CN102703537B - Novel production method for glutamic acid - Google Patents
Novel production method for glutamic acid Download PDFInfo
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- CN102703537B CN102703537B CN 201210211393 CN201210211393A CN102703537B CN 102703537 B CN102703537 B CN 102703537B CN 201210211393 CN201210211393 CN 201210211393 CN 201210211393 A CN201210211393 A CN 201210211393A CN 102703537 B CN102703537 B CN 102703537B
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- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 title claims abstract description 188
- 229960002989 Glutamic Acid Drugs 0.000 title claims abstract description 103
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 21
- 235000013922 glutamic acid Nutrition 0.000 title abstract description 19
- 239000004220 glutamic acid Substances 0.000 title abstract description 19
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 53
- 239000007788 liquid Substances 0.000 claims abstract description 44
- 238000000855 fermentation Methods 0.000 claims abstract description 28
- 230000004151 fermentation Effects 0.000 claims abstract description 28
- QGZKDVFQNNGYKY-UHFFFAOYSA-N ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000005342 ion exchange Methods 0.000 claims abstract description 9
- 239000006228 supernatant Substances 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- WQZGKKKJIJFFOK-GASJEMHNSA-N D-Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 16
- 239000008103 glucose Substances 0.000 claims description 16
- 230000005611 electricity Effects 0.000 claims description 15
- 229910052760 oxygen Inorganic materials 0.000 claims description 12
- 239000001301 oxygen Substances 0.000 claims description 12
- MYMOFIZGZYHOMD-UHFFFAOYSA-N oxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 12
- 239000001963 growth media Substances 0.000 claims description 10
- HNBDQABBWNOTRU-UHFFFAOYSA-N thalline Chemical compound C1=CC=[Tl]C=C1 HNBDQABBWNOTRU-UHFFFAOYSA-N 0.000 claims description 10
- 239000002253 acid Substances 0.000 claims description 9
- 241000209149 Zea Species 0.000 claims description 8
- 235000002017 Zea mays subsp mays Nutrition 0.000 claims description 8
- 235000005822 corn Nutrition 0.000 claims description 8
- 235000005824 corn Nutrition 0.000 claims description 8
- 239000002054 inoculum Substances 0.000 claims description 8
- XSQUKJJJFZCRTK-UHFFFAOYSA-N urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 8
- 230000001580 bacterial Effects 0.000 claims description 7
- 241000186226 Corynebacterium glutamicum Species 0.000 claims description 6
- 102000004169 proteins and genes Human genes 0.000 claims description 6
- 108090000623 proteins and genes Proteins 0.000 claims description 6
- 108010021006 Tyrothricin Proteins 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 238000005469 granulation Methods 0.000 claims description 5
- 230000003179 granulation Effects 0.000 claims description 5
- 239000002609 media Substances 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 238000004062 sedimentation Methods 0.000 claims description 5
- 229960003281 tyrothricin Drugs 0.000 claims description 5
- 229930003756 Vitamin B7 Natural products 0.000 claims description 4
- 238000010564 aerobic fermentation Methods 0.000 claims description 4
- YBJHBAHKTGYVGT-ZKWXMUAHSA-N biotin Chemical compound N1C(=O)N[C@@H]2[C@H](CCCCC(=O)O)SC[C@@H]21 YBJHBAHKTGYVGT-ZKWXMUAHSA-N 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 238000011081 inoculation Methods 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 230000001954 sterilising Effects 0.000 claims description 4
- 238000004659 sterilization and disinfection Methods 0.000 claims description 4
- 239000011735 vitamin B7 Substances 0.000 claims description 4
- 235000011912 vitamin B7 Nutrition 0.000 claims description 4
- 241000186146 Brevibacterium Species 0.000 claims description 2
- GSXRBRIWJGAPDU-BBVRJQLQSA-N Tyrothricin Chemical compound C([C@H]1C(=O)N[C@H](C(=O)N[C@@H](CCCN)C(=O)N[C@H](C(N[C@H](CC=2C=CC=CC=2)C(=O)N2CCC[C@H]2C(=O)N[C@@H](CC=2C=CC=CC=2)C(=O)N[C@H](CC=2C=CC=CC=2)C(=O)N[C@@H](CC(N)=O)C(=O)N[C@@H](CCC(N)=O)C(=O)N1)=O)CC(C)C)C(C)C)C1=CC=C(O)C=C1 GSXRBRIWJGAPDU-BBVRJQLQSA-N 0.000 claims 1
- 238000000034 method Methods 0.000 abstract description 22
- 238000001704 evaporation Methods 0.000 abstract description 9
- 239000002351 wastewater Substances 0.000 abstract description 7
- 238000000605 extraction Methods 0.000 abstract description 6
- 235000013923 monosodium glutamate Nutrition 0.000 abstract description 6
