CN101863789A - Method for separation and purification of L-potassium glutamate monohydrate - Google Patents

Method for separation and purification of L-potassium glutamate monohydrate Download PDF

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Publication number
CN101863789A
CN101863789A CN 201010214565 CN201010214565A CN101863789A CN 101863789 A CN101863789 A CN 101863789A CN 201010214565 CN201010214565 CN 201010214565 CN 201010214565 A CN201010214565 A CN 201010214565A CN 101863789 A CN101863789 A CN 101863789A
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potassium glutamate
purification
monohydrate
potassium
glutamate monohydrate
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席日新
李海涛
吴国伟
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YIXING QIANCHENG BIOLOGICAL CO Ltd
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YIXING QIANCHENG BIOLOGICAL CO Ltd
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Abstract

The invention belongs to the chemical field, and discloses a method for separation and purification of L-potassium glutamate monohydrate, which comprises the following specific steps: filling deionized water into a reactor, heating, adding L-glutamic acid and potassium carbonate, correcting the PH value after clarification of reaction solution, adding a proper amount of activated carbon for decolorization, filtering, concentrating to a certain concentration, adding a certain amount of L-potassium glutamate as a seed crystal into the reaction solution, and inducing the L-potassium glutamate in the reaction solution for crystallization, thereby forming an L-potassium glutamate monohydrate crystal. The L-potassium glutamate monohydrate crystal obtained in the method has the advantages of large and uniform particle size and stable water contents in each batch of products. Moreover, the invention can greatly reduce the cost, lower the energy consumption, increase the yield, improve the production environment, and reduce the pollution.

Description

A kind of method of separating purification of L-potassium glutamate monohydrate
Technical field
The present invention relates to a kind of method of separating purification of L-potassium glutamate monohydrate, be specifically related to a kind of method of separating purification of L-potassium glutamate monohydrate with the induced crystallization method.
Background technology
L-Potassium glutamate (Monopotassium L-Glutamate), another name: L-kaglutam, molecular formula: C 5H 8KNO 4, molecular weight: 185.22, molecular structural formula:
Figure BSA00000189116800011
Its monohydrate, i.e. L-potassium glutamate monohydrate (molecular formula: C 5H 8KNO 4H 2O, molecular weight: 203.24, molecular structural formula:
Figure BSA00000189116800012
) have application widely at foodstuff additive and medical material medicine field.
Bread is the staff of life, and the industry relevant with food possesses stable development environment; At present food from the marched toward variation of industrial chain of primary demand, particularly has the China of long cooking culture already.At all kinds of fermented-milk base beverages, can or bottled vegetables and jam product, aspects such as flour products, food flavouring, dietary food product, partial function beverage are realizable value all as the Potassium glutamate of additive.The polygamy side of food-flavoring comps makes that Sodium Glutamate no longer is independent one.Potassium glutamate is a kind of as flavour agent equally, progressively promotes abroad at present and come; And too much relative some crowd of the intake of Sodium Glutamate has the faint side effect of part, and the welcome degree of Potassium glutamate is improved.
Pharmaceutically Potassium glutamate is mainly used in hepatogenic encephalopathy, hepatic coma and other mental symptom of treatment due to the hyperammonemia, and the rehabilitation of liver function is cut much ice.Potassium glutamate also participates in brain Proteometabolism and carbohydrate metabolism, and the promotes oxidn process is improved the function of central nervous system.Modern's sub-health state and secular operating pressure make liver often be in depressive state, toast each other also to make liver be subjected to the infringement of alcohol and impaired heavy drinking and cause state such as stupor grade.By the intravenous infusion of Sodium Glutamate and Potassium glutamate, can be combined into nontoxic glutamine with too much ammonia in the blood, the latter dissociates ammonia through the effect of glutamine enzyme at kidney, is discharged by urine, therefore can alleviate the hepatic coma symptom.
