CN101671705A - Extraction technology of glutamic acid recovered by combining crystal transformation and ion exchange - Google Patents
Extraction technology of glutamic acid recovered by combining crystal transformation and ion exchange Download PDFInfo
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- CN101671705A CN101671705A CN200910012705A CN200910012705A CN101671705A CN 101671705 A CN101671705 A CN 101671705A CN 200910012705 A CN200910012705 A CN 200910012705A CN 200910012705 A CN200910012705 A CN 200910012705A CN 101671705 A CN101671705 A CN 101671705A
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Abstract
The invention relates to an extraction technology of a glutamic acid recovered by combining crystal transformation and ion exchange, belonging to the technical field of food industry. The extraction technology comprises the following technical steps: using the fermentation liquor of the glutamic acid, and heating, evaporating and concentrating the fermentation liquor; cooling the fermentation liquor to 25-50 DEG C after the fermentation liquor is evaporated and concentrated so that the glutamic acid is crystallized and separated out in an alpha form; obtaining an alpha form glutamic acid crystal, a first isoelectric separation mother liquor and a secondary separation mother liquor; enabling the glutamic acid to be crystallized and separated out in a beta crystal form, calling crystal transformation; separating feed liquor to obtain a beta crystal form glutamic acid crystal after the crystal transformation; after the secondary separation mother liquor is concentrated, adding a sulphuricacid to hydrolyze the concentrated secondary separation mother liquor, separating to obtain hydrolysis liquid and solid filter residues, i.e. humus; returning the first isoelectric separation motherliquor to a continuous crystallizing tank, and then using the first isoelectric separation mother liquor as an acid for isoelectric crystallization. The invention achieves the total extraction yield of 97-98 percent, greatly enhances the crystallization purity, greatly reduces the consumption of the sulphuric acid and liquid ammonia, recovers the mycoprotein and thoroughly eliminates the pollutionof high-concentration waste water.
Description
Technical field
The invention belongs to the foodstuffs industry technology, particularly a kind of extraction technology of glutamic acid that changes brilliant coupled ion exchange recovery.
Background technology
96116404.2 1 kinds of methods of extracting L-glutamic acid from fermented liquid), concentrate continuous isoelectric point crystallization and add and change the extraction process (Chinese patent application number: the extraction technology of glutamic acid of 200710135413.0 combining rotation crystals) that crystalline substance adds the tropina recovery in prior art, the current technology of extracting L-glutamic acid from fermented liquid normally adopts following several method: the extraction process that a step is freezing to be waited electricity to add ion-exchange to reclaim, concentrate continuous isoelectric point crystallization and add and change brilliant technology, closed cycle extraction process (Chinese patent application number:.
The extraction process that electricity such as one step is freezing add the ion-exchange recovery is the most widely used extraction process of domestic L-glutamic acid manufacturing enterprise, its advantage is the extract yield height of L-glutamic acid, reach more than 95%, but shortcoming is also a lot, because the supernatant liquor that waits electricity to extract to discharge is all through residual 2～2.5% L-glutamic acid in the ion-exchange recovery supernatant liquor, make that the consumption of sulfuric acid, liquefied ammonia is bigger, wastewater discharge also ferments the liquid measure increase more than 50%.Along with the raw and auxiliary material rise in price of sulfuric acid, liquefied ammonia etc., its cost also improves, and does not also meet environmental requirement.
Concentrating continuous isoelectric point crystallization, to add the advantage of changeing brilliant technology be that the L-glutamic acid quality extracted is good, do not have ion-exchange to reclaim link, sulfuric acid, liquefied ammonia consumption reduction, and high-concentration waste liquid reduces more than 60%, has alleviated environmental protection pressure; Shortcoming is that extract yield is low, generally only 88～90%, and the primary raw materials that is equivalent to resource consumes high, and fox extracting thallus protein not, has wasted the waste liquid resource.