- 239000003337 fertilizer Substances 0.000 abstract description 4
- 229940073490 Sodium Glutamate Drugs 0.000 abstract description 2
- 235000001014 amino acid Nutrition 0.000 abstract description 2
- 150000001413 amino acids Chemical class 0.000 abstract description 2
- 239000000463 material Substances 0.000 abstract description 2
- LPUQAYUQRXPFSQ-UHFFFAOYSA-M monosodium glutamate Chemical compound [Na+].[O-]C(=O)C(N)CCC(O)=O LPUQAYUQRXPFSQ-UHFFFAOYSA-M 0.000 abstract description 2
- 239000012530 fluid Substances 0.000 abstract 2
- 241001052560 Thallis Species 0.000 abstract 1
- 238000004134 energy conservation Methods 0.000 abstract 1
- 238000005265 energy consumption Methods 0.000 abstract 1
- 239000004615 ingredient Substances 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 239000000284 extract Substances 0.000 description 8
- 238000002425 crystallisation Methods 0.000 description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 230000005712 crystallization Effects 0.000 description 5
- 238000010291 electrical method Methods 0.000 description 5
- 235000018102 proteins Nutrition 0.000 description 5
- NLJVXZFCYKWXLH-DXTIXLATSA-N 3-[(3R,6S,9S,12S,15S,17S,20S,22R,25S,28S)-20-(2-amino-2-oxoethyl)-9-(3-aminopropyl)-3,22,25-tribenzyl-15-[(4-hydroxyphenyl)methyl]-6-(2-methylpropyl)-2,5,8,11,14,18,21,24,27-nonaoxo-12-propan-2-yl-1,4,7,10,13,16,19,23,26-nonazabicyclo[26.3.0]hentriacontan Chemical compound C([C@H]1C(=O)N[C@H](C(=O)N[C@@H](CCCN)C(=O)N[C@H](C(N[C@H](CC=2C=CC=CC=2)C(=O)N2CCC[C@H]2C(=O)N[C@@H](CC=2C=CC=CC=2)C(=O)N[C@H](CC=2C=CC=CC=2)C(=O)[C@H](CC(N)=O)NC(=O)[C@H](CCC(O)=O)N1)=O)CC(C)C)C(C)C)C1=CC=C(O)C=C1 NLJVXZFCYKWXLH-DXTIXLATSA-N 0.000 description 4
- LPUQAYUQRXPFSQ-DFWYDOINSA-M monosodium L-glutamate Chemical compound [Na+].[O-]C(=O)[C@@H](N)CCC(O)=O LPUQAYUQRXPFSQ-DFWYDOINSA-M 0.000 description 4
- 239000004223 monosodium glutamate Substances 0.000 description 4
- 241000894006 Bacteria Species 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 210000000697 sensory organs Anatomy 0.000 description 3
- 239000011734 sodium Substances 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- VEXZGXHMUGYJMC-UHFFFAOYSA-N HCl Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- 230000036740 Metabolism Effects 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- JVTAAEKCZFNVCJ-UHFFFAOYSA-N lactic acid Chemical compound CC(O)C(O)=O JVTAAEKCZFNVCJ-UHFFFAOYSA-N 0.000 description 2
- 239000004310 lactic acid Substances 0.000 description 2
- 235000014655 lactic acid Nutrition 0.000 description 2
- 230000004060 metabolic process Effects 0.000 description 2
- 230000035786 metabolism Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000012452 mother liquor Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- -1 resource cost is few Substances 0.000 description 2
- RPAJSBKBKSSMLJ-DFWYDOINSA-N (2S)-2-aminopentanedioic acid;hydrochloride Chemical compound Cl.OC(=O)[C@@H](N)CCC(O)=O RPAJSBKBKSSMLJ-DFWYDOINSA-N 0.000 description 1
- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 102000016901 Glutamate dehydrogenases Human genes 0.000 description 1
- 108091000037 Glutamate dehydrogenases Proteins 0.000 description 1
- 102000004316 Oxidoreductases Human genes 0.000 description 1
- 108090000854 Oxidoreductases Proteins 0.000 description 1
- 210000002966 Serum Anatomy 0.000 description 1
- NWONKYPBYAMBJT-UHFFFAOYSA-L Zinc sulfate Chemical compound [Zn+2].[O-]S([O-])(=O)=O NWONKYPBYAMBJT-UHFFFAOYSA-L 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 230000034659 glycolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000003317 industrial substance Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011068 load Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000012666 negative regulation of transcription by glucose Effects 0.000 description 1
- 230000003204 osmotic Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- OZAIFHULBGXAKX-UHFFFAOYSA-N precursor Substances N#CC(C)(C)N=NC(C)(C)C#N OZAIFHULBGXAKX-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 230000001105 regulatory Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 238000004642 transportation engineering Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
Abstract
