CN116649557A - Microcrystalline monosodium glutamate and preparation method and application thereof - Google Patents
Microcrystalline monosodium glutamate and preparation method and application thereof Download PDFInfo
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- CN116649557A CN116649557A CN202210158345.4A CN202210158345A CN116649557A CN 116649557 A CN116649557 A CN 116649557A CN 202210158345 A CN202210158345 A CN 202210158345A CN 116649557 A CN116649557 A CN 116649557A
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- monosodium glutamate
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- glutamate
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- LPUQAYUQRXPFSQ-DFWYDOINSA-M monosodium L-glutamate Chemical compound [Na+].[O-]C(=O)[C@@H](N)CCC(O)=O LPUQAYUQRXPFSQ-DFWYDOINSA-M 0.000 title claims abstract description 194
- 235000013923 monosodium glutamate Nutrition 0.000 title claims abstract description 193
- 239000004223 monosodium glutamate Substances 0.000 title claims abstract description 151
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000013078 crystal Substances 0.000 claims abstract description 90
- 238000001816 cooling Methods 0.000 claims abstract description 75
- 238000000034 method Methods 0.000 claims abstract description 67
- 238000002425 crystallisation Methods 0.000 claims abstract description 49
- 229940073490 sodium glutamate Drugs 0.000 claims abstract description 42
- 230000008025 crystallization Effects 0.000 claims abstract description 39
- 238000001704 evaporation Methods 0.000 claims abstract description 18
- 238000004519 manufacturing process Methods 0.000 claims abstract description 14
- 235000013305 food Nutrition 0.000 claims abstract description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 48
- 238000001035 drying Methods 0.000 claims description 48
- 239000002245 particle Substances 0.000 claims description 36
- GJBHGUUFMNITCI-QTNFYWBSSA-M sodium;(2s)-2-aminopentanedioate;hydron;hydrate Chemical compound O.[Na+].OC(=O)[C@@H](N)CCC([O-])=O GJBHGUUFMNITCI-QTNFYWBSSA-M 0.000 claims description 32
- 239000007788 liquid Substances 0.000 claims description 19
- 238000009826 distribution Methods 0.000 claims description 17
- 238000001914 filtration Methods 0.000 claims description 13
- 239000012141 concentrate Substances 0.000 claims description 8
- BBJIPMIXTXKYLZ-UHFFFAOYSA-N isoglutamic acid Chemical compound OC(=O)CC(N)CC(O)=O BBJIPMIXTXKYLZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000002994 raw material Substances 0.000 claims description 5
- 159000000000 sodium salts Chemical class 0.000 claims description 4
- 230000003472 neutralizing effect Effects 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 29
- 238000004090 dissolution Methods 0.000 abstract description 7
- 230000006340 racemization Effects 0.000 abstract description 5
- 235000021168 barbecue Nutrition 0.000 abstract description 3
- 238000007086 side reaction Methods 0.000 abstract description 3
- 229940045635 sodium pyroglutamate Drugs 0.000 abstract description 3
- CRPCXAMJWCDHFM-DFWYDOINSA-M sodium;(2s)-5-oxopyrrolidine-2-carboxylate Chemical compound [Na+].[O-]C(=O)[C@@H]1CCC(=O)N1 CRPCXAMJWCDHFM-DFWYDOINSA-M 0.000 abstract description 3
- 239000000243 solution Substances 0.000 description 116
- 238000006386 neutralization reaction Methods 0.000 description 59
- WHUUTDBJXJRKMK-VKHMYHEASA-N L-glutamic acid Chemical compound OC(=O)[C@@H](N)CCC(O)=O WHUUTDBJXJRKMK-VKHMYHEASA-N 0.000 description 48
- WHUUTDBJXJRKMK-UHFFFAOYSA-N Glutamic acid Natural products OC(=O)C(N)CCC(O)=O WHUUTDBJXJRKMK-UHFFFAOYSA-N 0.000 description 46
- 239000004220 glutamic acid Substances 0.000 description 46
- 235000013922 glutamic acid Nutrition 0.000 description 46
- 230000001276 controlling effect Effects 0.000 description 28
- 238000004042 decolorization Methods 0.000 description 28
- 238000003756 stirring Methods 0.000 description 27
- 238000000926 separation method Methods 0.000 description 23
- 239000000047 product Substances 0.000 description 21
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 20
- 239000000796 flavoring agent Substances 0.000 description 18
- 235000019634 flavors Nutrition 0.000 description 18
- 230000000052 comparative effect Effects 0.000 description 17
- VLTRZXGMWDSKGL-UHFFFAOYSA-N perchloric acid Chemical compound OCl(=O)(=O)=O VLTRZXGMWDSKGL-UHFFFAOYSA-N 0.000 description 16
- 235000011121 sodium hydroxide Nutrition 0.000 description 15
- 230000008569 process Effects 0.000 description 14
- 239000000463 material Substances 0.000 description 13
- 239000000843 powder Substances 0.000 description 13
- 230000008020 evaporation Effects 0.000 description 12
- 238000000855 fermentation Methods 0.000 description 11
- 230000004151 fermentation Effects 0.000 description 11
- 239000000706 filtrate Substances 0.000 description 11
- 238000001514 detection method Methods 0.000 description 10
- 229910000029 sodium carbonate Inorganic materials 0.000 description 10
- 238000002834 transmittance Methods 0.000 description 10
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 9
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 9
- 238000010009 beating Methods 0.000 description 9
- 239000000498 cooling water Substances 0.000 description 9
- 230000004580 weight loss Effects 0.000 description 9
- 239000003610 charcoal Substances 0.000 description 8
- 238000006243 chemical reaction Methods 0.000 description 8
- 238000007796 conventional method Methods 0.000 description 8
- 238000012544 monitoring process Methods 0.000 description 8
- 238000012216 screening Methods 0.000 description 8
- 238000004448 titration Methods 0.000 description 8
- 229910052799 carbon Inorganic materials 0.000 description 7
- 238000010438 heat treatment Methods 0.000 description 5
- 229910021529 ammonia Inorganic materials 0.000 description 4
- 238000005352 clarification Methods 0.000 description 4
- 239000011549 crystallization solution Substances 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000012528 membrane Substances 0.000 description 3
- 239000012452 mother liquor Substances 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- 230000001502 supplementing effect Effects 0.000 description 3
- 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 description 2
- ODHCTXKNWHHXJC-VKHMYHEASA-N 5-oxo-L-proline Chemical compound OC(=O)[C@@H]1CCC(=O)N1 ODHCTXKNWHHXJC-VKHMYHEASA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- 241000186226 Corynebacterium glutamicum Species 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- ODHCTXKNWHHXJC-GSVOUGTGSA-N Pyroglutamic acid Natural products OC(=O)[C@H]1CCC(=O)N1 ODHCTXKNWHHXJC-GSVOUGTGSA-N 0.000 description 2
- 241001052560 Thallis Species 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- ODHCTXKNWHHXJC-UHFFFAOYSA-N acide pyroglutamique Natural products OC(=O)C1CCC(=O)N1 ODHCTXKNWHHXJC-UHFFFAOYSA-N 0.000 description 2
- 238000005054 agglomeration Methods 0.000 description 2
- 230000002776 aggregation Effects 0.000 description 2
- PHKGGXPMPXXISP-DFWYDOINSA-N azanium;(4s)-4-amino-5-hydroxy-5-oxopentanoate Chemical compound [NH4+].[O-]C(=O)[C@@H]([NH3+])CCC([O-])=O PHKGGXPMPXXISP-DFWYDOINSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 230000004060 metabolic process Effects 0.000 description 2
- 230000000813 microbial effect Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 235000013917 monoammonium glutamate Nutrition 0.000 description 2
- 235000018102 proteins Nutrition 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 238000007670 refining Methods 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011343 solid material Substances 0.000 description 2
- 238000000108 ultra-filtration Methods 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 1
- 206010010075 Coma hepatic Diseases 0.000 description 1
- 229920002261 Corn starch Polymers 0.000 description 1
- 229910002651 NO3 Inorganic materials 0.000 description 1
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 description 1
- 239000001888 Peptone Substances 0.000 description 1
- 108010080698 Peptones Proteins 0.000 description 1
