CN109077289A - The method that anion exchange resin regenerated liquid recycles production monosodium glutamate - Google Patents

The method that anion exchange resin regenerated liquid recycles production monosodium glutamate Download PDF

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Publication number
CN109077289A
CN109077289A CN201810768602.XA CN201810768602A CN109077289A CN 109077289 A CN109077289 A CN 109077289A CN 201810768602 A CN201810768602 A CN 201810768602A CN 109077289 A CN109077289 A CN 109077289A
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Prior art keywords
anion exchange
exchange resin
monosodium glutamate
regeneration
mother solution
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冯文清
林琳
赵伟恩
伍钧
刘志坚
苏丽敏
王景林
黄东江
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Guangzhou Aosang Monosodium Glutamate Food Co Ltd
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Guangzhou Aosang Monosodium Glutamate Food Co Ltd
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Priority to CN201810768602.XA priority Critical patent/CN109077289A/en
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    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23LFOODS, 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
    • A23L27/00Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
    • A23L27/20Synthetic spices, flavouring agents or condiments
    • A23L27/21Synthetic spices, flavouring agents or condiments containing amino acids
    • A23L27/22Synthetic spices, flavouring agents or condiments containing amino acids containing glutamic acids
    • AHUMAN NECESSITIES
    • A23FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
    • A23VINDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
    • A23V2002/00Food compositions, function of food ingredients or processes for food or foodstuffs

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  • Life Sciences & Earth Sciences (AREA)
  • Proteomics, Peptides & Aminoacids (AREA)
  • Health & Medical Sciences (AREA)
  • Nutrition Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Food Science & Technology (AREA)
  • Polymers & Plastics (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention discloses a kind of methods that anion exchange resin regenerated liquid recycles production monosodium glutamate.A method of production monosodium glutamate is recycled by the anion exchange resin regenerated liquid of raw material of glutamic acid, comprising the following steps: 1) glutamic acid neutralizes;2) powder activity carbon decoloring, filtering;3) it collects anion exchange resin regeneration outflow salt hydrolysis imbibition, powder activity carbon decoloring, filtering is added;4) filtrate adds refined salt and food-grade caustic soda, filtrate constant volume, anion exchange resin regeneration;5) destainer is neutralized through anion exchange resin secondary decolourization;6) crystal product.Also disclose a kind of method that production monosodium glutamate is recycled as the anion exchange resin regenerated liquid of raw material using monosodium glutamate crystalline mother solution.The present invention has positive meaning to the regeneration cost for reducing macroporous strong-base anion exchange resin regeneration technology and the cycle-index for increasing regenerated liquid.

Description

The method that anion exchange resin regenerated liquid recycles production monosodium glutamate
Technical field
The present invention relates to the methods that anion exchange resin regenerated liquid recycles production monosodium glutamate.
Background technique
The ingredient of monosodium glutamate is sodium glutamate.Glutamic acid is one of 20 kinds of amino acid of constitutive protein matter, as long as containing in food There is protein, just contains glutamic acid.The glutamic acid (glutamate anion) of free state be prevalent in conventional food (such as: Mushroom, kelp, tomato, nut, beans, meat), it is a kind of product of natural metabolism in human body.Glutamate stimulates tongue The umami receptor of upper taste bud, makes people feel delicious flavour.The high food of delicate flavour is much content of glutamic acid food abundant.
The mankind eat existing more than 100 years history of monosodium glutamate, and as a kind of most widely used fresh adding flavouring, monosodium glutamate is day So safe and healthy fresh adding flavouring.Modern society, monosodium glutamate are widely used in family and restaurant culinary art, make an addition to various sides extensively Just in the products such as food, cooked meat product, soy sauce, sauce, even more chickens' extract and the most basic raw material of various compound seasoners.It is global every Year consumption monosodium glutamate is a kind of most widely used freshener ten thousand tons about more than 300.
China's glutamate production is with a long history, and is glutamate production and consumption big country, and annual output has broken through 2,000,000 tons.Monosodium glutamate It is through microorganism (Corynebacterium glutamicum) fermentation, to be extracted, neutralization, refined sodium glutamate using cereal such as corns as raw material Content is equal to or more than 99.0%, particle or powder with special delicate flavour.Glutamate production is to carry out deep processing to agricultural product High-tech industry.But macroporous strong-base anion exchange resin is according to the resin regeneration (10%NaCl+0.2%NaOH) of preparation method The preparation method of saline solution, pressure is very big under the increasingly severeer overall situation of current Environmental Protection Situation, how to reduce and is produced into Originally, reducing quantity of wastewater effluent can guarantee that resin decolorization effect becomes the Important Problems studied in production of gourmet powder again.
Summary of the invention
The present invention is by providing anion exchange resin regeneration to the production technology for improving existing glutamic acid manufacture monosodium glutamate The method that liquid recycles production monosodium glutamate.
The technical solution used in the present invention is:
A method of it is recycled using glutamic acid as the anion exchange resin regenerated liquid of raw material and produces monosodium glutamate, including with Lower step:
1) glutamic acid neutralizes: glutamic acid, edible soda ash and water being mixed and neutralized, control pH value is 6.5~7.4, neutralizes temperature Degree is 60 DEG C~65 DEG C, the Baume degrees >=23 ° B é of neutralizer;
2) powder activity carbon decoloring, filtering: Powdered Activated Carbon, stirring decoloration, mistake is added in the neutralizer obtained to step 1) Filter obtains neutralizing destainer;
3) it collects anion exchange resin regeneration outflow salt hydrolysis imbibition, powder activity carbon decoloring, filtering: recycling yin is added Ion exchange resin regeneration flows out salt water stripping liquid, and Powdered Activated Carbon, stirring decoloration is added, and filtering obtains resin regeneration filtrate;
4) filtrate adds refined salt and food-grade caustic soda, filtrate constant volume, anion exchange resin regeneration: step 3) is obtained The mass concentration that resin regeneration filtrate adds edible refined salt to NaCl is 9%~12%, adds the matter of food-grade caustic soda to NaOH Measuring concentration is 0.18%~0.22%, then by filtrate constant volume, is regenerated anion exchange resin with filtrate;
5) destainer is neutralized through anion exchange resin secondary decolourization: 40 DEG C~45 DEG C steps 2) being obtained into glutamic acid and are neutralized Destainer is with 2.5m3/ h~3m3/ h flow velocity passes through the exchange column of anion exchange resin, the white brilliant liquid after obtaining upper prop;
6) crystal product: the white brilliant liquid that step 5) is obtained is crystallized, separation, dry, obtains crystal gourmet powder product.