Potassium glutamate and Sodium Glutamate except that the effect with unique correction acid base equilibrium, can also reduce too much Ammonia toxicant in fire victim's body as alkaline drug by the liver effect.In addition, it also has the effect of stronger direct excitor nerve.Cooperate sodium bicarbonate to be used to the fluid-supplement therapy of burning it clinically, and obtained good effect.
The preparation method of present L-potassium glutamate monohydrate: after the reaction of L-L-glutamic acid and salt of wormwood acid-base neutralisation is dissolved in the aqueous solution, pass through decolouring, press filtration, be concentrated to finite concentration, adopt spray crystallization to obtain product after cooling to room temperature, promptly the L-L-glutamic acid of input calculated amount and salt of wormwood are solvent as raw material with the deionized water in reaction vessel.The batching reaction post-equalization PH=6.5-8.0 that finishes after adding activated carbon decolorizing, press filtration, being concentrated to finite concentration, is cooled to the direct spraying drying of room temperature and makes product.The L-L-glutamic acid of calculated amount and salt of wormwood are when L-L-glutamic acid and salt of wormwood can complete reactions under the theory state, the L-L-glutamic acid that is added and the amount of salt of wormwood.
The product that this method is produced is a pulverulent solids, can't obtain the extraordinary product of granularity; And the moisture of every batch of product to be difficult to the moisture difference of each position product in control, the drying chamber bigger, be difficult to produce stable, uniform, qualified L-potassium glutamate monohydrate (C 5H 8KNO 4H 2O); Very low to the humidity of production environment and temperature requirement control simultaneously in case the material deliquescence.This method fixed cost plant and equipment input ratio is big, yield is on the low side relatively, energy consumption is very high.
Potassium glutamate as while irradiated foods additive and medical material medicine field, growing in demand, with and the powerful environment that sets foot in support down, how to make it better, made full use of by market more widely, promote the development of related industries chain, this also is the problem that we think deeply about for it, by making great efforts and practice, we successfully utilize related resource to develop, and realize producing a kind of new technique method of Potassium glutamate.The success of exploitation also will be optimized structure indirectly and promote the industry stable development and be played effect for foodstuff additive, medicine two class industries.
Summary of the invention
Can't obtain technical problems such as good L potassium glutamate monohydrate of water content stable particle degree and cost and energy consumption height, productive rate be relatively low when the objective of the invention is to separate purification L-Potassium glutamate, provide a kind of induced crystallization method to separate the method for purification of L-potassium glutamate monohydrate at the direct spray drying process of the pointed employing of background technology.
Purpose of the present invention can reach by following measure:
A kind of induced crystallization method is separated the method for purification of L-potassium glutamate monohydrate, after in reaction vessel, adding deionized water and heating, drop into L-L-glutamic acid and salt of wormwood, pH value is proofreaied and correct in the clarification of question response liquid, add proper amount of active carbon decolouring, press filtration, be concentrated to finite concentration, the reaction soln cooling is separated purification of L-potassium glutamate monohydrate; When separating purification of L-potassium glutamate monohydrate, after the reaction soln cooling, add L-Potassium glutamate crystal as crystal seed in reaction soln, the L-Potassium glutamate crystallization in the induced reaction solution forms the stable L-potassium glutamate monohydrate crystal of water content.
Above-mentioned induced crystallization method is separated the method for purification of L-potassium glutamate monohydrate, and adding crystal seed L-Potassium glutamate crystalline weight is the 5%-12% of reactant L-L-glutamic acid input amount, is preferably 10%.
Above-mentioned induced crystallization method is separated the method for purification of L-potassium glutamate monohydrate, and when adding crystal seed L-Potassium glutamate crystal, solution temperature is controlled at 20 ℃-48 ℃, is preferably 45 ℃.