- 108010009736 Protein Hydrolysates Proteins 0.000 description 1
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 1
- 240000008042 Zea mays Species 0.000 description 1
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 1
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 235000011114 ammonium hydroxide Nutrition 0.000 description 1
- 150000003863 ammonium salts Chemical class 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000036528 appetite Effects 0.000 description 1
- 235000019789 appetite Nutrition 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000002585 base Substances 0.000 description 1
- 229960002685 biotin Drugs 0.000 description 1
- 235000020958 biotin Nutrition 0.000 description 1
- 239000011616 biotin Substances 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 210000004556 brain Anatomy 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 229940041514 candida albicans extract Drugs 0.000 description 1
- 239000004202 carbamide Substances 0.000 description 1
- 210000003169 central nervous system Anatomy 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 235000005822 corn Nutrition 0.000 description 1
- 239000008120 corn starch Substances 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000011552 falling film Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 235000011194 food seasoning agent Nutrition 0.000 description 1
- 210000004211 gastric acid Anatomy 0.000 description 1
- ZDXPYRJPNDTMRX-UHFFFAOYSA-N glutamine Natural products OC(=O)C(N)CCC(N)=O ZDXPYRJPNDTMRX-UHFFFAOYSA-N 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 201000001059 hepatic coma Diseases 0.000 description 1
- 208000007386 hepatic encephalopathy Diseases 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 238000005374 membrane filtration Methods 0.000 description 1
- 235000013379 molasses Nutrition 0.000 description 1
- 238000001728 nano-filtration Methods 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 235000019319 peptone Nutrition 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000022558 protein metabolic process Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000010583 slow cooling Methods 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 230000004936 stimulating effect Effects 0.000 description 1
- 230000000638 stimulation Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 1
- 210000001779 taste bud Anatomy 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 238000011426 transformation method Methods 0.000 description 1
- 235000013311 vegetables Nutrition 0.000 description 1
- 239000012138 yeast extract Substances 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/20—Synthetic spices, flavouring agents or condiments
- A23L27/21—Synthetic spices, flavouring agents or condiments containing amino acids
- A23L27/22—Synthetic spices, flavouring agents or condiments containing amino acids containing glutamic acids
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/90—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in food processing or handling, e.g. food conservation
Abstract
The invention relates to the technical field of monosodium glutamate production, in particular to microcrystalline monosodium glutamate and a preparation method and application thereof. The preparation method of the microcrystalline monosodium glutamate comprises the following steps: evaporating and concentrating the sodium glutamate solution to supersaturated concentration to obtain sodium glutamate concentrated solution, rapidly cooling the sodium glutamate concentrated solution to 40-50 ℃ through first cooling treatment, adding seed crystal, and then performing second cooling treatment to generate sodium glutamate crystals; wherein the second cooling treatment is gradient cooling. The method can effectively avoid the generation of sodium pyroglutamate and racemization side reaction, and the prepared monosodium glutamate has high purity and high primary crystallization yield; the crystal growth can be well controlled, the self-initiated crystal is prevented, the operation is simple, and the monosodium glutamate with a specific granularity range can be prepared without repeatedly adding water to complete the crystal; meanwhile, the glossiness of monosodium glutamate is well ensured, and caking is avoided; the microcrystalline monosodium glutamate prepared by the method has high dissolution rate and is convenient to be applied to food such as cold dishes, barbecue and the like.
Description
Technical Field
The invention relates to the technical field of monosodium glutamate production, in particular to microcrystalline monosodium glutamate and a preparation method and application thereof.
Background
Monosodium glutamate, sodium glutamate and monosodium glutamate, mainly comprises L-monosodium glutamate monohydrate, and has chemical formula of C 5 H 8 NO 4 Na·H 2 O, moleculeThe amount of 187 is usually white columnar crystals or crystalline powder, and is widely applied to the food and seasoning industries because of the capability of stimulating taste buds and increasing the delicate flavor of foods, particularly meats and vegetables, so as to promote the appetite of people. Monosodium glutamate is converted into glutamic acid under the action of gastric acid after being eaten, and the glutamic acid is absorbed by a human body to form protein in human tissues; the composition can be combined with blood ammonia to form glutamine harmless to organisms, so that toxic effects of ammonia generated in a tissue metabolic process are relieved, and the composition is clinically used for treating hepatic coma patients; but also can participate in brain protein metabolism and sugar metabolism, promote oxidation process, and play a good role in normal activities of the central nervous system, so that the method has wide application in the pharmaceutical industry.
At present, the production of monosodium glutamate mainly adopts a microbial fermentation method. The process for producing monosodium glutamate by using a microbial fermentation method mainly comprises three parts of glutamic acid fermentation, glutamic acid extraction and monosodium glutamate refining. The glutamic acid fermentation is mainly produced by adopting a fermentation method of corynebacterium glutamicum with corn starch hydrolysis sugar or molasses as a carbon source and corn steep liquor, hydrolysate, yeast extract, peptone, ammonium salt, nitrate, urea, ammonia water, liquid ammonia and the like as nitrogen sources, and the glutamic acid fermentation strains mainly used at present comprise biotin sub-proper type and temperature-sensitive type strains. Glutamic acid is mainly extracted by an isoelectric point method according to the principle that glutamic acid is an ampholyte and has the minimum solubility at the isoelectric point (pH 3.22). The extraction process of glutamic acid mainly comprises isoelectric point-ion exchange method, continuous isoelectric point-crystal transformation method, low-temperature primary isoelectric point method and the like.
The monosodium glutamate refining process comprises the steps of glutamic acid neutralization, neutralization liquid decolorization and iron removal, sodium glutamate concentration and crystallization, separation, drying, packaging and the like. The glutamic acid neutralization is to carry out neutralization reaction on the extracted and separated glutamic acid and liquid caustic soda or sodium carbonate to generate monosodium glutamate solution, the neutralization solution is firstly decolorized by active carbon, the primary decolorized solution is then deironized by sodium sulfide or resin method, then the secondary decolorized solution is obtained by particle carbon decolorization, the secondary decolorized solution is transferred into a crystallization tank for continuous evaporation and crystallization, then the wet monosodium glutamate is obtained by centrifugal separation, and the wet monosodium glutamate is dried by a fluidized bed, screened and packaged to obtain the commercial monosodium glutamate.