Using glutamic acid as in the step 2) of feedstock production process, the quality of Powdered Activated Carbon accounts for the 0.5% of neutralizer volume ~1.5%;The time of stirring decoloration is 45 minutes~60 minutes;It obtains neutralizing decolorizing liquid rate >=94%.
Using glutamic acid as in the step 3) of feedstock production process, the quality of Powdered Activated Carbon accounts for resin regeneration outflow salt hydrolysis The 0.2%~0.3% of imbibition volume;Stirring decoloration be temperature be 60 DEG C~65 DEG C at decolourize 45 minutes~60 minutes.
Using glutamic acid as white brilliant liquid light transmittance >=98% that in the step 5) of feedstock production process, obtains.
Using glutamic acid as in the step 5) of feedstock production process, the diameter of exchange column is 1m~1.5m, a height of 3m~4m, yin The volume fraction that ion exchange resin accounts for exchange column is 50%~80%.
A method of production monosodium glutamate being recycled by the anion exchange resin regenerated liquid of raw material of monosodium glutamate crystalline mother solution, The following steps are included:
1) monosodium glutamate crystalline mother solution adjusts: it is 7.6~7.7 that monosodium glutamate crystalline mother solution glutamic acid, which is adjusted pH value, then uses water The Baume degrees for adjusting mother liquor is 24.5 ° of é~25.5 ° B B é;
2) powder activity carbon decoloring, filtering: Powdered Activated Carbon is added in the crystalline mother solution that step 1) adjustment obtains, stirring is de- Color, filtering, obtains crystalline mother solution destainer;
3) it collects anion exchange resin regeneration outflow salt hydrolysis imbibition, powder activity carbon decoloring, filtering: recycling yin is added Ion exchange resin regeneration flows out salt water stripping liquid, and Powdered Activated Carbon, stirring decoloration is added, and filtering obtains resin regeneration filtrate;
4) filtrate adds refined salt and food-grade caustic soda, filtrate constant volume, anion exchange resin regeneration: step 3) is obtained The mass concentration that resin regeneration filtrate adds edible refined salt to NaCl is 9%~12%, adds the matter of food-grade caustic soda to NaOH Measuring concentration is 0.18%~0.22%, then by filtrate constant volume, is regenerated anion exchange resin with filtrate;
5) crystalline mother solution destainer is through anion exchange resin secondary decolourization: it is female that 45 DEG C~50 DEG C steps 2) are obtained crystallization Liquid destainer is with 2.0m3/ h~2.5m3/ h flow velocity passes through the exchange column of anion exchange resin, the crystalline mother solution after obtaining upper prop Secondary decolourization liquid;
6) crystal product: the crystalline mother solution secondary decolourization liquid that step 5) is obtained is crystallized, separates, is dry, obtains crystal Msg product.
Using monosodium glutamate crystalline mother solution as in the step 2) of feedstock production process, the quality of Powdered Activated Carbon accounts for neutralizer volume 0.3%~0.4%;Obtain crystalline mother solution decolorizing liquid rate >=70%.
Using monosodium glutamate crystalline mother solution as in the step 3) of feedstock production process, the quality of Powdered Activated Carbon accounts for resin regeneration outflow The 0.2%~0.3% of salt water stripping liquid volume;Stirring decoloration be temperature be 60 DEG C~65 DEG C at decolourize 45 minutes~60 points Clock.
Using monosodium glutamate crystalline mother solution as in the step 3) of feedstock production process, the quality of Powdered Activated Carbon accounts for resin regeneration outflow The 0.2%~0.3% of salt water stripping liquid volume;Stirring decoloration be temperature be 60 DEG C~65 DEG C at decolourize 45 minutes~60 points Clock.
Using monosodium glutamate crystalline mother solution as the crystalline mother solution secondary decolourization liquid light transmittance that in the step 5) of feedstock production process, obtains >=80%.
Using monosodium glutamate crystalline mother solution as in the step 5) of feedstock production process, the diameter of exchange column is 1m~1.5m, a height of 3m ~4m, the volume fraction that anion exchange resin accounts for exchange column is 50%~80%.
Anion exchange resin is macroporous strong-base type styrene series anion exchange resin.
Further, anion exchange resin is the AMBERLITETM FPA90Cl resin of Tao Shi.
The beneficial effects of the present invention are:
The present invention is to the regeneration cost for reducing macroporous strong-base anion exchange resin regeneration technology and increases following for regenerated liquid Ring number has positive meaning.
Specific feature is as follows:
1, the present invention compares the direct preparation method of Tao Shi macroporous strong-base anion exchange resin regenerated liquid, light transmittance with again The method that raw liquid does not recycle is not much different;2, the present invention Tao Shi macroporous strong-base anion exchange resin regenerated liquid that compares directly is matched Method processed, light transmittance are not much different with the method that regenerated liquid does not recycle;3, the present invention can reduce regeneration cost 32.9%;4, originally The regenerated liquid cycle-index of invention can achieve 10 times;5, method of the invention can be in the production of existing glutamic acid manufacture monosodium glutamate Directly implement on line.