(Chinese patent application number: 96116404.2 1 kinds of methods of extracting L-glutamic acid from fermented liquid) advantage is to have removed ion-exchange to reclaim link, sulfuric acid, liquefied ammonia consumption and reduce, thoroughly solved problem of environmental pollution to the closed cycle extraction process, but because feed liquid closed cycle, there is not removal of impurity link, make that the glutamic acid crystallization impurity that obtains is many, color and luster heavy, poor quality.
Concentrating continuous isoelectric point crystallization adds and changes the brilliant extraction process that the tropina reclaims (Chinese patent application number: the extraction technology of glutamic acid of 200710135413.0 combining rotation crystals) just add at concentrated continuous isoelectric point crystallization and increased tropina recovery link on the basis of changeing brilliant technology that adds, superior product quality, fully utilized the waste liquid resource, extracted tropina, compliance with environmental protection requirements, but do not solve the low problem of extract yield, the primary raw materials of resource consumes high, products production cost height.
Summary of the invention
The objective of the invention is to overcome above-mentioned weak point, provide a kind of and can improve extraction yield, improve the quality of products, fully utilize the waste liquid resource, reduce to pollute the extraction technology of glutamic acid that the brilliant coupled ion exchange of commentaries on classics of compliance with environmental protection requirements is reclaimed.
The technical scheme that technical solution problem of the present invention adopts is:
Change the following processing step of extraction technology of glutamic acid employing that brilliant coupled ion exchange is reclaimed:
1, adopt starchy material such as corn, rice, wheat or molasses raw materials such as sugarcane, beet to obtain by fermentation to contain that concentration is 9～16%, pH value is the fermented liquid of 6.3～6.7 L-glutamic acid;
2, fermented liquid concentrates through heating evaporation, evaporator pressure :-0.01-0.1MPa, and temperature 40-95 ℃, the liquid volume ratio is 2～5: 1 before and after the evaporation of glutami acid fermentation liquor;
3, evaporation concentration secondary fermentation liquid is cooled to 25～50 ℃, enters continuous isoelectric point crystallization device, transfers PH to 3.0-3.2 with hydrolyzed solution or concentration greater than 90% sulfuric acid and the high stream of acidifying, is cooled to 5～15 ℃ again, and L-glutamic acid is separated out with the crystallization of α type;
4, crystallization feed liquid through separate, wash crystalline substance, secondary separation obtains α type glutamic acid crystal and separates mother liquor and secondary separation mother liquor with an inferior electricity;
5, in α type L-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, with concentration is that 15～35% yellow soda ash or sodium hydroxide lye are adjusted the solution pH value: 4.0～6.0, temperature is heated to 70～90 ℃, make the dissolving of alpha-crystal form L-glutamic acid, cool fast then to 5～30 ℃, L-glutamic acid is separated out with the beta crystal crystallization, be referred to as to change brilliant;
6, change brilliant back feed liquid and obtain the beta crystal glutamic acid crystallization, discharge simultaneously and change brilliant mother liquor through separation; Change brilliant mother liquor as washing brilliant water reuse;
7, the secondary mother liquid heating evaporation to secondary separation concentrates, control evaporator pressure :-0.01-0.1MPa, and temperature 40-95 ℃, the liquid volume ratio is before and after the evaporation of secondary mother liquid: 2～8: 1
8, secondary mother liquid concentrates back adding sulphuric acid hydrolysis, and adding sulfuric acid quality is 0.2～1 times of concentrated solution quality, and hydrolysis temperature is: 80-150 ℃, hydrolysis time is: 1～5 hour;
9, after hydrolysis finished, separation obtains hydrolyzed solution and the solid filter residue is a soil ulmin, and hydrolyzed solution returns continuous isoelectric point crystallization, and solid filter residue main component is a protein, can be used as the raw material of system biological fermentation fertilizer.