The crystallization process of monosodium glutamate comprises three stages of supersaturation solution formation, crystal nucleus formation and crystal growth, wherein the crystal nucleus formation method mainly comprises a natural crystallization method, a stimulated crystallization method and a crystal seed crystallization method. The natural crystallization method is to naturally form crystal nuclei by controlling higher saturation concentration, and the crystal nuclei formed by the method are irregular and difficult to control in quantity, so that particles are uneven. The crystal-stimulating method is to stimulate the solution concentration to form crystal nucleus through cooling when the solution concentration reaches the crystal-stimulating area, and the method has high crystal-stimulating speed, but the quantity of the crystal nucleus is difficult to control. At present, large-particle monosodium glutamate is produced by a seed crystal crystallization method, and the method can accurately control the number of crystal nuclei, and has the advantages of regular crystal size and large particles.
The current production method of commercial monosodium glutamate mainly adopts a continuous evaporation concentration crystallization method, firstly, a certain amount of neutralization decolorization liquid is added into a crystallization tank to concentrate the commercial monosodium glutamate, the neutralization decolorization liquid is taken as a base material, the vacuum degree and the temperature of the crystallization tank are controlled, seed crystals (20-40 meshes) are added when the concentration reaches supersaturation concentration, then sodium glutamate crystals are continuously grown by taking the input seed crystals as crystal nucleus, meanwhile, materials are continuously replenished, the evaporation speed and the crystallization speed are controlled in the process to ensure that the concentration in the tank is always kept in a metastable zone, when the concentration is too high and new crystal nucleus appears, water is required to be added to dissolve tiny crystals, thereby controlling the continuous growth of crystals, when the crystal size reaches the requirement, the crystals are placed into a crystallization assisting tank, and then centrifugal separation is carried out, and wet taste essence is dried to obtain commercial monosodium glutamate (10-20 meshes), and the primary crystallization yield is 50-60%.
Patent application CN107337611A discloses a method for preparing sodium glutamate by using a glutamic acid fermentation liquor, wherein the glutamic acid fermentation liquor is subjected to ultrafiltration membrane or flocculation air floatation to remove thalli to obtain an ammonium glutamate fermentation liquor, macromolecular proteins, polysaccharides and pigments in the fermentation liquor are removed by using the ultrafiltration membrane, the obtained ammonium glutamate solution is neutralized by NaOH, the pH is controlled to be 6-8, and the temperature is controlled to be 60-80 ℃ to obtain aqueous solution of sodium glutamate and ammonia. Removing ammonia generated in the neutralization solution by compressed air at 60-80deg.C, and concentrating to obtain primary concentrate with concentration of 20-30% by nanofiltration membrane. Evaporating and concentrating the sodium glutamate primary concentrate to 30-35 Bes by adopting an MVR evaporator to obtain sodium glutamate concentrate. And continuously crystallizing the sodium glutamate concentrate at a low temperature to obtain the finished sodium glutamate product.
Patent application CN102407030a discloses a method for crystallizing monosodium glutamate at normal pressure, which separates crystallization and heating evaporation processes, i.e. the crystallization process is completed in normal pressure crystallization equipment, and the heating evaporation process is completed in negative pressure heating evaporation equipment. The concentrated sodium glutamate solution after heating and evaporation is continuously crystallized in the normal pressure crystallization equipment, the crystal is kept in the normal pressure crystallization equipment to continuously grow, the sodium glutamate solution without precipitated crystal is sent into the negative pressure heating evaporation equipment to be flash evaporated and concentrated again, and then the sodium glutamate solution enters the normal pressure crystallization equipment again to reciprocate. By crystallization under normal pressure, the crystallization temperature is kept at 55-60 ℃ all the time, the production of pyroglutamic acid is reduced to the maximum extent, and racemization of glutamic acid is not generated.
Patent application CN113647601A discloses a monosodium glutamate and a preparation method thereof, wherein glutamic acid and sodium carbonate are mixed in the presence of water to obtain a neutralization solution with the sodium glutamate content of 30-55wt%; mixing the neutralization solution with activated carbon in the presence of a filter aid for primary decolorization, and then carrying out filter pressing on the obtained neutralization decolorization solution to obtain white crystal solution containing sodium glutamate; carrying out second decolorization on the white crystal liquid by anion resin group exchange columns with different filling volume ratios to obtain monosodium glutamate mother liquor, adding 30-40 mesh seed crystals with a certain proportion into a crystallization tank at 65-72 ℃ and a vacuum degree of-0.07-0.09 MPa, continuously stirring at 15-45rpm, adding 0.05-0.2L of water into the monosodium glutamate mother liquor at intervals of 60-100min, adding water for 3-8 times, continuously crystallizing and concentrating for 2h to obtain a first solution with a saturation degree of 32 Baume; introducing the first solution into a centrifuge (the pressure is 0.5-0.7MPa, the rotating speed is 900-1100rpm, and the time is 1-5 min) at 50 ℃ for solid-liquid separation to obtain a first separation liquid and a solid material, and then drying the solid material at 80 ℃ for 2min to obtain large-particle monosodium glutamate with the average particle size of 30-44 mm.
The main problems of the above prior art include: (1) Adopting a continuous feed supplementing evaporation concentration crystallization process, and continuously increasing the impurity concentration in a crystallization tank along with the increase of the feed supplementing amount, so that the purity of monosodium glutamate is continuously reduced, and the final purity is maintained at about 99%; (2) The crystallization control operation is complex, the material supplementing speed, the evaporating speed and the crystallization speed are required to be strictly controlled in the crystal growing process, pseudomorphic crystals are formed when the concentration is too high, water is required to be repeatedly added for crystal finishing, the water adding amount is also required to be strictly controlled, and excessive water adding amount can cause crystal dissolution and material dilution; (3) Because the crystallization process is carried out at a higher temperature, the concentration of sodium glutamate in the mother liquor is higher, so that the primary crystallization yield is lower, and simultaneously, sodium pyroglutamate and racemization are easy to generate in the high-temperature crystallization process; (4) Crystallization is carried out by adopting a low-temperature stimulation crystallization method, and the number of crystal seeds cannot be controlled, so that the crystal size is different or a large amount of powder flavor essence is generated; (5) Although the large-particle monosodium glutamate is convenient to separate, the dissolution speed is low in the use process, so that the large-particle monosodium glutamate is not beneficial to being used in the flavoring of cold dishes and barbecue food.
Disclosure of Invention
The invention aims to provide microcrystalline monosodium glutamate, and a preparation method and application thereof.
Based on the problems of the prior large-particle monosodium glutamate and powder flavor essence, the invention develops the microcrystalline monosodium glutamate, the particle size of which is between that of the large-particle monosodium glutamate and the powder flavor essence, compared with the large-particle monosodium glutamate, the dissolution speed is obviously faster, the use is convenient, compared with the powder flavor essence, the moisture absorption and agglomeration are not easy, the storage is easier, and the crystallinity, the purity and the yield are higher.
