CN101402584A - Method for separating and extracting L-glutamic acid from fermentation liquor - Google Patents
Method for separating and extracting L-glutamic acid from fermentation liquor Download PDFInfo
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- CN101402584A CN101402584A CNA2008101528847A CN200810152884A CN101402584A CN 101402584 A CN101402584 A CN 101402584A CN A2008101528847 A CNA2008101528847 A CN A2008101528847A CN 200810152884 A CN200810152884 A CN 200810152884A CN 101402584 A CN101402584 A CN 101402584A
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- glutamic acid
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Abstract
The invention relates to a method for extracting and refining glutamic acid from fermentation liquor by combining a metallic membrane separating technique and a concentrating continuous equal point method, and mainly solves the problems of low product purity and extraction yield, high cost and serious waste liquid pollution in the prior separating and extracting method. The method comprises the operation steps of filtering by a metallic membrane, decoloring by active carbon, crystallizing, and the like for the glutamic acid fermentation liquor; and the mother liquor in each step can be recycled. The method produces little waste liquor and reduces environmental pollution. The glutamic acid is separated and extracted to obtain refined glutamic acid crystal, wherein the extraction yield of the glutamic acid is larger than 96 percent and the purity can reach more than 98 percent. The method adopts the metallic membrane to filter germs, changes the prior methods of centrifugation, flocculence, heating adopted by treating the fermentation liquor, reduces the extraction cost of the glutamic acid greatly, removes the germs thoroughly, and has clear and transparent filter liquor; in addition, the stainless steel membrane adopted by the method has the characteristics of stable quality of the filter liquor, long service life, high temperature resistance, acid and alkali resistance, wide passage, easy cleaning, convenience for maintaining equipment, and the like.
Description
[technical field]:
Originally relate to a kind of extracting glutamic acid novel process in fermentative Production L-glutamic acid process, belong to technical field of producing amino acid by fermentation.
[background technology]:
At present, domestic monosodium glutamate industry is used corn, rice, molasses, beet etc. always and is adopted fermentative Production L-glutamic acid for raw material, and L-glutamic acid is mainly used in produces monosodium glutamate (Sodium Glutamate).Be impurity such as tropina, residual sugar in the separate fermentation liquid, electric sedimentation and ion exchange phase bonded methods such as common employing, the COD that it produced, sulfate radical, NH
3The hc effluent of-N (ammonia nitrogen), difficulty of governance is big, and contaminate environment is serious, has restricted China's monosodium glutamate industry and L-glutamic acid production and has entered benign Sustainable development track.For this reason, domestic many enterprises and scientific research institution have taked some clean preparation methods, separate with feed liquid as thalline, reclaim tropina, not only can simplify subsequent treatment process, but also can alleviate enterprise's sewage disposal burden.The main method of separating thallus, residual sugar impurity has centrifuging, flocculence heating method, membrane separation process (ultrafiltration and micro-filtration) etc. at present, takes all factors into consideration with membrane separation process the most advanced.
In addition, the subject matter of domestic present stage monosodium glutamate industry is the yield and the purity of L-glutamic acid, and two indexs all are lower than foreign level.It is reported that the L-glutamic acid proportion that present most of Gourmet Powder Factories run off from mother liquor in actual production process is bigger, and crystal formation is relatively poor, crystallization time is long, the cost height, and the difficulty of control and operation is big.
[summary of the invention]:
Main purpose of the present invention is to solve the problem that waste liquor contamination is serious, product purity is not high and yield is low in the existing separating and extracting method of L-glutamic acid, provides a kind of and utilizes the metallic membrane isolation technique and separation and Extraction from fermented liquid that the method for selecting combines such as concentrate continuously and the method for refining L-glutamic acid.