10, an inferior electric mother liquor adopts the molten gas of nature and evenly dissolves in the flocculation agent method, and dissolved air flotation obtains tropina and Deproteinization mother liquor;
11, the Deproteinization mother liquor adopts ion-exchange process for recovering glutamic acid, after the L-glutamic acid of recovery adds sulfuric acid acidation, gets back to the continuous crystallisation jar and does isoelectric point crystallization with sour.The tail washings that the Deproteinization mother liquor is discharged behind ion-exchange absorption L-glutamic acid, concentrate through multiple-effect evaporator, ammonium sulfate crystallization is separated out, the ammonium sulfate crystallization mother liquor concentrates through multiple-effect evaporation again, obtain dry matter content at 45～50% last mother liquor, the last mother liquor mixes employing dry method composting with ammonium sulfate, composting auxiliary material, secondary separation mother liquor hydrolysed filtrate slag, make biological fermentation fertilizer.
The invention has the beneficial effects as follows:
1, the present invention adopts ion-exchange to reclaim the L-glutamic acid technology, fully reclaimed the L-glutamic acid in the inferior electric mother liquor, change brilliant mother liquor as washing brilliant water reuse, change brilliant mother liquor secondary separation mother liquor and concentrate posthydrolysis, and the hydrolyzed solution reuse waited continuously, avoided washing brilliant and the brilliant influence to yield of commentaries on classics, total extract yield reaches 97-98%.
2, by changeing brilliant, removed most of impurity of crystal occlusion, crystallization purity improves greatly.
3, the present invention adopts fermented liquid to concentrate electricity extractions such as back, material liquid volume is 1/3～1/5 of a fermentating liquid volume, the amount of one inferior electric mother liquor is 1/3～1/5 of a fermentating liquid volume, the reduction of feed volume of ion-exchange recycling is that 1/3～1/5 of reduction of feed volume is handled in the conventional ion exchange, make that under the prerequisite that has guaranteed total extract yield, the consumption of sulfuric acid, liquefied ammonia reduces significantly.
4, an inferior electric mother liquor adopts the molten gas of nature (without air compressor machine) and evenly dissolves in the flocculation agent method, and thoroughly flocculation is floating to make tropina, realizes the comprehensive utilization of waste liquid, makes tropina obtain reclaiming.
5, recyclable ammonium sulfate, turn waste into wealth, produce biological fermentation fertilizer, thoroughly eliminate the pollution of high-concentration waste water again.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Enforcement during following the present invention incites somebody to action in conjunction with the accompanying drawings is further described:
Embodiment one:
The present invention changes the following processing step of extraction technology of glutamic acid employing that brilliant coupled ion exchange is reclaimed:
Fermented liquid of the present invention is with starchy material or molasses raw material, by fermentation the liquid that contains L-glutamic acid of Huo Deing.
1000ml glutami acid fermentation liquor, aminoglutaric acid concentration are 10.8%, and pH value is: 6.7.In vacuum-evaporator, concentrate earlier, fermentating liquid volume is dwindled.Evaporation operation adopts single-action to concentrate: evaporating pressure is :-0.09MPa, and temperature is: 52 ℃, cycles of concentration is about 3 times, concentrates the back material liquid volume to be: 350ml; The limit slowly drips the stirring of hydrolyzed solution limit in concentrated solution, makes final pH value be: 3.1, and cool 8 ℃, L-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 L-glutamic acid 122 grams and etc. electric mother liquor 310ml; Under agitation condition, 1.5% of adding mother liquor volume 1# flocculation agent in waiting electric mother liquor, 0.5% 2# flocculation agent, left standstill 10 minutes, use the B vacuum filtration, vacuum tightness is-0.09MPa, obtains wet thallus (tropina) 24 grams and clear mother liquor 300ml, and clear mother liquor is transferred PH to 1.5 with sulfuric acid, just going up ion exchange column, when ion exchange column does not have adsorption tail liquid and flows out, make eluent with 10% ammoniacal liquor, instead go up 120ml, soaked resin to liquid level, from the water inlet of ion exchange column top, collect the 75ml feed liquid simultaneously from the bottom earlier and flow as height, add sulfuric acid and transfer PH to 1.5, become the high stream of acidifying 85ml, add acid for electricity such as next batchs and use; Collection of ions exchange column lower prop material 45ml, the wash-out supplement when criticizing the post wash-out are down collected and are pushed down water 70ml, are used for following batch post and prepare ammoniacal liquor eluent usefulness.Adsorption tail liquid makes ammonium sulfate crystallization through vacuum concentration again, and evaporating pressure is :-0.09MPa, and temperature is: 50 ℃, concentrating the back final volume is 126ml, after being cooled to 30 ℃, with the rotating speed centrifugation that per minute 1400 changes, obtain 76 gram ammonium sulfate and ammonium sulfate crystallization mother liquor 50ml with tripod pendulum type batch centrifugal; Crystalline mother solution through being concentrated in vacuo to 10ml, is the last mother liquor again.