Specifically, the invention provides the following technical scheme:
the invention provides a preparation method of microcrystalline monosodium glutamate, which comprises the following steps: evaporating and concentrating the sodium glutamate solution to supersaturated concentration to obtain sodium glutamate concentrated solution, rapidly cooling the sodium glutamate concentrated solution to 40-50 ℃ through first cooling treatment, adding seed crystal, and then performing second cooling treatment to generate sodium glutamate crystals; wherein the second cooling treatment is gradient cooling.
Preferably, the second cooling treatment has a gradient cooling rate of 3-5 ℃/h.
And the second cooling treatment is finished when the temperature is reduced to 12-15 ℃.
The first cooling treatment is to cool to 40-50 ℃ within 1-2h. Preferably, the temperature at which the concentration by evaporation is carried out is reduced to 40-45 ℃ in 1-2h.
According to the invention, the seed crystal crystallization method is adopted to be matched with the intermittent cooling crystallization method, firstly, the sodium glutamate concentrated solution is rapidly cooled to 40-50 ℃ from the evaporation concentration temperature, then the seed crystal is added, and the gradient slow cooling is carried out, so that the generation of pyroglutamic acid and the occurrence of racemization side reaction can be reduced, and the primary crystallization yield and the purity of sodium glutamate are obviously improved; moreover, the high-efficiency crystallization of sodium glutamate can be promoted and the spontaneous crystallization of crystals can be effectively prevented by controlling the cooling speed, so that the crystal growth can be well controlled.
In the above method, the seed crystal has an average particle size of 100-120 mesh.
By combining the intermittent cooling crystallization method, the crystal seeds are added and controlled within the granularity range, so that the crystal growth can be better controlled, the granularity of the prepared sodium glutamate monohydrate crystals is between 40 and 80 meshes, and the yield of sodium glutamate monohydrate crystals with specific granularity is obviously improved.
Preferably, the seed crystal is added in an amount of 4-8%. More preferably 5 to 7%.
In the sodium glutamate concentrate, the concentration of the sodium glutamate monohydrate is 60-65%.
Preferably, the temperature of the evaporative concentration is 55-65 ℃. More preferably 58-62 deg.c.
In the method, after the second cooling treatment is finished, the crystallization liquid is separated to obtain wet microcrystalline monosodium glutamate, and the wet microcrystalline monosodium glutamate is dried until the total moisture content is 9-10%.
In the existing preparation method of large-particle monosodium glutamate or powder monosodium glutamate, the crystal water content of monosodium glutamate is not controlled in most cases, and a higher drying temperature (above 100 ℃) is adopted in most cases. The invention discovers that the glossiness of the microcrystalline monosodium glutamate can be better ensured and the caking generation can be reduced by controlling the content of crystal water in the drying process of sodium glutamate crystals. On the basis of controlling the content of crystal water, the glossiness of monosodium glutamate can be further improved by adopting a lower drying temperature, the stability of crystal water is improved, and moisture absorption and agglomeration are reduced.
Further preferably, the drying temperature is 60-65 ℃ and the drying time is 1-2h.
In the method, the sodium glutamate solution is prepared by taking beta-glutamic acid as a raw material, neutralizing with sodium hydroxide or sodium salt, and then decoloring and filtering.
Preferably, the sodium glutamate solution has a light transmittance of 90-96%.
The concentration of sodium hydroxide or sodium salt adopted in the neutralization is 20-25%.
The sodium salt is preferably a sodium carbonate solution.
In the neutralization process, the temperature of the neutralization liquid system is controlled to be 50-55 ℃ and the pH value is controlled to be 6.3-6.8.
The decoloring can be performed by adopting special gourmet powder decoloring carbon, the adding amount of the special carbon is 0.3-0.5% (W/V), the decoloring condition is that the decoloring temperature is 50-55 ℃ and the decoloring time is 30-60min.
As a preferable scheme of the invention, the preparation method of the microcrystalline monosodium glutamate comprises the following steps:
(1) Glutamic acid neutralization: glutamic acid is taken as a raw material, 20-25% sodium hydroxide or sodium carbonate solution is fed into the raw material, stirring is carried out while feeding, the temperature of the neutralization solution is controlled to be 50-55 ℃, and feeding is stopped after the pH value reaches 6.3-6.8, so that the neutralization solution is obtained;
(2) And (3) decoloring the neutralization solution: mixing the neutralization solution obtained in the step (1) with special carbon for monosodium glutamate decolorization to decolorize, wherein the addition amount of the special carbon is 0.3-0.5% (W/V), the decolorization temperature is 50-55 ℃, the decolorization time is 30-60min, filtering after decolorization is finished, performing cyclic material beating, and collecting filtrate after clarification to obtain sodium glutamate solution with the light transmittance of 90-96%;
(3) Concentrating and crystallizing: evaporating and concentrating the sodium glutamate solution at 58-62 ℃, stopping concentrating after the concentration of the sodium glutamate monohydrate reaches 60-65%, and obtaining sodium glutamate concentrated solution; stirring the sodium glutamate concentrate at a stirring speed of 25-35rpm, cooling to 40-45 ℃ within 1-2h, adding 100-120 mesh seed crystals according to a proportion of 5-7%, cooling at a cooling speed of 3-5 ℃/h, ending crystallization after cooling to 12-15 ℃, and centrifuging the crystallization liquid to obtain wet microcrystalline monosodium glutamate;
(4) And (3) drying: and drying the wet product microcrystalline monosodium glutamate obtained by separation at 60-65 ℃ for 1-2h to obtain a microcrystalline monosodium glutamate finished product.
In the step (1), the concentration by evaporation may be performed in a rotary evaporator.
In the step (2), filtering after the decolorization is finished can be performed by using a plate-and-frame filter.
In the step (3), crystallization can be performed in a crystallizer, and cooling can be performed by introducing cooling water into a jacket of the crystallizer.
The invention provides the microcrystalline monosodium glutamate prepared by the preparation method of the microcrystalline monosodium glutamate.
Preferably, the grain size distribution of the microcrystalline monosodium glutamate is more than 90% of the grain with the particle size distribution of 40-80 meshes. More preferably, the particle size distribution is above 95% of the particles with 40-80 mesh size; the purity of the microcrystalline monosodium glutamate is more than or equal to 99.0 percent (preferably more than or equal to 99.3 percent).
As a preferable scheme of the invention, the particle size distribution of the microcrystalline monosodium glutamate is as follows: larger than 40 meshes, 0-0.5%;40-80 meshes, 97-99%; less than 80 meshes, 1-3%; sodium glutamate monohydrate content (purity of microcrystalline monosodium glutamate) of 99.0-99.8% (preferably 99.3-99.8%); the crystallinity is 98-99.9%.
The invention also provides application of the microcrystalline monosodium glutamate in preparing food.
The invention has the beneficial effects that:
1. the preparation method of the microcrystalline monosodium glutamate can effectively avoid generation of sodium pyroglutamate and racemization side reaction, and the prepared monosodium glutamate has high purity and high primary crystallization yield;
2. the preparation method of the microcrystalline monosodium glutamate can well control crystal growth, prevent self-initiated crystallization, is simple to operate, and can prepare microcrystalline monosodium glutamate with a specific granularity range without repeatedly adding water for crystallization;
3. the preparation method of the microcrystalline monosodium glutamate controls the crystallization water quantity by controlling the drying temperature and time, so that the glossiness of the monosodium glutamate is better ensured, and meanwhile, caking is effectively avoided;
4. the microcrystalline monosodium glutamate prepared by the method has high dissolution rate and is convenient to apply to food such as cold dishes, barbecue and the like.