The invention discloses a novel production method for glutamic acid, belonging to the technical field of the production of amino acid. The novel production method for the glutamic acid comprises the following steps of: removing thalli and insolubles by means of high-speed disc separation; evaporating and concentrating separated glutamic acid material liquid through a multi-effect plate type evaporator at low temperature, wherein the generated secondary steam condensed water is used for fermentation ingredients of the glutamic acid; performing continuous isoelectric extraction on the glutamic acid in the evaporated glutamic acid concentrated solution; absorbing the glutamic acid by making supernatant fluid pass through ion exchange columns; performing isoelectric reextraction on the analyzed glutamic acid; inputting high-concentration wastewater into a fertilizer workshop for producing fertilizer; squeezing heavy phase (mycoprotein) through a plate frame, and granulating; and drying through a fluid bed, and thus producing high-protein feed. The novel production method for the glutamic acid has the advantages of low unit consumption of liquid ammonia and sulfuric acid, high extraction yield of the glutamic acid, less ion exchange investment and the like; and meanwhile, the purity of the extracted glutamic acid is high, sodium glutamate can be produced without crystalloblast, resources are fully used in the whole process, the aims of energy conservation and consumption reduction are achieved, and the novel production method for the glutamic acid has a wide application prospect.
Description
Technical field
The present invention relates to a kind of method of High-efficient Production L-glutamic acid, belong to technical field of producing amino acid by fermentation.
Background technology
L-glutamic acid is the precursor of monosodium glutamate, be mainly used in the production of monosodium glutamate, the inside and outside most popular method of the producing country of L-glutamic acid is fermentation method, the technology of extracting L-glutamic acid from fermented liquid has multiple, main method to have: wait electrical method to extract L-glutamic acid, ion exchange method extraction L-glutamic acid, zincate process extraction L-glutamic acid, hydrochloride method extraction L-glutamic acid or electroosmose process and extract L-glutamic acid etc.
It is the following character of utilizing L-glutamic acid that its medium electrical method extracts L-glutamic acid: L-glutamic acid is a kind of amphotericeledrolyte, the solubleness minimum of L-glutamic acid in solution when the isoelectric pH value 3.22 of L-glutamic acid, industrial by in glutami acid fermentation liquor, adding sulfuric acid or hydrochloric acid, make fermented liquid pH value drop to 3.0～3.2, glutamic acid crystallization is separated out, and is referred to as isoelectric point crystallization.When isoelectric pH, the positive and negative charge of L-glutamic acid equates that total charge is 0, forms dipole ion, its solubleness minimum at this moment, and become crystal habit to separate out.Concrete extracting method can be divided into and waits electrical method intermittence and wait electrical method continuously, and intermittence etc., the electrical method advantage was technical maturity, and crystalline particle is more even, and shortcoming is can not operate continuously, and efficient is low; The advantage of isoelectric point crystallization method is continuous discharging continuously, and every grade of crystallizer is set with fixing isoelectric pH value, is easy to control, and shortcoming is that particle is inhomogeneous; Falling the pH value at crystallizer adds on this link of sulfuric acid, traditional technology adopts and directly the sulfuric acid pipeline is linked crystallizer, when adding sulfuric acid, local supersaturation occurs easily and produce the crystallization of β type, the crystallization of β type is difficult for centrifuge dehydration, tap density is little, has all brought certain difficulty to later stage packing, transportation.The prior art extracting method does not separate with L-glutamic acid liquid tropina in addition, waits the electricity cycle long, and the mother liquor hydrolysis of metacrystal process will expend a large amount of sulfuric acid, and not only wastewater treatment capacity is big, and to the equipment requirements height.Directly carry out from friendship the large usage quantity of ammonia elutriant without the feed liquid that concentrates.The liquid volume of its ubiquity ion-exchange is huge, has increased the defective of the consumption of sulfuric acid, ammoniacal liquor, has inevitably increased a large amount of waste water, raw material simultaneously.Not only environment protection treating cost height, and the many poor quality of L-glutamic acid impurity that obtain.