Specific embodiment
A method of it is recycled using glutamic acid as the anion exchange resin regenerated liquid of raw material and produces monosodium glutamate, including with Lower step:
1) glutamic acid neutralizes: glutamic acid, edible soda ash and water being mixed and neutralized, control pH value is 6.5~7.4, neutralizes temperature Degree is 60 DEG C~65 DEG C, the Baume degrees >=23 ° B é of neutralizer;
2) powder activity carbon decoloring, filtering: Powdered Activated Carbon, stirring decoloration, mistake is added in the neutralizer obtained to step 1) Filter obtains neutralizing destainer;
3) it collects anion exchange resin regeneration outflow salt hydrolysis imbibition, powder activity carbon decoloring, filtering: recycling yin is added Ion exchange resin regeneration flows out salt water stripping liquid, and Powdered Activated Carbon, stirring decoloration is added, and filtering obtains resin regeneration filtrate;
4) filtrate adds refined salt and food-grade caustic soda, filtrate constant volume, anion exchange resin regeneration: step 3) is obtained The mass concentration that resin regeneration filtrate adds edible refined salt to NaCl is 9%~12%, adds the matter of food-grade caustic soda to NaOH Measuring concentration is 0.18%~0.22%, then by filtrate constant volume, is regenerated anion exchange resin with filtrate;
5) destainer is neutralized through anion exchange resin secondary decolourization: 40 DEG C~45 DEG C steps 2) being obtained into glutamic acid and are neutralized Destainer is with 2.5m3/ h~3m3/ h flow velocity passes through the exchange column of anion exchange resin, the white brilliant liquid after obtaining upper prop;
6) crystal product: the white brilliant liquid that step 5) is obtained is crystallized, separation, dry, obtains crystal gourmet powder product.
Preferably, using glutamic acid as in the step 1) of feedstock production process, the Baume degrees of neutralizer is 25 ° of B é.
Preferably, using glutamic acid as in the step 2) of feedstock production process, the quality of Powdered Activated Carbon accounts for neutralizer volume 0.5%~1.5% (W/V).
It preferably, is 45 minutes~60 points by the time in the step 2) of feedstock production process, stirring decoloration of glutamic acid Clock.
Preferably, decolorizing liquid rate >=94% is neutralized using glutamic acid to obtain in the step 2) of feedstock production process.
Preferably, using glutamic acid as in the step 3) of feedstock production process, the quality of Powdered Activated Carbon accounts for resin regeneration stream 0.2%~0.3% (W/V) of salt water stripping liquid volume out;It is further preferred that the step of using glutamic acid as feedstock production process 3) in, the quality of Powdered Activated Carbon accounts for 0.25% (W/V) of resin regeneration outflow salt water stripping liquid volume.
Preferably, using glutamic acid as in the step 3) of feedstock production process, it is 60 DEG C~65 DEG C that stirring decoloration, which is in temperature, Lower decoloration 45 minutes~60 minutes.
Preferably, using glutamic acid in the step 2) of feedstock production process or step 3), to be filtered into plate and frame filter press filtering.
Preferably, it is mended by the resin regeneration filtrate that in the step 4) of feedstock production process, step 3) is obtained of glutamic acid The mass concentration (W/W) for adding edible refined salt to NaCl is 10%, and the mass concentration (W/W) for adding food-grade caustic soda to NaOH is 0.2%.
Preferably, using glutamic acid as in the step 4) of feedstock production process, filtrate is settled to 11m3~13m3;Further Preferably, using glutamic acid as in the step 4) of feedstock production process, filtrate is settled to 12m3
Preferably, using glutamic acid as white brilliant liquid light transmittance >=98% that in the step 5) of feedstock production process, obtains.
Preferably, using glutamic acid as in the step 5) of feedstock production process, the diameter of exchange column is 1m~1.5m, a height of 3m ~4m, the volume fraction that anion exchange resin accounts for exchange column is 50%~80%;It is further preferred that using glutamic acid as raw material In the step 5) of production method, the diameter of exchange column is 1.2m, a height of 3.5m, and exchange column is provided with 2m3~3m3Anion hand over Change resin;Still further preferably, using glutamic acid as in the step 5) of feedstock production process, exchange column is provided with 2.5m3Yin Ion exchange resin.
Further, using glutamic acid as in the step 6) of feedstock production process, crystallization, separation are specially to pass through white brilliant liquid Vacuum concentration crystallizes monosodium glutamate, using centrifuge separation.
A method of production monosodium glutamate being recycled by the anion exchange resin regenerated liquid of raw material of monosodium glutamate crystalline mother solution, The following steps are included:
1) monosodium glutamate crystalline mother solution adjusts: it is 7.6~7.7 that monosodium glutamate crystalline mother solution glutamic acid, which is adjusted pH value, then uses water The Baume degrees for adjusting mother liquor is 24.5 ° of é~25.5 ° B B é;
2) powder activity carbon decoloring, filtering: Powdered Activated Carbon is added in the crystalline mother solution that step 1) adjustment obtains, stirring is de- Color, filtering, obtains crystalline mother solution destainer;
3) it collects anion exchange resin regeneration outflow salt hydrolysis imbibition, powder activity carbon decoloring, filtering: recycling yin is added Ion exchange resin regeneration flows out salt water stripping liquid, and Powdered Activated Carbon, stirring decoloration is added, and filtering obtains resin regeneration filtrate;
4) filtrate adds refined salt and food-grade caustic soda, filtrate constant volume, anion exchange resin regeneration: step 3) is obtained The mass concentration that resin regeneration filtrate adds edible refined salt to NaCl is 9%~12%, adds the matter of food-grade caustic soda to NaOH Measuring concentration is 0.18%~0.22%, then by filtrate constant volume, is regenerated anion exchange resin with filtrate;
5) crystalline mother solution destainer is through anion exchange resin secondary decolourization: it is female that 45 DEG C~50 DEG C steps 2) are obtained crystallization Liquid destainer is with 2.0m3/ h~2.5m3/ h flow velocity passes through the exchange column of anion exchange resin, the crystalline mother solution after obtaining upper prop Secondary decolourization liquid;
6) crystal product: the crystalline mother solution secondary decolourization liquid that step 5) is obtained is crystallized, separates, is dry, obtains crystal Msg product.
Preferably, using monosodium glutamate crystalline mother solution as in the step 1) of feedstock production process, monosodium glutamate crystalline mother solution is by monosodium glutamate knot Monosodium glutamate crystalline mother solution brilliant, obtained after separation, as using glutamic acid to pass through white brilliant liquid described in the step 6) of feedstock production process Crystallization, monosodium glutamate crystalline mother solution obtained after separation.