Drawings
FIG. 1 is a picture of microcrystalline monosodium glutamate prepared in example 1 of the present invention.
FIG. 2 is a photograph of microcrystalline monosodium glutamate prepared in example 2 of the present invention.
FIG. 3 is a photograph of microcrystalline monosodium glutamate prepared in example 3 of the present invention.
FIG. 4 is a photograph of microcrystalline monosodium glutamate prepared in example 4 of the present invention.
FIG. 5 is a photograph of microcrystalline monosodium glutamate prepared in example 5 of the present invention.
FIG. 6 is a photograph of large monosodium glutamate particles prepared in comparative example 1 of the present invention.
Fig. 7 is a picture of monosodium glutamate powder prepared in comparative example 2, wherein a is a powder flavor picture and B is a powder flavor agglomerate picture.
FIG. 8 is a photograph of monosodium glutamate prepared in comparative example 3 of the present invention.
Detailed Description
The following examples are illustrative of the invention and are not intended to limit the scope of the invention.
The preparation method of crude glutamic acid (β -glutamic acid) used in the following examples and comparative examples is as follows: the glutamic acid fermentation liquid produced by fermenting temperature-sensitive corynebacterium glutamicum is taken as a raw material, thalli are removed through ceramic membrane filtration, a filter liquor is concentrated by adopting a five-effect falling film evaporator, the discharging temperature is 80 ℃, the concentration of discharged glutamic acid is 30-35%, the concentrated solution is added into an isoelectric tank for isoelectric pulling and cooling, the pH value of the concentrated solution is regulated to 3.2-3.4 through continuous flow adding concentrated sulfuric acid, then gradient cooling is carried out, and centrifugal separation is carried out when the temperature is reduced to 10 ℃, so that alpha-glutamic acid crystals are obtained. Adding wet alpha-glutamic acid into a crystal transformation tank, adding 90 ℃ hot water according to 2 times mass for dissolution, adopting liquid alkali to adjust pH to 3.7-4.3, maintaining for 1-2h, then introducing cooling water into an interlayer to cool to 10 ℃, and adopting a belt filter for filtering to obtain beta-glutamic acid, wherein the purity of the glutamic acid can reach more than 98%.
In the following examples and comparative examples, the crystallinity is defined as the ratio of sodium glutamate crystals containing one crystal water to total sodium glutamate crystals, the theoretical content of crystal water in sodium glutamate monohydrate=18/187×100% = 9.626%, the crystal water content is calculated from total moisture and loss on drying, and the calculation formula of the crystallinity is as follows:
crystallinity= (total moisture-loss on drying)/9.626%. 100%.
Example 1
The embodiment provides a production method of ultrapure microcrystalline monosodium glutamate, which comprises the following steps:
(1) Glutamic acid neutralization: adding 1Kg of crude glutamic acid into a 5L reaction kettle, adding 20% sodium hydroxide solution to dissolve glutamic acid, stirring while adding, controlling the temperature of the neutralization solution to 50 ℃, monitoring the pH of the neutralization solution on line, and stopping adding the sodium hydroxide solution when the pH reaches 6.5;
(2) And (3) decoloring the neutralization solution: adding special charcoal for flavor essence decolorization into the neutralization solution, wherein the addition amount is 0.3%, the stirring speed is 50rpm, the temperature is 50 ℃ for 30min, filtering by a plate-frame filter after decolorization is finished, circularly beating materials, clarifying, and then collecting a clear filtrate, wherein the light transmittance of the clear filtrate finally reaches 92%;
(3) Concentrating and crystallizing: transferring the filtered solution into a rotary evaporator for concentration, controlling the water bath temperature to be 60 ℃, concentrating until the concentration of sodium glutamate monohydrate reaches 60% (w/v), and stopping concentrating; pouring the concentrated solution into a crystallizer, slowly starting stirring at 30rpm, introducing cooling water into a jacket for cooling, rapidly cooling in the early stage, cooling to 40 ℃ in 1h, adding 120-mesh seed crystals according to the proportion of 5%, slowly cooling, cooling by 3 ℃ per hour, observing the number and the size of crystals in the crystallizer, controlling the cooling rate, preventing self-initiated crystals, and transferring the crystallized solution into a three-legged centrifugal machine for centrifugal separation for 15min after the temperature is reduced to 15 ℃ to obtain wet microcrystalline monosodium glutamate;
(4) And (3) drying: and (3) putting the wet product microcrystalline monosodium glutamate obtained by separation into a blast drying oven for drying at the temperature of 60 ℃ for 2 hours to obtain the ultrapure microcrystalline monosodium glutamate.
The ultrapure microcrystalline monosodium glutamate prepared by the method is shown in figure 1. Through detection, the yield of the finished product of the sodium glutamate monohydrate prepared by the method can reach 65 percent. The sodium glutamate monohydrate content is detected by a perchloric acid nonaqueous solution titration method, the drying weight loss of the microcrystalline monosodium glutamate is detected by a conventional method, the total moisture is detected by a Karl Fischer method, the crystallinity of the microcrystalline monosodium glutamate is calculated, and screening is carried out by a 40-mesh screen and a 80-mesh screen respectively, so that the particle size distribution is detected.
Example 2
The embodiment provides a production method of ultrapure microcrystalline monosodium glutamate, which comprises the following steps:
(1) Glutamic acid neutralization: adding 1Kg of crude glutamic acid into a 5L reaction kettle, adding a sodium carbonate solution with the concentration of 20% to dissolve glutamic acid, stirring while adding, controlling the temperature of a neutralization solution to 55 ℃, monitoring the pH of the neutralization solution on line, and stopping adding the sodium carbonate solution when the pH reaches 6.3;
(2) And (3) decoloring the neutralization solution: adding special charcoal for flavor essence decolorization into the neutralization solution, wherein the addition amount is 0.5%, the stirring speed is 50rpm, the temperature is 55 ℃ and maintained for 50min, filtering by a plate-frame filter after decolorization is finished, circularly beating materials, clarifying, and then collecting a clear filtrate, wherein the light transmittance of the clear filtrate finally reaches 95%;
(3) Concentrating and crystallizing: transferring the filtered solution into a rotary evaporator for concentration, controlling the water bath temperature to 55 ℃, and concentrating until the concentration of sodium glutamate monohydrate reaches 62% (w/v) to stop concentrating; pouring the concentrated solution into a crystallizer, slowly starting stirring at 30rpm, introducing cooling water into a jacket for cooling, rapidly cooling in the early stage, cooling to 40 ℃ in 1h, adding 120-mesh seed crystals according to the proportion of 5%, slowly cooling, cooling to 5 ℃ per hour, observing the number and the size of crystals in the crystallizer, controlling the cooling rate, preventing self-initiated crystals, transferring the crystallization solution into a tripodal centrifuge for centrifugal separation at 12 ℃ for 20min, and obtaining wet microcrystalline monosodium glutamate;
(4) And (3) drying: and (3) putting the wet product microcrystalline monosodium glutamate obtained by separation into a blast drying oven for drying at the temperature of 60 ℃ for 2 hours to obtain the ultrapure microcrystalline monosodium glutamate.