In recent years, industrial chemicals prices such as sulfuric acid, liquefied ammonia rose steadily, and society requires to improve constantly to pollutant discharge of enterprise simultaneously.Therefore, inventing a kind of sulfuric acid, liquefied ammonia, the alkali consumption is little, wastewater flow rate is little, and can guarantee the extraction process of extracting glutamic acid yield and quality product, is very important.And, along with " green, low consumption, environmental protection, the efficient " new historical stage has been come in the development of monosodium glutamate industry, environmental issue becomes the key that influences Sustainable Development of Enterprises, and how the production technique of L-glutamic acid just becomes important environmental protection problem from source control pollution.
Summary of the invention
The contriver passes through a series of a kind of new L-glutamic acid production methods of having researched and developed, this method is utilized high-speed dish piece to separate and is removed thalline and insolubles, L-glutamic acid feed liquid through after separating concentrates through multiple-effect plate-type evaporator low-temperature evaporation, the secondary steam water of condensation that produces, be used for the glutamic acid fermentation batching, L-glutamic acid concentrated solution after the evaporation extracts L-glutamic acid by waiting electricity continuously, supernatant liquor is by adsorbing L-glutamic acid from the friendship post, the L-glutamic acid of resolving goes to wait electricity to extract again, hc effluent removes fertilizer Workshop Production fertilizer, heavy phase (tropina) is produced high protein feed by sheet frame squeezing back granulation by fluidised bed drying.
The present invention has that liquefied ammonia, sulfuric acid unit consumption are low, extracting glutamic acid yield height, from handing over advantage such as less investment, the L-glutamic acid purity height that extracts simultaneously, whole process takes full advantage of resource, has reached the purpose of energy-saving consumption-reducing.
For achieving the above object, the concrete operations step of a kind of L-glutamic acid novel process of the present invention extracting method is:
(1) cultivates seed: preparation seed culture medium (below be mass percent): glucose 2.5%, corn steep liquor 3%, K
2HPO
43H
2O 0.2%, Na
2HPO
40.2%, vitamin H 0.5%, MgSO
47H
2O 0.2%, 0.025%, 115 ℃ of sterilization of urea 15min; Bacterial classification is inserted in the seed culture medium, and inoculum size is 3%; Under suitable temperature, pH and dissolved oxygen condition, control automatically in 5L and be cultured to logarithmic phase in the fermentor tank, make seed liquor;
(2) aerobic fermentation: the seed liquor that step (1) is made is with 15% inoculum size inoculation fermentation, and control fermented liquid temperature employing order temperature raising pattern: 0～5h is 33 ℃, and 5～10h is 34 ℃, and 10～18h is 35 ℃, and 18～26h is 36 ℃, and 26～32h is 37 ℃; Feed suitable air, regulate the agitation as appropriate rotating speed, adopting the control of oxygen supply pattern stage by stage dissolved oxygen level: 0～15h is that 18%, 16～32h is 6%; Control pH 7.0～7.2 by auto-feeding ammoniacal liquor; And by stream add concentration be the glucose solution of 500～800g/L with residual sugar control 0.5～1.0%, fermenting to 32h stops, and gets fermented liquid;
(3) glutami acid fermentation liquor utilizes the high-speed dish piece separating machine that the L-glutamic acid feed liquid in the fermented liquid is separated with tropina, remove the fermentation thalline, the rotating speed of high-speed dish piece machine separating thallus is 4000～5000r/min, by above condition, the L-glutamic acid feed liquid is separated with tropina.
