CN102757354A - Method for extracting and separating L-leucine by using combined technology of membrane separation and electrodialysis - Google Patents
Method for extracting and separating L-leucine by using combined technology of membrane separation and electrodialysis Download PDFInfo
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Abstract
The invention discloses a method for extracting and separating L-leucine by using a combined technology of membrane separation and electrodialysis, and belongs to the technical field of biochemical engineering. The invention comprises the following steps: (1) removing thallus from fermentation liquid; (2) removing inorganic salt through electrodialysis; (3) removing inorganic salt clear liquid and small-molecule impurities; and (4) concentrating and crystallizing the fermentation liquid. The method has the advantages that the condition is mild, the operation is simple and convenient, the separation steps are less, the selectivity is good, and the production is clean, overcomes the defects of low yield, large sewage discharge amount and high production strength in the conventional ion exchange technology, and improves the yield and the quality of L-leucine remarkably.
Description
Technical field
The present invention relates to the leucic extraction and separation method of a kind of L-, relate in particular to a kind of method of utilizing membrane sepn and electrodialysis combination technique from L-leucine fermented liquid, to remove the separation and Extraction of inorganic salt, belong to technical field of biochemical industry.
Background technology
The L-leucine is the necessary amino acid of human body as one of branched-chain amino acid, has different physiological roles.Because of its particular structural and function, in human life's metabolism, occupy an important position, mainly in order to the transfusion of preparation aminoacids complex, synthetic polypeptide medicaments and food antioxidant etc., the especially effect in medical research and treatment comes into one's own day by day.It is in the treatment of hemato encephalic barrier, hepatic coma, chronic liver cirrhosis and renal failure; The dietary therapy that inborn errors of metabolism is sick; The surgical wound healing is accelerated in septicemia and postoperative diabetic subject's treatment, is widely used in the nutritional support treatment of tumour patient.Therefore, have application and commercial value widely at medicine and food service industry.
Having advantages such as raw materials cost is low, reaction conditions is gentle, easy realization of large-scale production with producing L-leucine by fermentation, is to produce the topmost method of L-leucine at present.
Amino acid zymotic fluid is that substratum produces through liquid fermenting, comprising product, sub product, and materials such as substratum residue, thalline.The separation of tunning occupies critical positions aborning with extraction, will from product, remove thalline, colloidal suspended substance, inorganic salt in the amino acid zymotic fluid in the production.At present, the leucic extraction traditional production process of L-generally adopts ion exchange process, removes the inorganic salt in the fermented liquid through the IX means.The general process of this technology is: filtering fermentation liquor is removed thalline, IX through absorb-elute process amino acid separation; Adopt this technology separation and Extraction L-leucine from fermented liquid to have following problem: the one, adopt filtering method to remove thalline; Because thalline is tiny, thalline is removed not thorough usually; The 2nd, L-leucine fermented liquid colour is than higher, and common activated carbon decolorizing is incomplete and consumption is big, influences quality product and yield; The 3rd, impurity component is many in the L-leucine fermented liquid, content is high; Directly use ion exchange method to handle, resin stain is serious, causes that easily resin structure breaks ring and loses regenerative power; Increased running cost; High-load ionic substance can make resin saturated fast simultaneously, increases the resin regeneration number of times, causes problems such as quantity of wastewater effluent is big.
Above-mentioned L-leucine extraction process is to set up the 1980s.Along with the progress of biochemical stripping technique, various advanced persons' separating device and technology are played a greater and greater role aborning, and particularly the development and the application of membrane separation technique and electrodialysis desalination technology are greatly taken on a new look various biochemical separating technologies.Membrane separation technique is used for the existing successful precedent of separation and purification of leavened prod, but utilizes membrane sepn and electrodialysis combination technique separation and Extraction L-leucine from fermented liquid, does not also appear in the newspapers.
