to 30 ℃, with the rotating speed centrifugation that per minute 1400 changes, obtain 70 gram ammonium sulfate and concentrated mother liquor 40 grams with tripod pendulum type batch centrifugal;
112 gram alpha-crystal form glutamic acid with separation obtains are dissolved in the 200ml water, and dripping concentration is the sodium hydroxide solution 20ml of 4% (w/w), make the pH value of solution value be: 4.0, and be heated to 85 ℃, make the glutamic acid dissolving, be cooled fast to 10 ℃ with ice-water bath then, glutamic acid is separated out with the beta crystal crystallization; Vacuum filtration, vacuum is :-0.09MPa, obtain beta crystal glutamic acid 105 gram and mother liquor 220ml, described beta crystal glutamic acid crystal has irregular needle-like or lamellar morphology.The mother liquor vacuum is concentrated, evaporating pressure is :-0.09MPa, temperature is: 50 ℃, final concentrate volume 40ml, adding 18g concentration is the concentrated sulfuric acid of 92% (w/w), 121 ℃ of hydrolysis 1 hour, be cooled to 25 ℃ with water-bath after, suction filtration under-0.06MPa vacuum degree condition obtains 40ml hydrolyzate and 15g filter residue; Hydrolyzate returns next group isoelectric point crystallization operation adjust pH and uses.
Embodiment two:
The extraction technology of glutamic acid of combining rotation crystal of the present invention adopts following processing step:
Get 100m
3Glutami acid fermentation liquor, aminoglutaric acid concentration is: 10.5%, temperature: 36 ℃, the pH value is: 6.7.Send into tubular heat exchanger, respectively with quadruple effect discharging concentrate and degerming after etc. the clear mother liquor heat exchange of electricity, with the recovery section heat, heat exchange after fermentation liquid temp rises to 65 ℃, entering four-effect evaporator concentrates, 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 ℃, third effect evaporator pressure is :-0.02MPa, temperature is: 90 ℃, fourth evaporator pressure is :-0.06MPa, and temperature is: 72 ℃, cycles of concentration is 2.5 times, concentrate volume 40m
3Enter continuous isoelectric point crystallization workshop section, the electricity such as hydrolyzate accent that batch operation obtains before adding, isoelectric pH value ladder is: 4.2~3.0, the temperature ladder is: 45~10 ℃, promptly final isoelectric pH value is: 3.0, temperature is: 10 ℃; Isoelectric point crystallization is used the horizontal spiral centrifuge centrifugation after finishing, and rotating speed is that per minute 6000 changes, and obtains 10.6 tons in alpha-crystal form glutamic acid; Described alpha-crystal form glutamic acid crystal has irregular prism or pyramidal morphology.Electric mother liquors such as residue filter with flame filter press then with the livings Steam Heating to 80 of 0.3MPa ℃, obtain 2.2 tons of wet thallus and mother liquor 29m clearly
3Clear mother liquor single-action vacuum concentrates, and vacuum be-0.08MPa that temperature is: 65 ℃, evaporation process discontinuous stream adds clearly mother liquor and with liquefied ammonia adjusting pH value 4.0, controls final concentrate volume and is: 10m
3, evaporation and concentration is cooled with circulating water 40 ℃ after finishing; Separate with the conic basket type centrifuge then, obtain 4.2 tons of 6.5 tons of ammonium sulfate crystallizations and concentrated mother liquors; Concentrated mother liquor send granulating and drying machine, under 180 ℃ of conditions of EAT, and dry 2.8 tons of solids, this solid can be used as composite fertilizer.
Alpha-crystal form glutamic acid is poured into to be changeed in brilliant jar, adds 8m
3The monosodium glutamate refinement mother liquor adds 13m again
3Running water is heated to 90 ℃ while stirring, and 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 glutamic acid.Open crystallisation by cooling pot bottom bleeder valve, make crystal solution flow into belt vacuum filter, vacuum is-0.08MPa to filter and obtain 10.5 tons in beta crystal glutamic acid and mother liquor 21m
3Described beta crystal glutamic acid crystal has irregular needle-like or lamellar morphology.Mother liquor send four-effect evaporator to concentrate, and operating condition is the same, and final concentrate volume is 5m
3, pump is transported to 10m
3Hydrolytic decomposition pot adds 2.5 tons of concentration and is 93% the concentrated sulfuric acid, 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 hydrolyzate 6m
3With 1.2 tons of filter residues, hydrolyzate returns next group isoelectric point crystallization operation adjust pH and uses.