(4) the L-glutamic acid feed liquid of separating is concentrated through multiple-effect plate-type evaporator low-temperature evaporation, obtaining L-glutamic acid content, to reach mass concentration be 25～32% L-glutamic acid concentrated solution.
(5) adopting Continuous Flow to add the sulfuric acid form by the L-glutamic acid concentrated solution after the evaporation of multiple-effect plate-type evaporator carries out waiting continuously electric sedimentation to extract L-glutamic acid to L-glutamic acid, reaches the purpose that L-glutamic acid separates with supernatant liquor.Continuously etc. in the galvanic process process, add to certain flow velocity Continuous Flow through the L-glutamic acid feed liquid of concentration and sulfuric acid and to wait in the electricity jar pH3.0～3.2.
(6) above-mentioned supernatant liquor adds sulfuric acid and transfers pH to carry out ion exchange column adsorbing and extracting L-glutamic acid after 1.5～1.8, liquefied ammonia is transferred to the ion exchange column of pH9.0 carry out wash-out.Elutriant adds sulfuric acid and transfers pH to pump into after 1.8 to wait electricity jar in the step (5), mixes with former concentrated solution and extracts L-glutamic acid.
(7) tropina of Fen Liing is produced high protein feed by sheet frame squeezing back granulation by fluidised bed drying.
Wherein fermention medium is preferably in the step (2): glucose 10%, corn steep liquor 0.5%, MgSO
47H
2O 0.2%, K
2HPO
43H
2O 0.2%, NaCl 0.2%, MnSO
40.001%, FeSO
40.0001%, V
B10.00001%, pH 7.0～7.2;
Fermented bacterium is preferred: Corynebacterium glutamicum (Corynebacterium glutamicum) ATCC13032, or Tianjin tyrothricin (Brevibacterium Tianjianense), described Tianjin tyrothricin is preferably Tianjin tyrothricin T613.
The present invention adds the glucose solution of higher concentration remaining sugar concentration is controlled in appropriate level by proper flow, make and cause because glucose concn is too high neither in the whole fermentation process that osmotic pressure is excessive and produce " glucose effect " and check catabolite, do not cross the low substrate restriction that constitutes because of glucose concn yet, residual sugar in the fermented liquid is exhausted rapidly, cause bacterial classification throughput not brought into play to greatest extent, and by suitably regulating fermentor tank mixing speed and air quantity oxyty is controlled on appropriate level, making in the whole fermentation process neither causes TCA cyclic metabolism flow to reduce because oxyty is low excessively, be not enough to balance glucose glycolysis speed, thereby stimulated the enzyme of serum lactic dehydrogenase to live, the metabolism circulation is generated to lactic acid, cause the lactic acid accumulation, also do not cause the glutamate dehydrogenase enzyme to be lived because oxyty is too high and obviously reduce, the TCA circular flow strengthens a large amount of losses that generate a large amount of CO2 and cause carbon source;
The present invention at first uses the high-speed dish piece separating machine that the L-glutamic acid feed liquid in the fermented liquid is separated with tropina, remove the fermentation thalline, the rotating speed of high-speed dish piece machine separating thallus is 4000～5000r/min, by above condition, the L-glutamic acid feed liquid is separated with tropina, this uses the high-speed dish piece separating machine to initiate as the applicant, disc separator is a kind of in the settling centrifuge, the material (emulsion of the liquid composition that for example suspension of viscous liquid and tiny solid granulometric composition or density are close etc.) that separates for separating of difficulty.The present invention used the thalline in the disc separator removal fermented liquid before isoelectric point crystallization, not only reach the purpose that reclaims glu thalline protein, can also obviously improve the L-glutamic acid one inferior electric rate of recovery and improve the glutamic acid crystal quality, adopt the high-speed dish piece separating machine except behind the tropina, the one inferior electric rate of recovery has improved 5% the rate of recovery with respect to electricity such as direct, alleviated the load of ion exchange process, make that the unit consumption of ammonia is low, and can avoid occurring thin crystalline substance, the electricity cycles such as shortening, save a large amount of sulfuric acid, whole process save energy of the present invention, resource cost is few, and wastewater discharge is few, pollute lowly, when reducing investment, not only save manpower and the time more can be improved economic benefit of enterprises.