Preferably, using monosodium glutamate crystalline mother solution to be with the Baume degrees that water adjusts mother liquor in the step 1) of feedstock production process 25°Bé。
Preferably, using monosodium glutamate crystalline mother solution as in the step 2) of feedstock production process, the quality of Powdered Activated Carbon accounts for neutralization 0.3%~0.4% (W/V) of liquid product.
Preferably, it is no less than 60 minutes using monosodium glutamate crystalline mother solution in the step 2) of production method, to stir the time of decoloration.
Preferably, using monosodium glutamate crystalline mother solution in the step 2) of feedstock production process, to obtain crystalline mother solution decolorizing liquid Rate >=70%.
Preferably, using monosodium glutamate crystalline mother solution as in the step 3) of feedstock production process, the quality of Powdered Activated Carbon accounts for resin 0.2%~0.3% (W/V) of regeneration outflow salt hydrolysis imbibition volume.
Preferably, using monosodium glutamate crystalline mother solution as in the step 3) of feedstock production process, it is 60 DEG C that stirring decoloration, which is in temperature, It decolourizes 45 minutes~60 minutes at~65 DEG C.
Preferably, using monosodium glutamate crystalline mother solution to be filtered into plate compression in the step 2) of feedstock production process or step 3) Machine filtering.
Preferably, using monosodium glutamate crystalline mother solution as resin regeneration that in the step 4) of feedstock production process, step 3) is obtained The mass concentration (W/W) that filtrate adds edible refined salt to NaCl is 10%, adds the mass concentration (W/ of food-grade caustic soda to NaOH It W) is 0.2%.
Preferably, using monosodium glutamate crystalline mother solution as in the step 4) of feedstock production process, filtrate is settled to 11m3~13m3; It is further preferred that using monosodium glutamate crystalline mother solution as in the step 4) of feedstock production process, filtrate is settled to 12m3
Preferably, using monosodium glutamate crystalline mother solution as the crystalline mother solution secondary decolourization that in the step 5) of feedstock production process, obtains Liquid light transmittance >=80%.
Preferably, using monosodium glutamate crystalline mother solution as in the step 5) of feedstock production process, the diameter of exchange column is 1m~1.5m, A height of 3m~4m, the volume fraction that anion exchange resin accounts for exchange column is 50%~80%;It is further preferred that with monosodium glutamate knot Brilliant mother liquor is in the step 5) of feedstock production process, and the diameter of exchange column is 1.2m, a height of 3.5m, and exchange column is provided with 2m3~ 3m3Anion exchange resin;Still further preferably, using monosodium glutamate crystalline mother solution to hand in the step 5) of feedstock production process It changes column and is provided with 2.5m3Anion exchange resin.
Further, using monosodium glutamate crystalline mother solution as in the step 6) of feedstock production process, crystallization, separation are specially will crystallization Mother liquor secondary decolourization liquid crystallizes monosodium glutamate by vacuum concentration, using centrifuge separation.
Preferably, anion exchange resin is macroporous strong-base type styrene series anion exchange resin.
It is further preferred that anion exchange resin is the AMBERLITETM FPA90Cl resin of Tao Shi.
It is exemplified below using the specific technological process of production that glutamic acid manufactures monosodium glutamate as raw material:
Glutamic acid, edible soda ash, tap water → glutamic acid neutralization → powder activity carbon decoloring → filtering → neutralization destainer The regeneration outflow salt hydrolysis imbibition → collection → addition powder activity carbon decoloring → filtering → collection → filter of → large pore anion resin Liquid adds that refined salt to NaCl (W/W) score is 10%, to mend food-grade caustic soda to NaOH (W/W) score be 0.2% → filtrate constant volume White crystalline substance liquid → monosodium glutamate crystallization → monosodium glutamate after → large pore anion resin regeneration → large pore anion resin column secondary decolourization → upper prop Dry → first packing → inspection of separation → monosodium glutamate → monosodium glutamate packaging.
It is exemplified below using the specific technological process of production that monosodium glutamate crystalline mother solution manufactures monosodium glutamate as raw material:
Monosodium glutamate crystalline mother solution → powder activity carbon decoloring → filtering → crystalline mother solution destainer → large pore anion resin is again Raw outflow salt water stripping liquid → collection → addition powder activity carbon decoloring → filtering → collection → filtrate adds refined salt to NaCl (W/ W) score is 10%, to mend food-grade caustic soda to NaOH (W/W) be 0.2% → filtrate constant volume → large pore anion resin regeneration → greatly Crystalline mother solution secondary decolourization liquid → monosodium glutamate crystallization → monosodium glutamate separation → monosodium glutamate is dry after hole resin anion (R.A.) column secondary decolourization → upper prop Dry → first packing → inspection → monosodium glutamate packaging.
The contents of the present invention are described in further detail below by way of specific embodiment.
Resin mentioned in Examples 1 to 4 is the macroporous type strong alkali anion of Dow Rhom and Hass production Exchanger resin AMBERLITETM FPA90Cl.Raw material or method used in remaining are the routine of this field unless otherwise specified Raw material or method.
Embodiment 1:
(1) glutamic acid neutralizes: a small amount of tap water is added in glutamic acid neutralizing tank, opens stirring, 4 tons of glutamic acid are slow Pouring into neutralizing tank, then constantly addition edible soda ash is neutralized, and neutralizer is settled to 10m with tap water3.Neutralization temperature is 60 DEG C~63 DEG C, it is 6.5~7.0 that pH value is controlled in N-process, 25 ° of B é of Baume degrees of neutralizer.
(2) powder activity carbon decoloring, filtering: by 10m3Neutralizer be added 100kg Powdered Activated Carbon, stirring decoloration 60 points Then clock carries out filters pressing with flame filter press, obtain the neutralization destainer of light transmittance 95%.
(3) it collects Tao Shi large pore anion resin regeneration outflow salt hydrolysis imbibition, powder activity carbon decoloring, filtering is added: Recycling Tao Shi large pore anion resin regeneration outflow salt hydrolysis imbibition is added the stirring of 0.25% (W/V) Powdered Activated Carbon and is warming up to 60 DEG C~65 DEG C decolourize 45 minutes, resin regeneration filtrate is obtained by filtration through plate and frame filter press.