The ultrapure microcrystalline monosodium glutamate prepared by the method is shown in figure 2. Through detection, the yield of the finished product of the sodium glutamate monohydrate prepared by the method can reach 68 percent. The sodium glutamate monohydrate content is detected by a perchloric acid nonaqueous solution titration method, the drying weight loss of the microcrystalline monosodium glutamate is detected by a conventional method, the total moisture is detected by a Karl Fischer method, the crystallinity of the microcrystalline monosodium glutamate is calculated, and screening is carried out by a 40-mesh screen and a 80-mesh screen respectively, so that the particle size distribution is detected.
Example 3
The embodiment provides a production method of ultrapure microcrystalline monosodium glutamate, which comprises the following steps:
(1) Glutamic acid neutralization: adding 1Kg of crude glutamic acid into a 5L reaction kettle, adding a sodium hydroxide solution with the concentration of 25% to dissolve the glutamic acid, stirring while adding the solution, controlling the temperature of the neutralization solution to 50 ℃, monitoring the pH of the neutralization solution on line, and stopping adding the sodium hydroxide solution when the pH reaches 6.8;
(2) And (3) decoloring the neutralization solution: adding special charcoal for flavor essence decolorization into the neutralization solution, wherein the addition amount is 0.3%, the stirring speed is 50rpm, the temperature is 50 ℃ for 30min, filtering by a plate-frame filter after decolorization is finished, circularly beating materials, clarifying, collecting filtrate, and finally obtaining the filtrate with the light transmittance reaching 90%;
(3) Concentrating and crystallizing: transferring the filtered solution into a rotary evaporator for concentration, controlling the water bath temperature to be 60 ℃, concentrating until the concentration of sodium glutamate monohydrate reaches 60% (w/v), and stopping concentrating; pouring the concentrated solution into a crystallizer, slowly starting stirring at 30rpm, introducing cooling water into a jacket for cooling, rapidly cooling in the early stage, cooling to 40 ℃ in 1h, adding 120-mesh seed crystals according to the proportion of 5%, slowly cooling, cooling by 4 ℃ per hour, observing the number and the size of crystals in the crystallizer, controlling the cooling rate, preventing self-initiated crystals, transferring the crystallization solution into a tripodia centrifuge for centrifugal separation at 15 ℃ to obtain wet microcrystalline monosodium glutamate;
(4) And (3) drying: and (3) putting the wet product microcrystalline monosodium glutamate obtained by separation into a blast drying oven for drying at the temperature of 60 ℃ for 1h to obtain the ultrapure microcrystalline monosodium glutamate.
The ultrapure microcrystalline monosodium glutamate prepared by the method is shown in figure 3. Through detection, the yield of the finished product of the sodium glutamate monohydrate prepared by the method can reach 63 percent. The sodium glutamate monohydrate content is detected by a perchloric acid nonaqueous solution titration method, the drying weight loss of the microcrystalline monosodium glutamate is detected by a conventional method, the total moisture is detected by a Karl Fischer method, the crystallinity of the microcrystalline monosodium glutamate is calculated, and screening is carried out by a 40-mesh screen and a 80-mesh screen respectively, so that the particle size distribution is detected.
Example 4
The embodiment provides a production method of ultrapure microcrystalline monosodium glutamate, which comprises the following steps:
(1) Glutamic acid neutralization: adding 1Kg of crude glutamic acid into a 5L reaction kettle, adding a sodium carbonate solution with the concentration of 25% to dissolve glutamic acid, stirring while adding, controlling the temperature of a neutralization solution to 55 ℃, monitoring the pH of the neutralization solution on line, and stopping adding the sodium carbonate solution when the pH reaches 6.5;
(2) And (3) decoloring the neutralization solution: adding special charcoal for flavor essence decolorization into the neutralization solution, wherein the addition amount is 0.5%, the stirring speed is 50rpm, the temperature is 50 ℃ and the time is maintained for 60min, filtering is carried out through a plate-frame filter after decolorization is finished, material beating is circulated, clear liquid is collected after clarification, and finally the light transmittance of the clear liquid reaches 96%;
(3) Concentrating and crystallizing: transferring the filtered solution into a rotary evaporator for concentration, controlling the water bath temperature to be 60 ℃, concentrating until the concentration of sodium glutamate monohydrate reaches 64% (w/v), and stopping concentrating; pouring the concentrated solution into a crystallizer, slowly starting stirring at 30rpm, introducing cooling water into a jacket for cooling, rapidly cooling in the early stage, cooling to 45 ℃ in 1h, adding 100-mesh seed crystals according to the proportion of 5%, slowly cooling, cooling by 3 ℃ per hour, observing the number and the size of crystals in the crystallizer, controlling the cooling rate, preventing self-initiated crystals, transferring the crystallization solution into a tripodal centrifuge for centrifugal separation at 15 ℃ for 12min, and obtaining wet microcrystalline monosodium glutamate;
(4) And (3) drying: and (3) putting the wet product microcrystalline monosodium glutamate obtained by separation into a blast drying oven for drying at 65 ℃ for 1h to obtain the ultrapure microcrystalline monosodium glutamate.
The ultrapure microcrystalline monosodium glutamate prepared by the method is shown in figure 4. Through detection, the yield of the finished product of the sodium glutamate monohydrate prepared by the method can reach 66 percent. The sodium glutamate monohydrate content is detected by a perchloric acid nonaqueous solution titration method, the drying weight loss of the microcrystalline monosodium glutamate is detected by a conventional method, the total moisture is detected by a Karl Fischer method, the crystallinity of the microcrystalline monosodium glutamate is calculated, and screening is carried out by a 40-mesh screen and a 80-mesh screen respectively, so that the particle size distribution is detected.
Example 5
The embodiment provides a production method of ultrapure microcrystalline monosodium glutamate, which comprises the following steps:
(1) Glutamic acid neutralization: adding 1Kg of crude glutamic acid into a 5L reaction kettle, adding 20% sodium hydroxide solution to dissolve glutamic acid, stirring while adding, controlling the temperature of the neutralization solution to 50 ℃, monitoring the pH of the neutralization solution on line, and stopping adding the sodium hydroxide solution when the pH reaches 6.6;
(2) And (3) decoloring the neutralization solution: adding special charcoal for flavor essence decolorization into the neutralization solution, wherein the addition amount is 0.5%, the stirring speed is 50rpm, the temperature is 50 ℃ and is maintained for 40min, filtering is carried out by a plate-frame filter after decolorization is finished, material beating is circulated, clear liquid is collected after clarification, and finally the light transmittance of the clear liquid reaches 95%;
(3) Concentrating and crystallizing: transferring the filtered solution into a rotary evaporator for concentration, controlling the water bath temperature to 65 ℃, and concentrating until the concentration of sodium glutamate monohydrate reaches 62% (w/v) to stop concentrating; pouring the concentrated solution into a crystallizer, slowly starting stirring at 30rpm, introducing cooling water into a jacket for cooling, rapidly cooling in the early stage, cooling to 40 ℃ in 2 hours, adding 100-mesh seed crystals according to the proportion of 7%, slowly cooling, cooling by 5 ℃ per hour, observing the number and the size of crystals in the crystallizer, controlling the cooling rate, preventing self-initiated crystals, transferring the crystallization solution into a tripodal centrifuge for centrifugal separation at 12 ℃ for 15 minutes, and obtaining wet microcrystalline monosodium glutamate;
(4) And (3) drying: and (3) putting the wet product microcrystalline monosodium glutamate obtained by separation into a blast drying oven for drying at the temperature of 60 ℃ for 1h to obtain the ultrapure microcrystalline monosodium glutamate.