L-glutamic acid production technique provided by the invention, the liquid circulation in the process system is used, and reduces product loss, saves process water.And reduce waste water from the source, guarantee product purity, improve extract yield and production efficiency height, reduce production costs, and then make the performance of enterprises better.
The present invention has shortened the whole production cycle comparing with existing production technique, seed culture foreshortens to 5h, and and the output that has significantly improved L-glutamic acid reaches more than the 200g/L, L-glutamic acid purity reaches more than 98.5%, extract yield reaches 93%, sulfate radical is less than 0.2mg/L, the finished color sense organ is good, crystal grain is even, the thalline that produces in the production, time condensation liquid, mother liquor etc. all are fully utilized, not only solve the sewage discharge problem that always perplexs industry, also turn waste into wealth, created new economic worth.And whole simple operation of process, production cost is lower, and remarkable in economical benefits very is suitable for suitability for industrialized production.
Embodiment
Embodiment 1
(1) at first prepares glutami acid fermentation liquor: cultivate seed, preparation seed culture medium (below be mass percent): glucose 2.5%, corn steep liquor 3%, K
2HPO
43H
2O 0.2%, Na
2HPO
40.2%, vitamin H 0.5%, MgSO
47H
2O 0.2%, 0.025%, 115 ℃ of sterilization of urea 15min; Bacterial classification is inserted in the seed culture medium, and inoculum size is 3%; Under suitable temperature, pH and dissolved oxygen condition, control automatically in 5L and be cultured to logarithmic phase in the fermentor tank, make seed liquor;
(2) aerobic fermentation: the seed liquor that step (1) is made is with 15% inoculum size inoculation fermentation, and control fermented liquid temperature employing order temperature raising pattern: 0～5h is 33 ℃, and 5～10h is 34 ℃, and 10～18h is 35 ℃, and 18～26h is 36 ℃, and 26～32h is 37 ℃; Feed suitable air, regulate the agitation as appropriate rotating speed, adopting the control of oxygen supply pattern stage by stage dissolved oxygen level: 0～15h is that 18%, 16～32h is 6%; Control pH 7.2 by auto-feeding ammoniacal liquor; And to add concentration by stream be that the glucose solution of 500g/L ferments residual sugar control to 32h 0.5～1.0% and stops, and gets fermented liquid;
Wherein fermention medium is (mass percent): glucose 10%, corn steep liquor 0.5%, MgSO
47H
2O 0.2%, K
2HPO
43H
2O 0.2%, NaCl 0.2%, MnSO
40.001%, FeSO
40.0001%, V
B10.00001%, pH 7.0～7.2;
(3) glutami acid fermentation liquor utilizes the high-speed dish piece separating machine that the L-glutamic acid feed liquid in the fermented liquid is separated with tropina, remove the fermentation thalline, the rotating speed of high-speed dish piece machine separating thallus is 4000～5000r/min, by above condition, the L-glutamic acid feed liquid is separated with tropina.
(4) the L-glutamic acid feed liquid of separating is concentrated through multiple-effect plate-type evaporator low-temperature evaporation, obtaining L-glutamic acid content, to reach mass concentration be 25% L-glutamic acid concentrated solution.
(5) adopting Continuous Flow to add the sulfuric acid form by the L-glutamic acid concentrated solution after the evaporation of multiple-effect plate-type evaporator carries out waiting continuously electric sedimentation to extract L-glutamic acid to L-glutamic acid, reaches the purpose that L-glutamic acid separates with supernatant liquor.Continuously etc. in the galvanic process process, add to certain flow velocity Continuous Flow through the L-glutamic acid feed liquid of concentration and sulfuric acid and to wait in the electricity jar pH3.0～3.2.
(6) above-mentioned supernatant liquor adds sulfuric acid and transfers pH to carry out after 1.5～1.8 from handing over post adsorbing and extracting L-glutamic acid, and liquefied ammonia is transferred to pH9.0 to from handing over post to carry out wash-out.The L-glutamic acid of resolving adds sulfuric acid and transfers pH to pump into after 1.8 to wait the electricity jar to mix with former concentrated solution to extract L-glutamic acid.Monosodium glutamate after the L-glutamic acid of the electric sedimentation of equity neutralizes is refining.