(4) filtrate adds refined salt and food-grade caustic soda, filtrate constant volume, the regeneration of Tao Shi large pore anion resin: regeneration filtrate Add edible refined salt to NaCl (W/W) be 10% and add food-grade caustic soda to NaOH (W/W) be 0.2%, then by filtrate constant volume To 12m3, the regeneration of Tao Shi macroporous strong-base anion exchange resin.
(5) it neutralizes destainer to decolourize through Tao Shi large pore anion resin column: being in 45 DEG C of glutamic acid and destainer by temperature With 2.5m3/ h flow velocity is equipped with 2.5m by Φ 1.2m × 3.5m3The exchange column of macroporous strong-base anion exchange resin, obtains upper prop White brilliant liquid afterwards, white crystalline substance liquid light transmission detects once per hour, and detecting instrument is white during upper prop using 722-S spectrophotometer Brilliant liquid light transmittance needs to keep >=98%.As white brilliant liquid light transmittance < 98%, then stops neutralizing destainer upper prop, prepare resin column again It is raw.
The regeneration of Tao Shi resin: the stirring of 0.25% (W/V) Powdered Activated Carbon is added to recycling resin regeneration outflow stripping liquid It is warming up to 60 DEG C~65 DEG C to decolourize 45 minutes, resin regeneration filtrate is obtained by filtration through plate and frame filter press, then regeneration filtrate is added Edible refined salt to NaCl (W/W) is 10% and adds food-grade caustic soda to NaOH (W/W) to be 0.2%, then filtrate is settled to 12m3, impregnate 2 hours, be then washed till efflux pH value 7.5, efflux light transmittance >=98% with tap water is suitable, then use tap water Backwash, which pulls loose, to be put back into.
(6) according to the general production technology of concentrated crystallization, white crystalline substance liquid is separated by monosodium glutamate crystallization, monosodium glutamate, monosodium glutamate is dry, Obtain crystal gourmet powder product.
Recycling regeneration according to new process 5 Tao Shi macroporous strong-base anion exchange resin regenerated liquids of progress can reach To the production requirement for neutralizing decolorizing liquid rate >=98%.
The light transmittance of 1 upper prop of embodiment decoloration front and back can be shown in Table 1.
The light transmittance of 1 embodiment of table, 1 upper prop decoloration front and back
Embodiment 2:
(1) glutamic acid neutralizes: a small amount of tap water is added in glutamic acid neutralizing tank, opens stirring, 4 tons of glutamic acid are slow Pouring into neutralizing tank, then constantly addition edible soda ash is neutralized, and neutralizer is settled to 10m with tap water3.Neutralization temperature is 62 DEG C~65 DEG C, it is 7.0~7.4 that pH value is controlled in N-process, 25 ° of B é of Baume degrees of neutralizer.
(2) powder activity carbon decoloring, filtering: by 10m3Neutralizer be added 100kg Powdered Activated Carbon, stirring decoloration 60 points Then clock carries out filters pressing with flame filter press, obtain the neutralization destainer of light transmittance 95%.
(3) it collects Tao Shi large pore anion resin regeneration outflow salt hydrolysis imbibition, powder activity carbon decoloring, filtering is added: Recycling Tao Shi large pore anion resin regeneration outflow salt hydrolysis imbibition is added the stirring of 0.25% (W/V) Powdered Activated Carbon and is warming up to 60 DEG C~65 DEG C decolourize 45 minutes, resin regeneration filtrate is obtained by filtration through plate and frame filter press.
(4) filtrate adds refined salt and food-grade caustic soda, filtrate constant volume, the regeneration of Tao Shi large pore anion resin: regeneration filtrate Add edible refined salt to NaCl (W/W) be 10% and add food-grade caustic soda to NaOH (W/W) be 0.2%, then by filtrate constant volume To 12m3, the regeneration of Tao Shi macroporous strong-base anion exchange resin.
(5) it neutralizes destainer to decolourize through Tao Shi large pore anion resin column: being in 45 DEG C of glutamic acid and destainer by temperature With 2.8m3/ h flow velocity is equipped with 2.5m by Φ 1.2m × 3.5m3The exchange column of macroporous strong-base anion exchange resin, obtains upper prop White brilliant liquid afterwards, white crystalline substance liquid light transmission detects once per hour, and detecting instrument is white during upper prop using 722-S spectrophotometer Brilliant liquid light transmittance needs to keep >=98%.As white brilliant liquid light transmittance < 98%, then stops neutralizing destainer upper prop, prepare resin column again It is raw.
The regeneration of Tao Shi resin: the stirring of 0.25% (W/V) Powdered Activated Carbon is added to recycling resin regeneration outflow stripping liquid It is warming up to 60 DEG C~65 DEG C to decolourize 45 minutes, resin regeneration filtrate is obtained by filtration through plate and frame filter press, then regeneration filtrate is added Edible refined salt to NaCl (W/W) is 10% and adds food-grade caustic soda to NaOH (W/W) to be 0.2%, then filtrate is settled to 12m3, impregnate 2 hours, be then washed till efflux pH value 7.5, efflux light transmittance >=98% with tap water is suitable, then use tap water Backwash, which pulls loose, to be put back into.
(6) according to the general production technology of concentrated crystallization, white crystalline substance liquid is separated by monosodium glutamate crystallization, monosodium glutamate, monosodium glutamate is dry, Obtain crystal gourmet powder product.
Regeneration is recycled according to new process 10 Tao Shi macroporous strong-base anion exchange resin regenerated liquids of progress to be ok Reach production requirement, but in cannot reach for 11 times and the production requirement of decolorizing liquid rate >=98%.
The light transmittance of 2 upper prop of embodiment decoloration front and back can be shown in Table 2.