The method of from the fermented liquid of fermentative Production L-glutamic acid, extracting refining L-glutamic acid provided by the invention, its concrete extraction step is as follows:
A, glutami acid fermentation liquor is put into the metal microfiltration membrane system carry out micro-filtration, remove tropina impurity, obtain clarifying glutami acid fermentation liquor; Described mineral membrane adopts stainless steel tubular type film separating system, and its aperture is 50nm～100nm, molecular weight cut-off 2000～50000MW, and pH scope 0～14, service temperature are 0～80 ℃, operation pressure reduction is 0.1～1.0Mpa;
B, will go up the step and obtain clarifying glutami acid fermentation liquor to adjust pH be 4.0～7.0, and add active carbon powder and decolour, the gac add-on is 0.1～0.5% of a fermentating liquid volume, and bleaching temperature is 20～80 ℃, and the time is 20～40min; Using 752 spectrophotometers to survey printing opacity down in 430nm reaches more than 90%;
C, with 1/4～1/3 fermented liquid as bed material, separate liquid with sulfuric acid/water and regulate pH value to 4.5～4.0 o'clock, add α-type L-glutamic acid crystal seed of 0.2%～0.3%, stir, educated brilliant 1～2 hour, add slowly sourer to the pH value be 3.0～3.2, as seed liquor; All the other glutami acid fermentation liquors are carried out reduction vaporization, concentrate the 1/5-1/2 of volume to stoste.Then, with the glutami acid fermentation liquor after concentrating and sulfuric acid/water separate liquid simultaneously stream add, keep pH value constant, temperature is controlled between 15～25 ℃, emits crystalline L-glutamic acid simultaneously, makes turnover feed liquid maintenance balance, the material of emitting carries out low temperature (4 ℃) and educates crystalline substance.
D, filtration, washing obtain glutamic acid crystal and mother liquor, and the glutamic acid crystal that this method obtains mainly is α-type glutamic acid crystal, and purity and yield are all higher.Mother liquor is squeezed into fermented liquid, enter metallic membrane and carry out micro-filtration, recycle.
E, impurity such as albumen and pigment can decolour again or directly carries out metal membrane filter more for a long time in glutamic acid mother liquor.
Above-mentioned b is in the step, and pH the best was 5.0～6.0 when clarifying glutami acid fermentation liquor decoloured, and temperature is 40～60 ℃.
Method according to claim 1 and 2 is characterized in that obtaining purified L-glutamic acid, and purity reaches more than 99%, and yield is more than 96%.
Advantage of the present invention and positively effect:
Compare with existing technology, method of the present invention has following characteristics:
1, the stainless steel membrane that adopts of the present invention has filtrate steady quality, long service life, filtrate precision height, high temperature resistant, acid and alkali-resistance, fat pipe, is easy to clean and characteristics such as convenience for device maintenance, is fit to scale operation;
2, the present invention adopts the stainless steel membrane filtration thalline, has changed methods such as centrifuging that conventional fermentation liquor treatment adopts, heating method, flocculence, has reduced the extraction cost of L-glutamic acid widely, and it is more thorough to remove thalline, the liquid clear after the filtration;
3, the glutamic acid solution quality after the present invention makes with extra care significantly improves, wait the L-glutamic acid product that obtains after the electrical method extraction can reach more than 99% continuously through concentrating through the amino acidanalyser purity assay, avoid the brilliant process of the commentaries on classics in the traditional technology, improved the extract yield of L-glutamic acid widely;
4, common production technique often adopts resin to reclaim L-glutamic acid in the mother liquor, the main source of high concentrated organic wastewater be the fermented liquid isoelectric point crystallization after the thalline of resin discharging and a large amount of rinsing waters are seriously polluted, administers very difficult, the consumption substantial contribution.The present invention utilizes the metallic membrane isolation technique that fermented liquid is carried out pre-treatment, efficiently solves the high concentrated organic wastewater pollution problems.
[embodiment]:
Embodiment 1:
A, get glutami acid fermentation liquor 30L, the pH value is about 6.5, add metallic membrane microfiltration equipment batch can in batches, start microfiltration equipment, 20～60 ℃ of controlled temperature, regulating the film inlet outlet pressure differential is 0.8～1MPa, utilize the difference of microfiltration membrane to differing molecular quantity of material interception capacity, thalline, foreign protein are trapped in the filter residue, when turnover mould difference obviously reduces, mend suitable quantity of water.After filtering end, obtain L-glutamic acid filtrate 40L, the filtrate thallus removing rate is 99.6%, and the albumen clearance is 87.2%, and rate of loss is lower than 1%.
B, will go up the step and obtain clarifying glutami acid fermentation liquor to adjust pH be 5.0, and add gac and decolour, the gac add-on is 0.2% of a fermentating liquid volume, and bleaching temperature is 50 ℃, and bleaching time is 30min.Fermented liquid after the decolouring is surveyed transmittance with 752 spectrophotometers down in 430nm and is reached 91.6%;
C, with the 8L fermented liquid as bed material, when regulating pH value to 4.2, add α-type L-glutamic acid crystal seed of 0.2% with the vitriol oil, fully stir, educated brilliant 2 hours, add slowly sourer to the pH value be 3.2, as seed liquor; All the other glutami acid fermentation liquors are carried out reduction vaporization, concentrate volume to about 1/3 of stoste.