Electrodialysis electricity drive membrane separator is that a kind of selection perviousness of utilizing film is separated the material in the water and reached desalination, a kind of membrane separation plant of intended purposes such as concentrates.The major parts of electrodialyzer is yin, yang ion-exchange membrane, dividing plate and electrode three parts.The compartment that dividing plate constitutes is the passage that liquid flow is crossed process.The compartment of material process is a desalting chamber, and the compartment of dense water process is the concentration compartments.Under the effect of DC electric field, utilize the selection perviousness of ion-exchange membrane, the cation permeation anode membrane, negatively charged ion sees through cavity block, and the ion of desalting chamber moves to the concentration compartments, and the ion of concentration compartments can't move to desalting chamber owing to the selection perviousness of film.The ionic concn of light like this chamber reduces gradually, and the ionic concn of corresponding dense chamber is corresponding to raise gradually, promptly removes the salinity of material, reaches and separates spissated purpose.The dense chamber solution that is wherein obtained by electrodialysis can be used for the fermention medium inorganic salt and recycles, and has practiced thrift starting material.
Process explanation: amino acid zymotic fluid through the freshwater room desalination of electrodialysis electricity drive membrane, is purified solution through being adjusted to iso-electric point then.Solution is sent into the electrodialysis electricity drive membrane separator that ionic membrane is formed through feedstock pump, orientation movement under the effect of direct current field force, and positively charged ion moves down to negative electrode, moves under the negatively charged ion anode.Solution moves away charged ion such as sodium ion, cl ions respectively under DC electric field, and former L-leucine fermented liquid specific conductivity 15000～50000 μ S/cm regulate pH:5.0～7.5,10-40 ℃.Below the specific conductivity 1000 μ S/cm of desalination clear liquid, rate of loss is about below 5% after electrodialysis electricity drive membrane is handled.
Summary of the invention
Deficiency to existing ion exchange technique; The problem that the present invention will solve provides a kind of membrane sepn and electrodialysis combination technique leucic method of desalination separation and Extraction L-from fermented liquid of utilizing; This method has mild condition, easy and simple to handle, separating step is few, selectivity is good characteristics; The yield that has overcome the prior art existence is not high, sewage flow rate reaches the big shortcoming of production intensity greatly, and leucic yield of L-and quality are significantly improved.
Membrane sepn and the electrodialysis combination technique leucic basic step of separation and Extraction L-from fermented liquid of utilizing provided by the invention is: at first with the ultra-filtration membrane of fermented liquid through molecular weight cut-off 100,000-1,000,000; Thoroughly remove the thalline in the fermented liquid, obtain L-leucine fermentation clear liquid.The fermentation clear liquid that obtains uses molecular weight to remove pigment and small molecular weight impurity as the nf membrane of 100-3000 through continuous electric dialysis device separates inorganic salt again.The flaxen L-leucine solution of the clarification that obtains because its solubleness is lower, directly concentrates, step such as crystallization makes bullion, and bullion obtains highly purified L-leucine product after making with extra care.
Technical scheme of the present invention: a kind of membrane sepn and electrodialysis desalination combination technique leucic method of separation and Extraction L-from fermented liquid of utilizing, specifically form by following steps:
(1) fermented liquid removes thalline: L-leucine fermented liquid through molecular weight cut-off 100,000-1,000,000 ultra-filtration membrane, is thoroughly removed the thalline in the fermented liquid, obtain L-leucine fermentation clear liquid.Working pressure is 0.15-0.8MPa, and service temperature is 10-60 ℃, and the dialysis water yield accounts for the 10%-90% of fermented liquid feed volume in volume percent;
(2) electrodialysis desalination: with the L-leucine fermentation clear liquid that step (1) obtains, its specific conductivity 15000～50000 μ S/cm are adjusted to isoelectric pH 5.0～7.5, through the light chamber desalination of electrodialysis electricity drive membrane, make solution obtain purifying then.Service temperature is 10-40 ℃, dense chamber amount of water 0.5-4 times fermentation clear liquid material liquid volume, and light chamber specific conductivity and dense chamber keep specific conductivity less than 20 times; Solution is sent into the electrodialysis electricity drive membrane separator that ionic membrane is formed through feedstock pump, orientation movement under the effect of direct current field force, and positively charged ion moves down to negative electrode, moves under the negatively charged ion anode.Solution is gone out charged particles ion migration such as inorganic salt respectively under DC electric field, when liquid stock desalination rate greater than 90%, can get into subsequent processing.The dense chamber salt solution that is wherein obtained by electrodialysis can be used for the fermention medium inorganic salt and recycles.