(7) with disc separator the tropina that the fermentation thalline separates is squeezed the back granulation by sheet frame, produce high protein feed by fluidised bed drying.
Fermented bacterium is preferred: Corynebacterium glutamicum (Corynebacterium glutamicum) ATCC13032.
After testing, the output of L-glutamic acid reaches 205g/L, and L-glutamic acid purity is that sulfate radical is less than 0.2mg/L more than 98.5%, the finished color sense organ is good, crystal grain is even, and shortened fermentation period, etc. the electricity cycle, save a large amount of sulfuric acid, resource cost is few, wastewater discharge is few, pollutes lowly, not only saves manpower and the time more can be improved economic benefit of enterprises when reducing investment.
Embodiment 2
Fermented bacterium is selected Tianjin tyrothricin T613.
(1) at first prepares glutami acid fermentation liquor: cultivate seed, preparation seed culture medium (below be mass percent): glucose 2.5%, corn steep liquor 3%, K
2HPO
43H
2O 0.2%, Na
2HPO
40.2%, vitamin H 0.5%, MgSO
47H
2O 0.2%, 0.025%, 115 ℃ of sterilization of urea 15min; Bacterial classification is inserted in the seed culture medium, and inoculum size is 3%; Under suitable temperature, pH and dissolved oxygen condition, control automatically in 5L and be cultured to logarithmic phase in the fermentor tank, make seed liquor;
(2) aerobic fermentation: the seed liquor that step (1) is made is with 15% inoculum size inoculation fermentation, and control fermented liquid temperature employing order temperature raising pattern: 0～5h is 33 ℃, and 5～10h is 34 ℃, and 10～18h is 35 ℃, and 18～26h is 36 ℃, and 26～32h is 37 ℃; Feed suitable air, regulate the agitation as appropriate rotating speed, adopting the control of oxygen supply pattern stage by stage dissolved oxygen level: 0～15h is that 18%, 16～32h is 6%; Control pH 7.0～7.2 by auto-feeding ammoniacal liquor; And by stream add concentration be the glucose solution of 500g/L with residual sugar control 1.0%, fermenting to 32h stops, and gets fermented liquid;
Wherein fermention medium is preferably (mass percent): glucose 10%, corn steep liquor 0.5%, MgSO
47H
2O 0.2%, K
2HPO
43H
2O 0.2%, NaCl 0.2%, MnSO
40.001%, FeSO
40.0001%, V
Bl0.00001%, pH7.0～7.2;
(3) glutami acid fermentation liquor utilizes the high-speed dish piece separating machine that the L-glutamic acid feed liquid in the fermented liquid is separated with tropina, remove the fermentation thalline, the rotating speed of high-speed dish piece machine separating thallus is 4000～5000r/min, by above condition, the L-glutamic acid feed liquid is separated with tropina.
(4) the L-glutamic acid feed liquid of separating is concentrated through multiple-effect plate-type evaporator low-temperature evaporation, obtaining L-glutamic acid content, to reach mass concentration be 32% L-glutamic acid concentrated solution.
(5) adopting Continuous Flow to add the sulfuric acid form by the L-glutamic acid concentrated solution after the evaporation of multiple-effect plate-type evaporator carries out waiting continuously electric sedimentation to extract L-glutamic acid to L-glutamic acid, reaches the purpose that L-glutamic acid separates with supernatant liquor.Continuously etc. in the galvanic process process, add to certain flow velocity Continuous Flow through the L-glutamic acid feed liquid of concentration and sulfuric acid and to wait in the electricity jar pH3.0～3.2.
(6) above-mentioned supernatant liquor adds sulfuric acid and transfers pH to carry out after 1.5～1.8 from handing over post adsorbing and extracting L-glutamic acid, and liquefied ammonia is transferred to pH9.0 to from handing over post to carry out wash-out.Elutriant adds sulfuric acid and transfers pH to pump into after 1.8 to wait the electricity jar to mix with former concentrated solution to extract L-glutamic acid.