D, the glutami acid fermentation liquor after will concentrating and sulfuric acid/water separate liquid simultaneously stream add, it is 3.2 constant keeping the pH value, and temperature is controlled between 15～20 ℃, and making simultaneously, crystalline L-glutamic acid flows out from the bottom, keep turnover feed liquid balance, the low-temperature material of emitting (4 ℃) is educated crystalline substance.
E, filtration, washing obtain glutamic acid crystal and mother liquor, and what obtain mainly is α-type glutamic acid crystal, and purity is 99.2%, and the total recovery of L-glutamic acid is 96.8%.
Embodiment 2:
A, to get pH be 6.5 glutami acid fermentation liquor 40L, add the microfiltration equipment batch can in batches, start microfiltration equipment, 20～60 ℃ of controlled temperature, regulating film inlet and outlet pressure difference is 0.8～1.0MPa, utilize the difference of microfiltration membrane to the material interception capacity of different molecular weight, thalline, foreign protein are trapped in the filter residue, when turnover mould difference obviously reduces, mend suitable quantity of water, obtain thallus removing rate up to 99.9% L-glutamic acid filtrate 50L, the albumen clearance is 88.6%.
B, will go up the step and obtain clarifying glutami acid fermentation liquor to adjust pH be 5.5, and add gac and decolour, the gac add-on is 0.3% of a fermentating liquid volume, and bleaching temperature is 55 ℃, decolouring 40min; Use 752 spectrophotometers to survey transmittance down and reach 92.5% in 430nm;
C, with the 10L fermented liquid as bed material, when regulating pH value to 4.0, add α-type L-glutamic acid crystal seed of 0.3% with the vitriol oil, fully stir, educated brilliant 2 hours, add slowly sourer to the pH value be 3.2, as seed liquor; All the other glutami acid fermentation liquors are carried out reduction vaporization, concentrate volume to about 1/4 of stoste.
D, the glutami acid fermentation liquor after will concentrating and sulfuric acid stream simultaneously add, and it is 3.2 constant keeping pH value, and temperature is controlled between 15～20 ℃, make simultaneously that crystalline L-glutamic acid flows out from the bottom, keep passing in and out the feed liquid balance, and the low-temperature material of emitting (4 ℃) is educated crystalline substance.
E, filtration, washing obtain glutamic acid crystal and mother liquor, and what obtain mainly is α-type glutamic acid crystal, and purity is 99.7%, and the total recovery of L-glutamic acid is 96.6%.
Embodiment 3:
Utilize metal membrane filter to extract L-glutamic acid under the different turnover mould differences
Membrane filtration is held back particulate and macromolecular substance greater than the filter membrane micropore by sieving action, can guarantee quantitatively to hold back, and membrane filtration divides static filtering and cross flow filter.The mode of metal membrane filter is a cross flow filter, cross flow filter can filter the higher liquid of turbidity, its mode of action is, liquid flows through the film surface with tangential direction, the shearing force that produces during through the film surface can make the muddy particle that is deposited on the film surface spread back main body stream, thereby make the film surface contamination layer remain on thin maintenance level, prevent quick obstruction.The variation of pressure can have influence on the thickness of film surface contamination layer, so influential to filtering speed etc. in filtration procedure.During to the influencing of metal membrane filter result, because main difference is to pass in and out the pressure reduction of film, and the resistance to pressure of metallic membrane is good especially, so can bear bigger pressure and pressure reduction in filtration procedure at research pressure.When system temperature is 30 ℃, compared the not effect of damming of film when 1.0Mpa and 0.6Mpa of turnover mould difference, the result is as shown in table 1.
The filter result of paddy ammonia enzymic fermentation liquid under the different pressure reduction of table 1
Embodiment 4
Utilize metal membrane filter to extract L-glutamic acid under the differing temps
Temperature is to cause the increase of feed liquid viscosity degradation and spread coefficient because temperature raises to the influence of membrane flux, and film surface flow speed increases, and film surface shear power increases, and makes the filtering layer attenuation, thereby filtering rate increases.But too high temperature can cause the fermented liquid colour-darkening, and this may be because due to compositions such as residual sugar, protein colloid material at high temperature react in the fermented liquid, thereby influences follow-up extraction operation.Studied of the influence of different filtration temperatures, and measured the extract yield of gained glutami acid fermentation liquor under the different filtration temperatures, the results are shown in Table 2 the filter effect of glutami acid fermentation liquor.