The 122 gram alpha-crystal form L-glutamic acid that separation is obtained are dissolved in the 220ml water, and dripping concentration is the sodium hydroxide solution 18ml of 5% (w/w), makes solution PH be: 4.0, and be heated to 90 ℃, make the L-glutamic acid dissolving, be cooled fast to 8 ℃ with frozen water then, L-glutamic acid is separated out with the beta crystal crystallization; Vacuum filtration, vacuum tightness is :-0.09MPa obtains beta crystal L-glutamic acid 114 gram and mother liquor 240ml; Mother liquor is as the brilliant water of washing of next batch.
Embodiment two:
The present invention changes the following processing step of extraction technology of glutamic acid employing that brilliant coupled ion exchange is reclaimed:
Get 80m
3Glutami acid fermentation liquor, aminoglutaric acid concentration is: 11.5%, 37 ℃ of temperature, pH value is: 6.5.Sending into the quadruple effect evaporator system concentrates, concentrated condition is: first imitates well heater pressure: 0.09MPa, temperature: 85 ℃, second imitates well heater pressure :-0.04MPa, temperature: 75 ℃, triple effect well heater pressure :-0.08MPa, temperature: 65 ℃, quadruple effect well heater pressure :-0.094MPa, temperature: 50 ℃, 2.5 times of cycles of concentration, concentrated solution volume 32m
3Enter continuous isoelectric point crystallization workshop section, add sulfuric acid and before the batch operation hydrolyzed solution and the high stream of acidifying that obtain, ladder is transferred PH, gradient cooling simultaneously, recording the PH gradient with test paper is: 4.2～3.2, the temperature ladder is: 45～8 ℃, electric pH value such as promptly final is: 3.2, and temperature is: 8 ℃; After isoelectric point crystallization finishes, separate with horizontal spiral centrifuge, rotating speed is that per minute 6000 changes, and obtains 10.89t alpha-crystal form crude product L-glutamic acid; The 29m that tells
3Send into the air supporting machine of tropina abstraction process Deng electric mother liquor, add 0.45m simultaneously
31# flocculant solution, 0.15m
3The 2# flocculant solution, discharge the wet thallus albumen 1.76t of air supporting flocculation from air supporting machine separator top; Discharge 27.4m from air supporting machine separator bottom
3Clear mother liquor adds sulfuric acid and transfers pH value 1.5-1.7 (test paper survey), sends into and exchanges absorption in the ion exchange column, adds the collection of 10% ammoniacal liquor wash-out and obtains 6.8m
3The recovery liquid that contains L-glutamic acid 8.4% adds sulfuric acid and recalls to receipts liquid PH to 1.5, obtains 7.2m
3The high stream of acidifying is delivered to continuous isoelectric point crystallization workshop section and is added acid and use.
Alpha-crystal form crude product L-glutamic acid is sent into and is washed brilliant jar, sends into horizontal spiral centrifuge after adding 19.6t water or changeing brilliant mother liquor mixing and carries out secondary separation, obtains 9.96 tons of alpha-crystal form L-glutamic acid and 20.5m
3The secondary separation mother liquor.