Detailed process is: add deionized water and be heated to certain temperature in reaction vessel, drop into the L-L-glutamic acid and the salt of wormwood of calculated amount, the weightmeasurement ratio of reactant L-L-glutamic acid and deionized water (Kg/L) is 0.1~0.4: 1, question response liquid clarification post-equalization PH=6.5-8.0.Neutralization reaction dissolving back adds proper amount of active carbon, pass through decolouring, press filtration, be concentrated to finite concentration, after cooling to 20 ℃-48 ℃, adding weight is the L-Potassium glutamate of the 5%-12% of L-L-glutamic acid charging capacity, progressively cooling is stirred and is induced L-potassium glutamate monohydrate crystal to separate out, separate solid material and mother liquor, oven dry finished product, bake out temperature is controlled at 65 ℃-70 ℃, can obtain big and even, that water content the is stable L-potassium glutamate monohydrate crystal of granularity.
The L-L-glutamic acid of calculated amount and salt of wormwood are when L-L-glutamic acid and salt of wormwood can complete reactions under the theory state, the L-L-glutamic acid that is added and the amount of salt of wormwood.
L-Potassium glutamate as crystal seed can be made by oneself according to ordinary method, also can buy on market.
Beneficial effect of the present invention:
1, the crystalline particle degree by this method separation purification gained is big and even, and every batch of product moisture is stable.Can produce stable qualified product (just in time being a water thing) and detect the product moisture content about 8.9%, and be all 2.4-6.5%, want just in time that a water thing is difficult to, can not realize substantially by the product moisture content that spraying drying obtains;
2, produce the L-potassium glutamate monohydrate by the modified version novel process, its equipment input cost reduces greatly: area of mill site minimizing 70%, equipment input reduce by 60%;
3, the yield of product can improve about 10%, energy consumption reduces by 50%.
4, simultaneously simple operating steps, the temperature humidity of operating environment is required to reduce significantly, change production environment, reduce and pollute;
Embodiment
Embodiment 1
Add the 500ml deionized water in the 1000ml beaker, heated and stirred on magnetic stirring apparatus when temperature rises to 70 ℃-75 ℃, adds L-L-glutamic acid 100g, K 2CO 347g.PH is surveyed in reaction soln clarification back sampling, proofreaies and correct terminal point PH=6.5-8.0.Add gac 0.01Kg/L, through decolouring, press filtration, concentrate and make it to form supersaturated solution, cool to 46 ℃ after, add crystal seed L-Potassium glutamate 6g and stir crystallisation by cooling, dry under suction filtration, 65 ℃ of-70 ℃ of temperature finished product 105g, yield 72.8%, it is qualified to detect, and detected result sees Table 1.
Embodiment 2
Add the 500ml deionized water in the 1000ml beaker, heated and stirred on magnetic stirring apparatus when temperature rises to 75 ℃, adds L-L-glutamic acid 100g, K 2CO 347g.PH is surveyed in reaction soln clarification back sampling, proofreaies and correct terminal point PH=6.7-8.0.Add gac 0.01Kg/L, through decolouring, press filtration, concentrate and make it to form supersaturated solution, cool to 46 ℃ after, add crystal seed L-Potassium glutamate 8g and stir crystallisation by cooling, dry under suction filtration, 65 ℃ of-70 ℃ of temperature finished product 118g, yield 80.73%, it is qualified to detect, and detected result sees Table 1.
Embodiment 3
Add the 500ml deionized water in the 1000ml beaker, heated and stirred on magnetic stirring apparatus when temperature rises to 70 ℃, adds L-L-glutamic acid 100g, K 2CO 347g.PH is surveyed in reaction soln clarification back sampling, proofreaies and correct terminal point PH=6.7-7.5.Add gac 0.01Kg/L, through decolouring, press filtration, concentrate and make it to form supersaturated solution, cool to 45 ℃ after, add crystal seed L-Potassium glutamate 10g and stir crystallisation by cooling, dry under suction filtration, 65 ℃ of-70 ℃ of temperature finished product 130g, yield 87.74%, it is qualified to detect, and detected result sees Table 1.