Former L-leucine fermented liquid specific conductivity 15000～50000 μ S/cm, normal temperature.Below the specific conductivity 1000 μ S/cm of desalination clear liquid, rate of loss is below 5% after electrodialysis electricity drive membrane is handled.
(3) the desalination clear liquid removes impurity and pigments such as small molecular protein: the L-leucine desalination clear liquid that step (2) is obtained uses molecular weight cut-off to remove impurity such as pigment and small molecular protein as the nf membrane of 100-3000, obtains clarifying colourless L-leucine solution.Working pressure is 0.5-3.0MPa, and service temperature is 10-60 ℃, and the dialysis water yield accounts for the 10%-90% of desalination clear liquid feed volume with volume percent;
(4) concentrate, crystallization: with step (3) obtain clarifying colourless L-leucine solution with ordinary method concentrate, crystallization obtains L-leucine bullion, again bullion obtained highly purified L-leucine product after making with extra care.
The described filter membrane of above-mentioned steps (1) aperture is preferably molecular weight cut-off 300,000-800,000, the preferred 0.3-0.5MPa of working pressure, and the preferred 20-30 of service temperature ℃, the dialysis water yield accounts for the 10%-90% of fermented liquid feed volume in volume percent.
The described electrodialysis electricity of above-mentioned steps (2) drive membrane separator, the preferred 20-40 of service temperature ℃, dense chamber amount of water 0.5-2 times fermentation clear liquid material liquid volume, light chamber specific conductivity and dense chamber keep specific conductivity less than 20 times; Below the specific conductivity 1000 μ S/cm of desalination clear liquid, rate of loss is below 5% after electrodialysis electricity drive membrane is handled.
The preferred 300-1000 of the described nf membrane molecular weight of above-mentioned steps (3), the preferred 0.5-2.5MPa of working pressure, the preferred 20-40 of service temperature ℃, the dialysis water yield accounts for the 10%-50% of desalination clear liquid feed volume in volume percent.
Beneficial effect of the present invention: the leucic method of desalination separation and Extraction L-from fermented liquid that the present invention relates to; First electrodialytic technique is introduced the separation and Extraction of producing L-leucine by fermentation; And set up one according to the size-grade distribution of impurity in the fermented liquid and overlapped multistage continuous electrodialysis desalination system; The yield that has overcome the prior art existence is not high, quantity of wastewater effluent reaches the high defective of production intensity greatly, and leucic yield of L-and quality are significantly improved, and production cost reduces.
Compare with existing Technology, the meliority of utilizing method of the present invention to have is following:
1, the present invention adopts ultrafiltration membrance filter to remove the thalline in the fermented liquid, has changed the filtering method of conventional pressure filter.It is thorough to remove thalline through ultrafiltration membrance filter, crosses the cleaner liquid clear, and can remove high molecular weight protein, and bacteria-eliminating efficacy is much higher than filtration method.
2, the present invention adopts membrane separation technique that ionic impurity and pigment content in the L-leucine fermented liquid are reduced greatly, the feed liquid transmittance has improved, and has reduced the ion exchange liquid activated carbon decolorizing operation again after handing over.
3, the electrodialysis desalination technology has substituted the traditional processing technology of IX, and the process water amount compares:
The maximum water consumption of electrodialysis is mainly the required diluting water in dense chamber, is at most 4 times of feed liquid water.The IX water is the great amount of wastewater that ion exchange regenerant, elution process form, and accounts for 10 times of material liquid volumes.
The dense chamber salt solution that obtains through electrodialysis process simultaneously is back to use fermented liquid and is used as the inorganic salt batching, and product gas purity obviously improves than the purity of conventional ion exchange extraction process.Therefore electrodialysis desalination technology has been brought into play the effect of cleaner production.
Description of drawings
Fig. 1 electrodialysis schematic diagram.