The ultrapure microcrystalline monosodium glutamate prepared by the method is shown in figure 5. Through detection, the yield of the finished product of the sodium glutamate monohydrate prepared by the method can reach 63 percent. The sodium glutamate monohydrate content is detected by a perchloric acid nonaqueous solution titration method, the drying weight loss of the microcrystalline monosodium glutamate is detected by a conventional method, the total moisture is detected by a Karl Fischer method, the crystallinity of the microcrystalline monosodium glutamate is calculated, and screening is carried out by a 40-mesh screen and a 80-mesh screen respectively, so that the particle size distribution is detected.
Comparative example 1
The comparative example provides a large-particle monosodium glutamate production method, which comprises the following steps:
(1) Glutamic acid neutralization: adding 1Kg of crude glutamic acid into a 5L reaction kettle, adding 20% sodium hydroxide solution to dissolve glutamic acid, stirring while adding, controlling the temperature of the neutralization solution to 50 ℃, monitoring the pH of the neutralization solution on line, and stopping adding the sodium hydroxide solution when the pH reaches 6.5;
(2) And (3) decoloring the neutralization solution: adding special charcoal for flavor essence decolorization into the neutralization solution, wherein the addition amount is 0.3%, the stirring speed is 50rpm, the temperature is 50 ℃ for 30min, filtering by a plate-frame filter after decolorization is finished, circularly beating materials, clarifying, and then collecting filtrate, wherein the light transmittance of the final filtrate reaches 92.5%;
(3) Concentrating and crystallizing: transferring the filtered solution into a rotary evaporator for concentration, controlling the water bath temperature to be 60 ℃, and concentrating until the concentration of sodium glutamate monohydrate reaches more than 60% (w/v); pouring out half of the concentrated solution for standby, adding 40 mesh seed crystals according to 5% of the residual concentrated solution in the rotary bottle, continuing concentrating, simultaneously feeding the poured concentrated solution at a rate of 100mL/h, observing the size of crystals in the rotary bottle, adding 10-20mL of pure water at 60 ℃ for crystal straightening when tiny crystals appear, stopping concentrating after all the poured concentrated solution is added into the rotary bottle, and transferring the crystallized solution into a tripodia centrifuge for centrifugal separation for 15min to obtain wet flavor essence;
(4) And (3) drying: and (3) putting the wet taste essence obtained by separation into a blast drying oven for drying at the temperature of 103+/-2 ℃ for 2 hours to obtain a monosodium glutamate finished product.
Monosodium glutamate prepared by the method is shown in figure 6. Through detection, the yield of the finished product of the sodium glutamate monohydrate prepared by the method is 52 percent. The sodium glutamate monohydrate content is detected by a perchloric acid nonaqueous solution titration method, the drying weight loss of the large-particle monosodium glutamate is detected by a conventional method, the total moisture is detected by a Karl Fischer method, the crystallinity of the large-particle monosodium glutamate is calculated, and screening is carried out by a screen mesh of 40 meshes and a screen mesh of 80 meshes respectively, so as to determine the particle size distribution.
Comparative example 2
The comparative example provides a powder flavor essence production method, which comprises the following steps:
(1) Glutamic acid neutralization: adding 1Kg of crude glutamic acid into a 5L reaction kettle, adding a sodium carbonate solution with the concentration of 20% to dissolve glutamic acid, stirring while adding, controlling the temperature of a neutralization solution to 50 ℃, monitoring the pH of the neutralization solution on line, and stopping adding the sodium carbonate solution when the pH reaches 6.5;
(2) And (3) decoloring the neutralization solution: adding special charcoal for flavor essence decolorization into the neutralization solution, wherein the addition amount is 0.3%, the stirring speed is 50rpm, the temperature is 50 ℃ for 30min, filtering by a plate-frame filter after decolorization is finished, circularly beating materials, clarifying, and collecting filtrate, wherein the light transmittance of the final filtrate reaches 93%;
(3) Concentrating and crystallizing: transferring the filtered solution into a rotary evaporator for concentration, controlling the water bath temperature to be 60 ℃, concentrating until the concentration of sodium glutamate monohydrate reaches 65% (w/v), and stopping concentrating; pouring the concentrated solution into a crystallizer, slowly starting stirring at 30rpm, introducing cooling water into a jacket for cooling, continuously cooling, cooling to about 15 ℃, and transferring the crystallized solution into a three-legged centrifuge for centrifugal separation for 20min to obtain wet flavor essence;
(4) And (3) drying: and (3) putting the wet taste essence obtained by separation into a blast drying oven for drying at the temperature of 103+/-2 ℃ for 2 hours to obtain a monosodium glutamate finished product.
Monosodium glutamate prepared by the method is shown in figure 7A. Through detection, the yield of the finished product of the sodium glutamate monohydrate prepared by the method is 58 percent. The sodium glutamate monohydrate content is detected by a perchloric acid nonaqueous solution titration method, the weight loss on drying of the powder monosodium glutamate is detected by a conventional method, the total moisture is detected by a Karl Fischer method, the crystallinity of the powder monosodium glutamate is calculated, and screening is carried out by a 40-mesh screen and a 80-mesh screen respectively, so that the particle size distribution is detected.
Comparative example 3
The comparative example provides a production method of monosodium glutamate, which comprises the following steps:
(1) Glutamic acid neutralization: adding 1Kg of crude glutamic acid into a 5L reaction kettle, adding 20% sodium hydroxide solution to dissolve glutamic acid, stirring while adding, controlling the temperature of the neutralization solution to 50 ℃, monitoring the pH of the neutralization solution on line, and stopping adding the sodium hydroxide solution when the pH reaches 6.4;
(2) And (3) decoloring the neutralization solution: adding special charcoal for flavor essence decolorization into the neutralization solution, wherein the addition amount is 0.5%, the stirring speed is 50rpm, the temperature is 50 ℃ and is maintained for 40min, filtering is carried out by a plate-frame filter after decolorization is finished, material beating is circulated, clear liquid is collected after clarification, and finally the light transmittance of the clear liquid reaches 95%;
(3) Concentrating and crystallizing: transferring the filtered solution into a rotary evaporator for concentration, controlling the water bath temperature to be 60 ℃, concentrating until the concentration of sodium glutamate monohydrate reaches 65% (w/v), and stopping concentrating; pouring the concentrated solution into a crystallizer, slowly starting stirring at 30rpm, introducing cooling water into a jacket for cooling, rapidly cooling in the early stage, cooling to 36 ℃ in 2 hours, adding 100-mesh seed crystals according to the proportion of 7%, slowly cooling, cooling by 10 ℃ per hour, observing the number and the size of crystals in the crystallizer, controlling the cooling rate, cooling to 12 ℃ and transferring the crystal solution into a three-legged centrifuge for centrifugal separation for 15 minutes to obtain wet microcrystalline monosodium glutamate;
(4) And (3) drying: and (3) putting the wet product microcrystalline monosodium glutamate obtained by separation into a blast drying oven for drying at the temperature of 60 ℃ for 1h to obtain the ultrapure microcrystalline monosodium glutamate.