The light transmittance of 2 embodiment of table, 2 upper prop decoloration front and back
Project Light transmittance (%) before upper prop decolourizes Light transmittance (%) after upper prop decoloration
It recycles for 1st time 96.3 100
It recycles for 2nd time 95.5 100
It recycles for 3rd time 95.8 100
The 4th recycles 95.3 100
The 5th recycles 96.0 100
It recycles for 6th time 96.5 100
It recycles for 7th time 95.1 99
It recycles for 8th time 95.3 99
It recycles for 9th time 95.2 98
It recycles for 10th time 95.3 98
It recycles for 11st time 95.5 97
Embodiment 3:
(1) crystalline mother solution: being adjusted to pH value 7.6 with a small amount of glutamic acid for the sodium glutamate mother liquid that centrifuge separates, then with certainly The Baume degrees that water adjusts crystalline mother solution is 25 ° of B é.
(2) 0.3% (W/V) powder powder activity carbon decoloring, filtering: is added in the crystalline mother solution for adjusting pH value and Baume degrees Last active carbon stirring decoloration 60 minutes or more, carries out filters pressing with flame filter press, obtains the crystalline mother solution decoloration of light transmittance 75% Liquid.
(3) it collects Tao Shi large pore anion resin regeneration outflow salt hydrolysis imbibition, powder activity carbon decoloring, filtering is added: Recycling Tao Shi large pore anion resin regeneration outflow salt hydrolysis imbibition is added the stirring of 0.25% (W/V) Powdered Activated Carbon and is warming up to 60 DEG C~65 DEG C decolourize 45 minutes, resin regeneration filtrate is obtained by filtration through plate and frame filter press.
(4) filtrate adds refined salt and food-grade caustic soda, filtrate constant volume, the regeneration of Tao Shi large pore anion resin: regeneration filtrate Add edible refined salt to NaCl (W/W) be 10% and add food-grade caustic soda to NaOH (W/W) be 0.2%, then by filtrate constant volume To 12m3, the regeneration of Tao Shi macroporous strong-base anion exchange resin.
The regeneration of Tao Shi resin: the stirring of 0.25% (W/V) Powdered Activated Carbon is added to recycling resin regeneration outflow stripping liquid It is warming up to 60 DEG C~65 DEG C to decolourize 45 minutes, resin regeneration filtrate is obtained by filtration through plate and frame filter press, then regeneration filtrate is added Edible refined salt to NaCl (W/W) is 10% and adds food-grade caustic soda to NaOH (W/W) to be 0.2%, then filtrate is settled to 12m3, impregnate 2 hours, be then washed till efflux pH value 7.5, efflux light transmittance >=98% with tap water is suitable, then use tap water Backwash, which pulls loose, to be put back into.
(5) crystalline mother solution destainer is through Tao Shi large pore anion resin column secondary decolourization: by 50 DEG C of crystalline mother solution destainers With 2.5m3/ h flow velocity is equipped with 2.5m by Φ 1.2m × 3.5m3The exchange column of macroporous strong-base anion exchange resin, obtains upper prop Crystalline mother solution secondary decolourization liquid afterwards, the light transmission of crystalline mother solution secondary decolourization liquid detect once per hour, and detecting instrument uses 722-S Spectrophotometer, crystalline mother solution secondary decolourization liquid light transmittance needs to keep >=80% during upper prop.When crystalline mother solution secondary decolourization Liquid light transmittance < 80% then stops crystalline mother solution destainer upper prop, prepares resin column regeneration.
(6) according to the general production technology of concentrated crystallization, crystalline mother solution secondary decolourization liquid is by monosodium glutamate crystallization, monosodium glutamate point It is dry from, monosodium glutamate, obtain crystal gourmet powder product.
Recycling regeneration according to new process 5 Tao Shi macroporous strong-base anion exchange resin regenerated liquids of progress can reach To the production requirement of decolorizing liquid rate >=80%.
The light transmittance of 3 upper prop of embodiment decoloration front and back can be shown in Table 3.
The light transmittance of 3 embodiment of table, 3 upper prop decoloration front and back
Project Light transmittance (%) before upper prop decolourizes Light transmittance (%) after upper prop decoloration
It recycles for 1st time 75.3 85.1
It recycles for 2nd time 74.4 85.6
It recycles for 3rd time 76.1 85.7
The 4th recycles 74.2 84.3
The 5th recycles 75.3 84.8
Embodiment 4:
(1) crystalline mother solution: being adjusted to pH value 7.7 with a small amount of glutamic acid for the sodium glutamate mother liquid that centrifuge separates, then with certainly The Baume degrees that water adjusts crystalline mother solution is 25 ° of B é.
(2) 0.3% (W/V) powder powder activity carbon decoloring, filtering: is added in the crystalline mother solution for adjusting pH value and Baume degrees Last active carbon stirring decoloration 60 minutes or more, carries out filters pressing with flame filter press, obtains the crystalline mother solution decoloration of light transmittance 75% Liquid.
(3) it collects Tao Shi large pore anion resin regeneration outflow salt hydrolysis imbibition, powder activity carbon decoloring, filtering is added: Recycling Tao Shi large pore anion resin regeneration outflow salt hydrolysis imbibition is added the stirring of 0.25% (W/V) Powdered Activated Carbon and is warming up to 60 DEG C~65 DEG C decolourize 45 minutes, resin regeneration filtrate is obtained by filtration through plate and frame filter press.
(4) filtrate adds refined salt and food-grade caustic soda, filtrate constant volume, the regeneration of Tao Shi large pore anion resin: regeneration filtrate Add edible refined salt to NaCl (W/W) be 10% and add food-grade caustic soda to NaOH (W/W) be 0.2%, then by filtrate constant volume To 12m3, the regeneration of Tao Shi macroporous strong-base anion exchange resin.
The regeneration of Tao Shi resin: the stirring of 0.25% (W/V) Powdered Activated Carbon is added to recycling resin regeneration outflow stripping liquid It is warming up to 60 DEG C~65 DEG C to decolourize 45 minutes, resin regeneration filtrate is obtained by filtration through plate and frame filter press, then regeneration filtrate is added Edible refined salt to NaCl mass is 10% and adds food-grade caustic soda to NaOH (W/W) to be 0.2%, then filtrate is settled to 12m3, impregnate 2 hours, be then washed till efflux pH value 7.5, efflux light transmittance >=98% with tap water is suitable, then use tap water Backwash, which pulls loose, to be put back into.