Embodiment
Embodiment 1
L-leucine fermented liquid 5.0L removes thalline through molecular weight cut-off 200,000 ultrafiltration membrance filters, working pressure 0.3MPa, and 30 ℃ of temperature, the dialysis water yield 1.5 L, filtrating is thoroughly removed thalline.Through the combined electrical dialyzer equipment of 6L, 30 ℃ of temperature obtain desalination L-leucine clear liquid then.The desalination clear liquid is that 500 nf membrane is filtered and removed small molecular weight impurity and pigment through molecular weight cut-off, working pressure 1.2MPa, and 30 ℃ of temperature, dialysis water yield 3.6L, and then obtain product with the method condensing crystal of routine.The result sees the following form 1:
Electrodialysis electricity drive membrane separator: stoste specific conductivity: 22400 μ S/cm
Desalination clear liquid specific conductivity: 500 μ S/cm
Ratio of desalinization: 97.8%
Table 1
| ? | T（640nm） | Volume (L) | L-leucine (g/L) | Yield (%) |
| Fermented liquid | 8.1 | 5.0 | 31.2 | 100 |
| Ultra-filtration membrane filtrating | 71.0 | 5.8 | 26.5 | 98.4 |
| Electrodialysis | 74.6 | 5.3 | 28.6 | 97.3 |
| The nanofiltration clear liquid | 99.5 | 7.0 | 21.4 | 96.1 |
| Total recovery | ? | ? | ? | 96.1 |
Embodiment 2
L-leucine fermented liquid 350L removes thalline through molecular weight cut-off 800,000 ultrafiltration membrance filters, working pressure 0.36 MPa, and 30 ℃ of temperature, dialysis water yield 120L, filtrating is thoroughly removed thalline.Through the combined electrical dialyzer equipment of 500L, 30 ℃ of temperature obtain desalination L-leucine clear liquid then.The desalination clear liquid is that 500 nf membrane is filtered and removed small molecular weight impurity and pigment through molecular weight cut-off, working pressure 1.2MPa, and 30 ℃ of temperature, dialysis water yield 240L, and then obtain product with the method condensing crystal of routine.The result sees the following form 2:
Electrodialysis electricity drive membrane separator: stoste specific conductivity: 22500 μ S/cm
Desalination clear liquid specific conductivity: 600 μ S/cm
Ratio of desalinization: 97.3%
Table 2
| ? | T（640nm） | Volume (L) | L-leucine (g/L) | Yield (%) |
| Fermented liquid | 9.1 | 350 | 32.5 | 100 |
| Ultra-filtration membrane filtrating | 75.2 | 410 | 27.3 | 98.4 |
| Electrodialysis | 78.6 | 392 | 28.3 | 97.6 |
| The nanofiltration clear liquid | 99.1 | 510 | 21.5 | 96.3 |
| Total recovery | ? | ? | ? | 96.3 |
Embodiment 3
L-leucine fermented liquid 4.5M
3Remove thalline through molecular weight cut-off 800,000 ultrafiltration membrance filters, working pressure 0.4MPa, 30 ℃ of temperature, the dialysis water yield 1.5 M
3Filtrating is thoroughly removed thalline, then through 8M
3Combined electrical dialyzer equipment, 30 ℃ of temperature obtain desalination L-leucine clear liquid.Desalination clear liquid process molecular weight cut-off is 1000 nf membrane filtration removal small molecular weight impurity and pigment, working pressure 1.2MPa, 30 ℃ of temperature, dialysis water yield 3.1M
3, and then obtain product with conventional method condensing crystal.The result sees the following form 3:
Electrodialysis electricity drive membrane separator: stoste specific conductivity: 22650 μ S/cm
Desalination clear liquid specific conductivity: 600 μ S/cm
Ratio of desalinization: 97.3%
Table 3
| ? | T（640nm） | Volume (M 3） | L-leucine (g/L) | Yield (%) |
| Fermented liquid | 9.0 | 4.5 | 32.3 | 100 |
| Ultra-filtration membrane filtrating | 74.8 | 5.7 | 25.0 | 98.2 |
| Electrodialysis | 79.3 | 5.3 | 26.8 | 97.8 |
| The nanofiltration clear liquid | 92.9 | 7.4 | 19.0 | 96.6 |
| Total recovery | ? | ? | ? | 96.6 |
Claims (4)
1. one kind is utilized membrane sepn and the electrodialysis combination technique leucic method of extraction separation L-from fermented liquid, it is characterized in that being made up of following steps:
(1) fermented liquid removes thalline: with the ultra-filtration membrane of L-leucine fermented liquid through molecular weight cut-off 100,000-1,000,000, thoroughly remove the thalline in the fermented liquid, obtain L-leucine fermentation clear liquid; Working pressure is 0.15-0.8MPa, and service temperature is 10-60 ℃, and the dialysis water yield accounts for the 10%-90% of fermented liquid feed volume in volume percent;