Alpha-crystal form elaboration L-glutamic acid is sent into to be changeed in brilliant jar, adds 22m
3Tap water, the liquid caustic soda with content 30% transfers to PH4.2 simultaneously, is heated to 87～90 ℃ while stirring, and L-glutamic acid is fully dissolved, and pumps into the crystallisation by cooling jar then, with water quench to 12 ℃, separates out beta crystal L-glutamic acid.Crystal solution flows into belt vacuum filter from the crystallisation by cooling jar, and control vacuum tightness per hour adds 2～3t wash water about-0.085MPa, filters to obtain 10.5 tons in beta crystal L-glutamic acid and change brilliant mother liquor.Change brilliant mother liquor loopback and wash brilliant operation, use as wash water.
Wash the brilliant isolated 20.5m in back
3The secondary separation mother liquor send quadruple effect evaporator to concentrate, and operational condition is the same, and final concentrated solution volume is 4.1m
3, pump delivery is to 10m
3Hydrolytic decomposition pot adds 2 tons of concentration and is 92% the vitriol oil, is heated to 145 ℃ of hydrolysis 1 hour, adds cover with water coolant then and is cooled to 55 ℃, pumps into flame filter press and filters, and obtains hydrolyzed solution 4.8m
3With 1 ton of filtration slag, hydrolyzed solution returns next batch isoelectric point crystallization operation and transfers pH value to use.
Ion exchange column is discharged 30m
3Adsorption tail liquid, regulate pH value 4.0 with liquefied ammonia, again through the quadruple effect evaporator Concentrated and crystallized in vacuum, operational condition is the same, 2.5 times of cycles of concentration, obtain 5.2 tons of ammonium sulfate crystallizations and separate 4.2 tons in mother liquor, separate mother liquor and further concentrate and obtain 1.4 tons of dry matter contents at 50% concentrated last mother liquor, the last mother liquor mixes employing dry method composting and makes 14 tons of biological fermentation fertilizer with ammonium sulfate, composting auxiliary material, secondary separation mother liquor hydrolysed filtrate slag.
Claims (1)
1, a kind of extraction technology of glutamic acid that changes brilliant coupled ion exchange recovery, adopt following processing step:
(1), adopt starchy material such as corn, rice, wheat or molasses raw materials such as sugarcane, beet to obtain by fermentation to contain that concentration is 9～16%, pH value is the fermented liquid of 6.3～6.7 L-glutamic acid;
(2), fermented liquid concentrates through heating evaporation, evaporator pressure :-0.01-0.1MPa, temperature 40-95 ℃, the liquid volume ratio is 2～5: 1 before and after the evaporation of glutami acid fermentation liquor;
(3), evaporation concentration secondary fermentation liquid is cooled to 25～50 ℃, enters continuous isoelectric point crystallization device, transfers PH to 3.0-3.2 with hydrolyzed solution or concentration greater than 90% sulfuric acid and the high stream of acidifying, is cooled to 5～15 ℃ again, and L-glutamic acid is separated out with the crystallization of α type;
(4), crystallization feed liquid through separate, wash crystalline substance, secondary separation obtains α type glutamic acid crystal and separates mother liquor and secondary separation mother liquor with an inferior electricity;
(5), in α type L-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, with concentration is that 15～35% yellow soda ash or sodium hydroxide lye are adjusted the solution pH value: 4.0～6.0, temperature is heated to 70～90 ℃, make the dissolving of alpha-crystal form L-glutamic acid, cool fast then to 5～30 ℃, L-glutamic acid is separated out with the beta crystal crystallization, be referred to as to change brilliant;
(6), changeing brilliant back feed liquid obtains the beta crystal glutamic acid crystallization through separation, the brilliant mother liquor of discharge commentaries on classics simultaneously; Change brilliant mother liquor as washing brilliant water reuse;
(7), the secondary mother liquid heating evaporation of secondary separation is concentrated, control evaporator pressure :-0.01-0.1MPa, temperature 40-95 ℃, the liquid volume ratio is before and after the evaporation of secondary mother liquid: 2～8: 1
(8), secondary mother liquid concentrates the back and adds sulphuric acid hydrolysis, adds the sulfuric acid quality and be 0.2～1 times of concentrated solution quality, hydrolysis temperature is: 80-150 ℃, hydrolysis time is: 1～5 hour;
(9), after hydrolysis finishes, separate obtaining hydrolyzed solution and the solid filter residue is a soil ulmin, hydrolyzed solution returns continuous isoelectric point crystallization, and solid filter residue main component is a protein, can be used as the raw material of system biological fermentation fertilizer.