(5) crystalline mother solution destainer is through Tao Shi large pore anion resin column secondary decolourization: by 50 DEG C of crystalline mother solution destainers With 2.0m3/ h flow velocity is equipped with 2.5m by Φ 1.2m × 3.5m3The exchange column of macroporous strong-base anion exchange resin, obtains upper prop Crystalline mother solution secondary decolourization liquid afterwards, the light transmission of crystalline mother solution secondary decolourization liquid detect once per hour, and detecting instrument uses 722-S Spectrophotometer, crystalline mother solution secondary decolourization liquid light transmittance needs to keep >=80% during upper prop.When crystalline mother solution secondary decolourization Liquid light transmittance < 80% then stops crystalline mother solution destainer upper prop, prepares resin column regeneration.
(6) according to the general production technology of concentrated crystallization, crystalline mother solution secondary decolourization liquid is by monosodium glutamate crystallization, monosodium glutamate point It is dry from, monosodium glutamate, obtain crystal gourmet powder product.
Regeneration is recycled according to new process 10 Tao Shi macroporous strong-base anion exchange resin regenerated liquids of progress to be ok Reach the production requirement of decolorizing liquid rate >=80%, but is carrying out that production requirement cannot be reached 11 times.
The light transmittance of 4 upper prop of embodiment decoloration front and back can be shown in Table 4.
The light transmittance of 4 embodiment of table, 4 upper prop decoloration front and back
Project Light transmittance (%) before upper prop decolourizes Light transmittance (%) after upper prop decoloration
It recycles for 1st time 76.5 85.8
It recycles for 2nd time 75.6 85.0
It recycles for 3rd time 76.2 85.2
The 4th recycles 73.7 85.4
The 5th recycles 75.5 84.5
It recycles for 6th time 76.0 84.9
It recycles for 7th time 72.6 83.1
It recycles for 8th time 73.1 83.2
It recycles for 9th time 75.4 82.5
It recycles for 10th time 75.5 80.3
It recycles for 11st time 76.6 78.1
Method of the invention has the advantage that
One, Tao Shi macroporous strong-base anion exchange resin of the invention recycles benefit by flowing out stripping liquid using reclaiming With after regeneration, neutralize method of the destainer through Tao Shi macroporous strong-base anion exchange resin upper prop secondary decolourization, compare Tao Shi The direct preparation method of macroporous strong-base anion exchange resin regenerated liquid, light transmittance are not much different with the method that regenerated liquid does not recycle. 5 can be shown in Table by neutralizing the new old technology decoloration light transmittance comparing result of destainer, crystalline mother solution destainer.
The new old technology decoloration light transmittance comparison of 5 crystalline mother solution destainer of table
Two, Tao Shi macroporous strong-base anion exchange resin of the invention recycles benefit by flowing out stripping liquid using reclaiming With after regeneration, method of the crystalline mother solution destainer through Tao Shi macroporous strong-base anion exchange resin upper prop secondary decolourization, compare The direct preparation method of Tao Shi macroporous strong-base anion exchange resin regenerated liquid, light transmittance differ not with the method that regenerated liquid does not recycle Greatly.
Three, Tao Shi macroporous strong-base anion exchange resin of the invention recycles benefit by flowing out stripping liquid using reclaiming With after regeneration, neutralize destainer or crystalline mother solution destainer through Tao Shi macroporous strong-base anion exchange resin upper prop secondary decolourization, White brilliant liquid or crystalline mother solution secondary decolourization liquid after obtaining upper prop, according still further to the general production technology of concentrated crystallization, by taste Essence crystallization, monosodium glutamate separation, monosodium glutamate is dry, obtains crystal gourmet powder product, can reduce regeneration cost 32.9%.
Four, Tao Shi macroporous strong-base anion exchange resin of the invention recycles benefit by flowing out stripping liquid using reclaiming With after regeneration, neutralize destainer or crystalline mother solution destainer through Tao Shi macroporous strong-base anion exchange resin upper prop secondary decolourization, Regenerated liquid cycle-index can achieve 10 times.
Five, method of the invention needs not move through a large amount of technological transformation, can be in the production of existing glutamic acid manufacture monosodium glutamate Directly implement on line.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment Limitation, other any changes made without departing from the spirit and principles of the present invention, modification, substitution, combination or simplified, It should be equivalent substitute mode, be included within the scope of the present invention.

Claims (10)

1. a kind of method that anion exchange resin regenerated liquid recycles production monosodium glutamate, it is characterised in that: the following steps are included:
1) glutamic acid neutralizes: glutamic acid, edible soda ash and water being mixed and neutralized, control pH value is 6.5~7.4, and neutralization temperature is 60 DEG C~65 DEG C, the Baume degrees >=23 ° B é of neutralizer;
2) powder activity carbon decoloring, filtering: Powdered Activated Carbon, stirring decoloration is added in the neutralizer obtained to step 1), and filtering obtains To neutralization destainer;
3) it collects anion exchange resin regeneration outflow salt hydrolysis imbibition, powder activity carbon decoloring, filtering: recycling anion is added Exchanger resin regeneration outflow salt hydrolysis imbibition, is added Powdered Activated Carbon, stirring decoloration, and filtering obtains resin regeneration filtrate;
4) filtrate adds refined salt and food-grade caustic soda, filtrate constant volume, anion exchange resin regeneration: the resin that step 3) is obtained The mass concentration that regeneration filtrate adds edible refined salt to NaCl is 9%~12%, and the quality for adding food-grade caustic soda to NaOH is dense Degree is 0.18%~0.22%, then by filtrate constant volume, is regenerated anion exchange resin with filtrate;
5) destainer is neutralized through anion exchange resin secondary decolourization: 40 DEG C~45 DEG C steps 2) are obtained in glutamic acid and decolourized Liquid is with 2.5m3/ h~3m3/ h flow velocity passes through the exchange column of anion exchange resin, the white brilliant liquid after obtaining upper prop;
6) crystal product: the white brilliant liquid that step 5) is obtained is crystallized, separation, dry, obtains crystal gourmet powder product.