(2) electrodialysis desalination: the L-leucine fermentation clear liquid that step (1) is obtained; Its specific conductivity 15000～50000 μ S/cm; Be adjusted to isoelectric pH 5.0～7.5, cross electrodialysis electricity drive membrane feed liquid membrane separation apparatus device, service temperature is 10-40 ℃; Dense chamber amount of water 0.5-4 times fermentation clear liquid material liquid volume, light chamber specific conductivity and dense chamber keep specific conductivity less than 20 times; The specific conductivity of gained desalination clear liquid is that rate of loss is below 5% below the 1000 μ S/cm after electrodialysis electricity drive membrane is handled;
(3) the desalination clear liquid removes small molecular protein impurity and pigment: the inorganic salt clear liquid of removing that step (2) is obtained uses molecular weight cut-off to remove small molecular protein and pigment impurity as the nf membrane of 100-3000; Obtain clarifying colourless L-leucine solution; Working pressure is 0.5-3.0MPa; Service temperature is 10-60 ℃, and the dialysis water yield accounts for the 10%-90% of desalination clear liquid feed volume with volume percent;
(4) concentrate, crystallization: with step (3) obtain clarifying colourless L-leucine solution with ordinary method concentrate, crystallization obtains L-leucine bullion, again bullion obtained highly purified L-leucine product after making with extra care.
2. a kind of membrane sepn and electrodialysis combination technique leucic method of extraction separation L-from fermented liquid of utilizing as claimed in claim 1; It is characterized in that; The ultra-filtration membrane of the described molecular weight cut-off 300,000-800,000 of step (1); The preferred 0.3-0.5MPa of working pressure, the preferred 20-30 of service temperature ℃, the dialysis water yield accounts for the 10%-90% of fermented liquid feed volume in volume percent.
3. a kind of membrane sepn and electrodialysis combination technique leucic method of extraction separation L-from fermented liquid of utilizing as claimed in claim 1; It is characterized in that; The described electrodialysis electricity of step (2) drive membrane feed liquid membrane separation apparatus device, former L-leucine fermentation clear liquid specific conductivity 15000～50000 μ S/cm, pH:5.0～7.5; Cross electrodialysis electricity drive membrane feed liquid membrane separation apparatus device; The preferred 20-40 of service temperature ℃, preferred 0.5-2 times of fermentation clear liquid material liquid volume of dense chamber amount of water, light chamber specific conductivity and dense chamber keep specific conductivity less than 20 times; Below the specific conductivity 1000 μ S/cm of gained desalination clear liquid, rate of loss is below 5% after electrodialysis electricity drive membrane is handled.
4. a kind of membrane sepn and electrodialysis combination technique leucic method of extraction separation L-from fermented liquid of utilizing as claimed in claim 1; It is characterized in that; The preferred 300-1000 of the described nf membrane molecular weight cut-off of step (3); The preferred 0.5-2.5MPa of working pressure, the preferred 20-40 of service temperature ℃, the dialysis water yield accounts for the 10%-50% of desalination clear liquid feed volume in volume percent.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103951572A (en) * | 2014-04-21 | 2014-07-30 | 无锡晶海氨基酸有限公司 | Separation and purification process for producing branched chain amino acid by using fermentation method |
| CN111888940A (en) * | 2020-08-19 | 2020-11-06 | 自然资源部天津海水淡化与综合利用研究所 | Electrodialyzer with embedded ultrafiltration membrane |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1387458A (en) * | 1999-11-03 | 2002-12-25 | 巴斯福股份公司 | Method for Purification of Amino Acid-Containing Solutions by Electrodialysis |
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