The filter result of glutami acid fermentation liquor under table 2 differing temps
Claims (4)
1, a kind of method of extracting L-glutamic acid from the fermented liquid of fermentative Production L-glutamic acid is characterized in that the concrete extraction step of this method is as follows:
A, glutami acid fermentation liquor is entered metallic membrane carry out micro-filtration, remove impurity such as tropina, obtain clarifying glutami acid fermentation liquor and thalline concentrated solution, the thalline concentrated solution continues to filter after can adding suitable quantity of water, also can sneak in the fermented liquid to recycle; Described metallic membrane adopts stainless steel tubular type film separating system, and its aperture is 50nm～100nm, molecular weight cut-off 2000～50000MW, and pH scope 0～14, service temperature are 0～80 ℃, operation pressure reduction is 0.1～1.0Mpa.
B, to regulate glutami acid fermentation liquor pH with the vitriol oil be 4.0～7.0, and the gac add-on is that 0.1～0.5% of fermentating liquid volume decolours, and temperature is 20～80 ℃, and the time is 20～40min.
C, with 1/4～1/3 fermented liquid as bed material, separate liquid with sulfuric acid/water and regulate pH value to 4.5～4.0 o'clock, add α-type L-glutamic acid crystal seed of 0.2%～0.3%, stir, educated brilliant 1～2 hour, add sour more slowly to pH 3.0～3.2, as seed liquor; All the other glutami acid fermentation liquors are carried out reduction vaporization, concentrate the 1/5-1/2 of volume to stoste.Then, the glutami acid fermentation liquor after concentrating and sulfuric acid (or hydrolyzed solution) are carried out stream simultaneously add, keep pH value (3.0～3.2), temperature is controlled between 15～25 ℃, emit crystalline L-glutamic acid simultaneously, make the turnover feed liquid keep balance, the low-temperature material of emitting (4 ℃) is educated crystalline substance.
D, filtration, washing obtain glutamic acid crystal and mother liquor, and the glutamic acid crystal that this method obtains mainly is α-type glutamic acid crystal, and yield is higher.Mother liquor is squeezed into fermented liquid, enter metallic membrane and carry out micro-filtration, recycle.
E, impurity such as albumen and pigment can decolour again or directly carries out metal membrane filter more for a long time in glutamic acid mother liquor.
2, method according to claim 1 is characterized in that above-mentioned b in the step, and best pH was 5.0～6.0 when clarifying glutami acid fermentation liquor decoloured, and temperature is 40～60 ℃.
3, method according to claim 1 is characterized in that the mother liquor that above-mentioned d obtained in the step repeats a or b step, guarantees the purity of L-glutamic acid product, and purity can reach more than 99%.
4, method according to claim 1 is characterized in that mother liquor that above-mentioned d obtained in the step repeats the step of a, saves the usage quantity of acid, improves yield, and yield reaches more than 96%.
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| CNA2008101528847A CN101402584A (en) | 2008-11-07 | 2008-11-07 | Method for separating and extracting L-glutamic acid from fermentation liquor |
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| CNA2008101528847A CN101402584A (en) | 2008-11-07 | 2008-11-07 | Method for separating and extracting L-glutamic acid from fermentation liquor |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102001972A (en) * | 2010-10-26 | 2011-04-06 | 广东肇庆星湖生物科技股份有限公司 | Method for separating and extracting L-arginine from fermentation liquor |
| CN103980137A (en) * | 2014-05-30 | 2014-08-13 | 上海沃凯生物技术有限公司 | Post-treatment method of L-glutamic acid fermentation liquid |
| CN104473120A (en) * | 2014-12-31 | 2015-04-01 | 广州双桥股份有限公司 | Monosodium glutamate production technology |
-
2008
- 2008-11-07 CN CNA2008101528847A patent/CN101402584A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102001972A (en) * | 2010-10-26 | 2011-04-06 | 广东肇庆星湖生物科技股份有限公司 | Method for separating and extracting L-arginine from fermentation liquor |
| CN103980137A (en) * | 2014-05-30 | 2014-08-13 | 上海沃凯生物技术有限公司 | Post-treatment method of L-glutamic acid fermentation liquid |
| CN104473120A (en) * | 2014-12-31 | 2015-04-01 | 广州双桥股份有限公司 | Monosodium glutamate production technology |
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Open date: 20090408 |