Embodiment three:
The extraction technology of glutamic acid of combining rotation crystal of the present invention adopts following processing step:
Get 100m
3Glutami acid fermentation liquor, aminoglutaric acid concentration are 9.8%, and 36 ℃ of temperature, pH value are 6.5.Send into tubular heat exchanger, respectively with quadruple effect discharging concentrate and degerming after etc. the clear mother liquor heat exchange of electricity, temperature rises to 60 ℃, enters four-effect evaporator to concentrate, cycles of concentration is 3.3 times, is concentrated to 30m
3, concentrated condition is: the first single-effect evaporator pressure is 0MPa, and temperature is 101 ℃, and the second single-effect evaporator pressure is-0.04MPa, temperature is 85 ℃, and third effect evaporator pressure is-0.07MPa that temperature is 70 ℃, fourth evaporator pressure is-0.08MPa, and temperature is 56 ℃; Enter continuous isoelectric point crystallization workshop section, stream adds electricity such as hydrolyzate accent, and the isoelectric pH ladder is 4.2~3.1, and the temperature ladder is 45~15 ℃, and promptly final isoelectric pH value is 3.1, and temperature is 15 ℃; After the electricity end, use the horizontal spiral centrifuge centrifugation, rotating speed is that per minute 6000 changes, and obtains 10.0 tons in alpha-crystal form glutamic acid; Described alpha-crystal form glutamic acid crystal has irregular prism or pyramidal morphology.Electric mother liquors such as residue filter with flame filter press then with the livings Steam Heating to 115 of 0.3MPa ℃, obtain 2.3 tons of wet thallus and mother liquor 28m clearly
3Clear mother liquor adopts two effect vacuum to concentrate, and first imitates pressure is-0.03MPa, and temperature is 92 ℃, and second imitates pressure is-0.08MPa, and temperature is 65 ℃, and controlling final concentrate volume is 10m
3, evaporation and concentration is cooled with circulating water 40 ℃ after finishing; Separate with the conic basket type centrifuge then, obtain 4.2 tons of 6.4 tons of ammonium sulfate crystallizations and concentrated mother liquors; After adding 2% potassium chloride, 0.5% calcium superphosphate in the concentrated mother liquor, concentrated mother liquor send spray dryer, under 160 ℃ of conditions of EAT, and dry 2.8 tons of solids, this solid can be used as composite fertilizer.
Alpha-crystal form glutamic acid is poured into to be changeed in brilliant jar, adds 5m
3The monosodium glutamate refinement mother liquor adds 20m again
3Running water, adding concentration and be 40% alkali lye, to adjust the pH value be 4.2, is heated to 85 ℃ while stirring, and glutamic acid is fully dissolved, and then with being pumped into the crystallisation by cooling jar, with water quench to 10 ℃, separates out beta crystal glutamic acid; Open crystallisation by cooling pot bottom bleeder valve, make crystal solution flow into belt vacuum filter, vacuum is-0.08MPa to filter and obtain 9.7 tons in beta crystal glutamic acid and mother liquor 24m
3Described beta crystal glutamic acid crystal has irregular needle-like or lamellar morphology.Mother liquor send four-effect evaporator to concentrate, and operating condition is the same, and final concentrate volume is 4m
3, pump is transported to 10m
3Hydrolytic decomposition pot adds 3 tons of concentration and is 93% the concentrated sulfuric acid, is heated to 145 ℃ of hydrolysis 1 hour, is cooled to 50 ℃ with cooling water jecket then, pumps into flame filter press and filters, and obtains hydrolyzate 4.5m
3With 1.2 tons of filter residues, hydrolyzate returns next group isoelectric point crystallization operation adjust pH and uses.