2. a kind of method that anion exchange resin regenerated liquid recycles production monosodium glutamate, it is characterised in that: the following steps are included:
1) monosodium glutamate crystalline mother solution adjusts: it is 7.6~7.7 that monosodium glutamate crystalline mother solution glutamic acid, which is adjusted pH value, is then adjusted with water The Baume degrees of mother liquor is 24.5 ° of é~25.5 ° B B é;
2) powder activity carbon decoloring, filtering: being added Powdered Activated Carbon for the crystalline mother solution that step 1) adjustment obtains, and stirring is decolourized, Filtering, obtains crystalline mother solution destainer;
3) it collects anion exchange resin regeneration outflow salt hydrolysis imbibition, powder activity carbon decoloring, filtering: recycling anion is added Exchanger resin regeneration outflow salt hydrolysis imbibition, is added Powdered Activated Carbon, stirring decoloration, and filtering obtains resin regeneration filtrate;
4) filtrate adds refined salt and food-grade caustic soda, filtrate constant volume, anion exchange resin regeneration: the resin that step 3) is obtained The mass concentration that regeneration filtrate adds edible refined salt to NaCl is 9%~12%, and the quality for adding food-grade caustic soda to NaOH is dense Degree is 0.18%~0.22%, then by filtrate constant volume, is regenerated anion exchange resin with filtrate;
5) crystalline mother solution destainer is through anion exchange resin secondary decolourization: it is de- that 45 DEG C~50 DEG C steps 2) are obtained crystalline mother solution Color liquid is with 2.0m3/ h~2.5m3/ h flow velocity passes through the exchange column of anion exchange resin, and the crystalline mother solution after obtaining upper prop is secondary Destainer;
6) crystal product: the crystalline mother solution secondary decolourization liquid that step 5) is obtained is crystallized, separates, is dry, obtains crystal gourmet powder Product.
3. the method that a kind of anion exchange resin regenerated liquid according to claim 1 or 2 recycles production monosodium glutamate, Be characterized in that: in step 3), the quality of Powdered Activated Carbon accounts for the 0.2%~0.3% of resin regeneration outflow salt water stripping liquid volume; Stirring decoloration be temperature be 60 DEG C~65 DEG C at decolourize 45 minutes~60 minutes.
4. the method that a kind of anion exchange resin regenerated liquid according to claim 1 or 2 recycles production monosodium glutamate, Be characterized in that: in step 5), the diameter of exchange column is 1m~1.5m, a height of 3m~4m, and anion exchange resin accounts for exchange column Volume fraction is 50%~80%.
5. the method that a kind of anion exchange resin regenerated liquid according to claim 1 recycles production monosodium glutamate, special Sign is: in step 2), the quality of Powdered Activated Carbon accounts for the 0.5%~1.5% of neutralizer volume;The time of stirring decoloration is 45 Minute~60 minutes;It obtains neutralizing decolorizing liquid rate >=94%.
6. the method that a kind of anion exchange resin regenerated liquid according to claim 1 recycles production monosodium glutamate, special Sign is: in step 5), obtained white brilliant liquid light transmittance >=98%.
7. the method that a kind of anion exchange resin regenerated liquid according to claim 2 recycles production monosodium glutamate, special Sign is: in step 2), the quality of Powdered Activated Carbon accounts for the 0.3%~0.4% of neutralizer volume;Obtain crystalline mother solution destainer Light transmittance >=70%.
8. the method that a kind of anion exchange resin regenerated liquid according to claim 2 recycles production monosodium glutamate, special Sign is: in step 5), obtained crystalline mother solution secondary decolourization liquid light transmittance >=80%.
9. a kind of described in any item anion exchange resin regenerated liquids recycle production monosodium glutamate according to claim 1~8 Method, it is characterised in that: anion exchange resin is macroporous strong-base type styrene series anion exchange resin.
10. the method that a kind of anion exchange resin regenerated liquid according to claim 9 recycles production monosodium glutamate, special Sign is: anion exchange resin is the AMBERLITETM FPA90Cl resin of Tao Shi.
CN201810768602.XA 2018-07-13 2018-07-13 The method that anion exchange resin regenerated liquid recycles production monosodium glutamate Pending CN109077289A (en)

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Cited By (6)

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CN110975327A (en) * 2019-12-17 2020-04-10 广东省生物工程研究所(广州甘蔗糖业研究所) Automatic control system and automatic control method for decoloring resin column in monosodium glutamate production
CN112471485A (en) * 2020-12-03 2021-03-12 山东均智生物科技有限公司 Decolouring refining process for producing gourmet powder
CN112914075A (en) * 2021-03-11 2021-06-08 广州奥桑味精食品有限公司 Monosodium glutamate raw material liquid and preparation method and application thereof
CN113558217A (en) * 2021-08-24 2021-10-29 温州快鹿集团公司 Refining process of monosodium glutamate
CN114260028A (en) * 2021-12-27 2022-04-01 同舟纵横(厦门)流体技术有限公司 Method and device for decoloring sodium glutamate feed liquid
CN114287603A (en) * 2021-12-30 2022-04-08 呼伦贝尔东北阜丰生物科技有限公司 Method for improving color intensity of monosodium glutamate product

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110975327A (en) * 2019-12-17 2020-04-10 广东省生物工程研究所(广州甘蔗糖业研究所) Automatic control system and automatic control method for decoloring resin column in monosodium glutamate production
CN112471485A (en) * 2020-12-03 2021-03-12 山东均智生物科技有限公司 Decolouring refining process for producing gourmet powder
CN112914075A (en) * 2021-03-11 2021-06-08 广州奥桑味精食品有限公司 Monosodium glutamate raw material liquid and preparation method and application thereof
CN113558217A (en) * 2021-08-24 2021-10-29 温州快鹿集团公司 Refining process of monosodium glutamate
CN114260028A (en) * 2021-12-27 2022-04-01 同舟纵横(厦门)流体技术有限公司 Method and device for decoloring sodium glutamate feed liquid
CN114287603A (en) * 2021-12-30 2022-04-08 呼伦贝尔东北阜丰生物科技有限公司 Method for improving color intensity of monosodium glutamate product

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