(7) tropina of Fen Liing is produced high protein feed by sheet frame squeezing back granulation by fluidised bed drying.
After testing, the output of L-glutamic acid reaches 200g/L, and L-glutamic acid purity is that sulfate radical is less than 0.2mg/L more than 98%, the finished color sense organ is good, crystal grain is even, and shortened fermentation period, etc. the electricity cycle, save a large amount of sulfuric acid, resource cost is few, wastewater discharge is few, pollutes lowly, not only saves manpower and the time more can be improved economic benefit of enterprises when reducing investment.
The present invention has that liquefied ammonia, sulfuric acid unit consumption are low, extracting glutamic acid yield height, from handing over advantage such as less investment, the L-glutamic acid purity height that extracts simultaneously, do not need metacrystal can produce Sodium Glutamate, whole process takes full advantage of resource, reached the purpose of energy-saving consumption-reducing, had broad application prospects.
Claims (2)
1. the production method of a L-glutamic acid is characterized in that comprising the steps:
(1) the preparation glutami acid fermentation liquor is at first prepared seed culture medium, and bacterial classification is inserted in the seed culture medium, makes seed liquor; Leavening temperature employing order temperature raising pattern feeds suitable air, control dissolved oxygen level and pH, and fermentation 32h gets fermented liquid;
(2) glutami acid fermentation liquor utilizes the high-speed dish piece separating machine that the L-glutamic acid feed liquid in the fermented liquid is separated with tropina, removes the fermentation thalline, and the rotating speed of high-speed dish piece machine separating thallus is 4000～5000r/min;
(3) the L-glutamic acid feed liquid of separating is concentrated, obtaining L-glutamic acid content is the L-glutamic acid concentrated solution of weight fraction 25～32%,
(4) Continuous Flow adds sulfuric acid and carries out waiting continuously electric sedimentation to extract L-glutamic acid to L-glutamic acid in waiting electricity jar, pH3.0～3.2,
(5) etc. electric supernatant liquor adds sulfuric acid and transfers pH to carry out ion exchange column adsorbing and extracting L-glutamic acid after 1.5～1.8, and liquefied ammonia is transferred to pH9.0, and ion exchange column is carried out wash-out, and the L-glutamic acid of wash-out adds sulfuric acid and transfers pH to pump into after 1.8 to wait electricity jar in the step (4);
(6) tropina of Fen Liing is produced high protein feed by sheet frame squeezing back granulation by fluidised bed drying;
Wherein the glutami acid fermentation liquor concrete operations are described in the step (1):
Cultivate seed: the preparation seed culture medium below is mass percent: glucose 2.5%, corn steep liquor 3%, K
2HPO
43H
2O0.2%, Na
2HPO
40.2%, vitamin H 0.5%, MgSO
47H
2O0.2%, urea 0.025%, all the other are water, 115 ℃ of sterilization 15min; Bacterial classification is inserted in the seed culture medium, and inoculum size is 3%; Automatically control in 5L and to be cultured to logarithmic phase in the fermentor tank, make seed liquor;
Aerobic fermentation: with 15% inoculum size inoculation fermentation, control fermented liquid temperature employing order temperature raising pattern: 0～5h is 33 ℃, and 5～10h is 34 ℃, and 10～18h is 35 ℃, and 18～26h is 36 ℃, and 26～32h is 37 ℃ with the seed liquor that makes; Feed suitable air, regulate the agitation as appropriate rotating speed, adopting the control of oxygen supply pattern stage by stage dissolved oxygen level: 0～15h is that 18%, 16～32h is 6%; Control pH 7.2 by auto-feeding ammoniacal liquor; And by stream add concentration be the glucose solution of 500g/L with residual sugar control 0.5～1.0%, fermenting to 32h stops, and gets fermented liquid;
Wherein fermention medium is, mass percent: glucose 10%, corn steep liquor 0.5%, MgSO
47H
2O0.2%, K
2HPO
43H
2O0.2%, NaCl0.2%, MnSO
40.001%, FeSO
40.0001%, V
B10.00001%, pH7.0～7.2.
2. method according to claim 1 is characterized in that bacterial classification is Corynebacterium glutamicum (Corynebacterium glutamicum) ATCC13032, or Tianjin tyrothricin (Brevibacterium Tianjianense).
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