(10), an inferior electric mother liquor adopts the molten gas of nature and evenly dissolves in the flocculation agent method, dissolved air flotation obtains tropina and Deproteinization mother liquor;
(11), the Deproteinization mother liquor adopts ion-exchange process for recovering glutamic acid, after the L-glutamic acid of recovery adds sulfuric acid acidation, get back to the continuous crystallisation jar and do isoelectric point crystallization with acid.The tail washings that the Deproteinization mother liquor is discharged behind ion-exchange absorption L-glutamic acid, concentrate through multiple-effect evaporator, ammonium sulfate crystallization is separated out, the ammonium sulfate crystallization mother liquor concentrates through multiple-effect evaporation again, obtain dry matter content at 45～50% last mother liquor, the last mother liquor mixes employing dry method composting with ammonium sulfate, composting auxiliary material, secondary separation mother liquor hydrolysed filtrate slag, make biological fermentation fertilizer.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102126975A (en) * | 2010-12-29 | 2011-07-20 | 菱花集团有限公司 | Method and device for producing glutamic acid |
| CN103395914A (en) * | 2013-08-13 | 2013-11-20 | 宝鸡阜丰生物科技有限公司 | Recycling method of glutamic acid crystalloblastic mother liquor |
| CN104230444A (en) * | 2014-10-08 | 2014-12-24 | 内蒙古阜丰生物科技有限公司 | Method for preparing fertilizers with sodium glutamate production waste |
| CN104262014A (en) * | 2014-10-07 | 2015-01-07 | 内蒙古阜丰生物科技有限公司 | Biological bacterial fertilizer prepared from glutamic acid fermentation wastes |
| CN104256056A (en) * | 2014-10-14 | 2015-01-07 | 内蒙古阜丰生物科技有限公司 | Animal feed prepared by glutamic acid fermentation waste |
| CN112521291A (en) * | 2020-12-15 | 2021-03-19 | 梁山菱花生物科技有限公司 | Glutamic acid crystal transformation method for shortening crystal transformation time |
| 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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2009
- 2009-07-23 CN CN200910012705A patent/CN101671705A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102126975A (en) * | 2010-12-29 | 2011-07-20 | 菱花集团有限公司 | Method and device for producing glutamic acid |
| CN103395914A (en) * | 2013-08-13 | 2013-11-20 | 宝鸡阜丰生物科技有限公司 | Recycling method of glutamic acid crystalloblastic mother liquor |
| CN103395914B (en) * | 2013-08-13 | 2015-04-08 | 宝鸡阜丰生物科技有限公司 | Recycling method of glutamic acid crystalloblastic mother liquor |
| CN104262014A (en) * | 2014-10-07 | 2015-01-07 | 内蒙古阜丰生物科技有限公司 | Biological bacterial fertilizer prepared from glutamic acid fermentation wastes |
| 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 |
| CN104230444A (en) * | 2014-10-08 | 2014-12-24 | 内蒙古阜丰生物科技有限公司 | Method for preparing fertilizers with sodium glutamate production waste |
| CN104230444B (en) * | 2014-10-08 | 2016-08-24 | 内蒙古阜丰生物科技有限公司 | A kind of method utilizing sodium glutamate production waste material to prepare fertilizer |
| CN104256056A (en) * | 2014-10-14 | 2015-01-07 | 内蒙古阜丰生物科技有限公司 | Animal feed prepared by glutamic acid fermentation waste |
| CN112521291A (en) * | 2020-12-15 | 2021-03-19 | 梁山菱花生物科技有限公司 | Glutamic acid crystal transformation method for shortening crystal transformation time |
| 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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