The ultrapure microcrystalline monosodium glutamate prepared by the method is shown in figure 8. Through detection, the yield of the finished product of the sodium glutamate monohydrate prepared by the method can reach 60 percent. The sodium glutamate monohydrate content is detected by a perchloric acid nonaqueous solution titration method, the drying weight loss of the microcrystalline monosodium glutamate is detected by a conventional method, the total moisture is detected by a Karl Fischer method, the crystallinity of the microcrystalline monosodium glutamate is calculated, and screening is carried out by a 40-mesh screen and a 80-mesh screen respectively, so that the particle size distribution is detected.
Experimental example 1 detection of the purity, crystallinity and particle size distribution of monosodium glutamate
The monosodium glutamate monohydrate content, the drying weight loss, the total moisture, the crystallinity and the particle size distribution of the monosodium glutamate prepared in each of the above examples and comparative examples are shown in table 1.
TABLE 1
Experimental example 2 solubility detection of monosodium glutamate
The monosodium glutamate prepared by the methods of examples 1-5 and comparative examples 1-3 was analyzed for solubility as follows: 16 beakers of 200mL are taken, 100mL of pure water at 20 ℃ is added into 8 beakers, 100mL of pure water at 50 ℃ is added into the other 8 beakers, the beakers are placed on a magnetic stirrer, a rotor is placed, the rotating speed is adjusted to 100rpm, 25g of monosodium glutamate finished products prepared in examples 1-5 and comparative examples 1-3 are respectively weighed, timing is started after the beakers are added, timing is stopped after monosodium glutamate is completely dissolved, and the time required for complete dissolution of each sample at different temperatures is recorded. The results are shown in Table 2.
TABLE 2
Experimental example 3 storage stability test of monosodium glutamate
The monosodium glutamate prepared by the methods of examples 1-5 and comparative examples 1-3 was analyzed for storage stability as follows: 100g of the monosodium glutamate finished products prepared in examples 1-5 and comparative examples 1-3 were weighed respectively, placed in a beaker, left open for 1 week at room temperature of 25 ℃ and relative humidity of 40%, and then observed for caking. The results are shown in Table 3, wherein the monosodium glutamate agglomerates of comparative example 2 are shown in FIG. 7B.
TABLE 3 Table 3
While the invention has been described in detail in the foregoing general description and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that modifications and improvements can be made thereto. Accordingly, such modifications or improvements may be made without departing from the spirit of the invention and are intended to be within the scope of the invention as claimed.
Claims (10)
1. The preparation method of the microcrystalline monosodium glutamate is characterized by comprising the following steps: evaporating and concentrating the sodium glutamate solution to supersaturated concentration to obtain sodium glutamate concentrated solution, rapidly cooling the sodium glutamate concentrated solution to 40-50 ℃ through first cooling treatment, adding seed crystal, and then performing second cooling treatment to generate sodium glutamate crystals;
wherein the second cooling treatment is gradient cooling.
2. The method for preparing microcrystalline monosodium glutamate according to claim 1, wherein the gradient cooling rate is 3-5 ℃/h.
3. The method for preparing microcrystalline monosodium glutamate according to claim 2, wherein the second cooling treatment is ended when the temperature is reduced to 12-15 ℃.
4. The method for preparing microcrystalline monosodium glutamate according to claim 1, wherein the first cooling treatment is to cool to 40-50 ℃ within 1-2 hours.
5. The method for producing a microcrystalline monosodium glutamate according to any one of claims 1 to 4, wherein the average particle size of the seed crystals is 100 to 120 mesh;
preferably, the seed crystal is added in an amount of 4-8%.
6. The method for preparing microcrystalline monosodium glutamate according to any one of claims 1 to 4, wherein the concentration of monosodium glutamate monohydrate in the sodium glutamate concentrate is 60-65%;
preferably, the temperature of the evaporative concentration is 55-65 ℃.
7. The method for preparing microcrystalline monosodium glutamate according to any one of claims 3 to 6, wherein after the second cooling treatment, separating the crystallization liquid to obtain wet microcrystalline monosodium glutamate, and drying the wet microcrystalline monosodium glutamate until the total moisture content is 9-10%;
preferably, the drying temperature is 60-65 ℃ and the drying time is 1-2h.
8. The method for preparing microcrystalline monosodium glutamate according to any one of claims 1 to 7, wherein the sodium glutamate solution is prepared by taking beta-glutamic acid as a raw material, neutralizing with sodium hydroxide or sodium salt, and then decoloring and filtering.
9. The microcrystalline monosodium glutamate prepared by the preparation method of microcrystalline monosodium glutamate according to any one of claims 1 to 8;
preferably, the grain size distribution of the microcrystalline monosodium glutamate is more than 90% of the grain with the particle size distribution of 40-80 meshes; more preferably, the particle size distribution is above 95% of the particles with 40-80 mesh size; the purity of the microcrystalline monosodium glutamate is more than or equal to 99.0 percent.
10. Use of the microcrystalline monosodium glutamate of claim 9 in the preparation of a food product.
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| CN (1) | CN116649557A (en) |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107602405A (en) * | 2017-09-26 | 2018-01-19 | 侯马高知新生物科技有限公司 | A kind of method of sodium glutamate crystal grain increase |
| CN108997159A (en) * | 2018-07-17 | 2018-12-14 | 廊坊梅花生物技术开发有限公司 | A kind of preparation method of L-Glutamine |
| CN109438274A (en) * | 2018-11-19 | 2019-03-08 | 廊坊梅花生物技术开发有限公司 | The method of glutamine is recycled from the thick mother liquor of glutamine |
| CN111187178A (en) * | 2020-01-13 | 2020-05-22 | 廊坊梅花生物技术开发有限公司 | Process for producing glutamine crystal |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107602405A (en) * | 2017-09-26 | 2018-01-19 | 侯马高知新生物科技有限公司 | A kind of method of sodium glutamate crystal grain increase |
| CN108997159A (en) * | 2018-07-17 | 2018-12-14 | 廊坊梅花生物技术开发有限公司 | A kind of preparation method of L-Glutamine |
| CN109438274A (en) * | 2018-11-19 | 2019-03-08 | 廊坊梅花生物技术开发有限公司 | The method of glutamine is recycled from the thick mother liquor of glutamine |
| CN111187178A (en) * | 2020-01-13 | 2020-05-22 | 廊坊梅花生物技术开发有限公司 | Process for producing glutamine crystal |
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