Claims (4)
1. the extraction technology of glutamic acid of a combining rotation crystal is characterized in that adopting following processing step:
(1), adopt starchy material or molasses raw material to obtain to contain the zymotic fluid of glutamic acid by fermentation;
(2), glutami acid fermentation liquor concentrates through heating evaporation, evaporator pressure :-0.01~0.1MPa, temperature is: 45~121 ℃, 2~5 times of glutami acid fermentation liquor evaporation and concentration;
(3), evaporation and concentration after fermentation liquid is cooled to 25~50 ℃, enters continuous isoelectric point crystallization device, with hydrolyzate or concentrated sulfuric acid adjust pH: 3.0~3.2, be cooled to 5~15 ℃ again, glutamic acid is separated out with the alpha-crystal form crystallization;
(4), the zymotic fluid behind the isoelectric point crystallization separate obtain the alpha-crystal form glutamic acid crystal and etc. electric mother liquor;
(5), etc. electric mother liquor be heated to 80~132 ℃, separate to obtain mycoprotein and clear mother liquor;
(6), clear mother liquor is by evaporative desalination workshop section evaporation and concentration, and ammonium sulfate crystallization is separated out; Evaporator pressure :-0.01~0.1MPa, temperature is: 45~121 ℃, clear mother liquid evaporation simmer down to: 2~6 times; Separate and obtain ammonium sulfate and concentrated mother liquor;
(7), concentrated mother liquor can partly or entirely continue evaporation and concentration, or adds potassium chloride and calcium superphosphate or phosphoric acid ammonia element, drying is made composite fertilizer;
(8), the water or the monosodium glutamate crystalline mother solution that in alpha-crystal form glutamic acid, add 2~5 times of mass ratioes, adjust the pH value of solution value with alkali lye: 4.0~6.0, temperature is heated to 70~90 ℃, make the dissolving of alpha-crystal form glutamic acid, cool then to 5~30 ℃, glutamic acid is separated out with the beta crystal crystallization, be referred to as to change brilliant;
(9), commentaries on classics brilliant back separation obtains the beta crystal glutamic acid crystallization, the brilliant mother liquor of discharge commentaries on classics simultaneously;
(10), change brilliant mother liquor heating evaporation and concentrate, control evaporator pressure :-0.01~0.1MPa, temperature is: 55~121 ℃, change 2~8 times of brilliant mother liquid evaporation simmer down tos;
(11), change brilliant concentrate and add sulphuric acid hydrolysis, add the sulfuric acid quality and be 0.2~1 times of concentrate quality, hydrolysis temperature is: 80~150 ℃, hydrolysis time is: 1~5 hour;
(12), hydrolysis finishes the back and separates that to obtain the solid filter residue be humus and hydrolyzate, the solid filter residue can be used as fertilizer, hydrolyzate loops back continuous isoelectric point crystallization.
2. the extraction technology of glutamic acid of combining rotation crystal according to claim 1 is characterized in that described alpha-crystal form glutamic acid crystal has irregular prism or pyramidal morphology.
3. the extraction technology of glutamic acid of combining rotation crystal according to claim 1 is characterized in that described sylvite is 0.2~3% of concentrate for the potassium chloride addition, and phosphate is calcium superphosphate or phosphoric acid ammonia element, and addition is 0.1~5% of a concentrate.
4. the extraction technology of glutamic acid of combining rotation crystal according to claim 1 is characterized in that described beta crystal glutamic acid crystal has irregular needle-like or lamellar morphology.
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CN101973901A (en) * | 2010-09-20 | 2011-02-16 | 江南大学 | Glutamic acid continuous isoelectric crystallization method |
CN101973901B (en) * | 2010-09-20 | 2013-10-30 | 江南大学 | Glutamic acid continuous isoelectric crystallization method |
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CN106674034B (en) * | 2016-12-28 | 2019-03-22 | 宝鸡阜丰生物科技有限公司 | The method of metacrystal mother liquid recycling in glutamic acid production |
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 |
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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