Embodiment 4
Add the 500ml deionized water in the 1000ml beaker, heated and stirred on magnetic stirring apparatus when temperature rises to 70 ℃, adds L-L-glutamic acid 100g, k 2CO 34 7g.PH is surveyed in reaction soln clarification back sampling, proofreaies and correct terminal point PH=6.7-7.5.Add gac 0.01Kg/L, through decolouring, press filtration, concentrate and make it to form supersaturated solution, after cooling to 46 ℃, add crystal seed L-Potassium glutamate 13g and stir crystallisation by cooling, dry under suction filtration, 65 ℃ of-70 ℃ of temperature finished product 136g, yield 90.57%, mother liquor this moment difficult separation, finished color is slightly yellow, and detected result sees Table 1.
Embodiment 5
Add the 500ml deionized water in the 1000ml beaker, heated and stirred on magnetic stirring apparatus when temperature rises to 70 ℃, adds L-L-glutamic acid 150g, K 2CO 370.5g.PH is surveyed in reaction soln clarification back sampling, proofreaies and correct terminal point PH=6.7-7.5.Add gac 0.01Kg/L, through decolouring, press filtration, concentrate and make it to form supersaturated solution, cool to 45 ℃ after, add crystal seed L-Potassium glutamate 15g and stir crystallisation by cooling, dry under suction filtration, 65 ℃ of-70 ℃ of temperature finished product 208g, yield 93.6%, it is qualified to detect, and detected result sees Table 2.
Embodiment 6
Add 1 ton of deionized water in 2 tons of stainless steel cauldrons, heated and stirred when temperature rises to 70 ℃, adds L-L-glutamic acid 300Kg, K 2CO 3140.9Kg.PH is surveyed in reaction soln clarification back sampling, proofreaies and correct terminal point PH=6.7-7.5.Add gac 0.01Kg/L, through decolouring, press filtration, concentrate and make it to form supersaturated solution, after cooling to 46 ℃, add crystal seed L-Potassium glutamate 30Kg, progressively induced crystallization is stirred in cooling, and cooling rate is controlled at and per hour descends 2 ℃-3 ℃, treats that feed temperature reduces to room temperature and keep centrifugation solid materials and mother liquor after 8 hours, dry under 65 ℃ of-70 ℃ of temperature finished product 400Kg, yield 89.99%.It is qualified to detect, and detected result sees Table 2.
Comparative example 1
Add the 70-80L deionized water in the 100L stainless steel cauldron, heated and stirred when temperature rises to 70 ℃, adds 15Kg L-L-glutamic acid, k 2CO 37Kg.PH is surveyed in reaction soln clarification back sampling, proofreaies and correct terminal point PH=6.7-7.5.Add gac 0.01Kg/L, through decolouring, press filtration, concentrate and make it to form supersaturated solution, be cooled to room temperature after, directly spraying drying makes finished product 15Kg, yield 72.39%, the gained finished product is the white powder crystal, detected result sees Table 2.The moisture of product is 3.62% after testing, and is defective, and all the other indexs are all qualified.Detected result sees Table 2.
Comparative example 2
Add 1 ton of deionized water in 2 tons of stainless steel cauldrons, heated and stirred when temperature rises to 70 ℃, adds 300KgL-L-glutamic acid, k 2CO 3L40.9Kg.PH is surveyed in reaction soln clarification back sampling, proofreaies and correct terminal point PH=6.5-8.0.Add gac 0.01Kg/L, through decolouring, press filtration, concentrate and make it to form supersaturated solution, be cooled to room temperature after, directly spraying drying makes finished product 330Kg, yield 79.62%, the gained finished product is the white powder crystal, detected result sees Table 2.The moisture of products obtained therefrom is 5.60% defective after testing, and all the other indexs are all qualified.Detected result sees Table 2.
The detected result of the product that table 1 embodiment is 1,2,3,4
Figure BSA00000189116800051
The detected result of the product that table 2 embodiment 5,6 and comparative example are 1,2
Figure BSA00000189116800061
Achievement after the improvement is except the improve of the reduction of cost, yield, mainly can produce stable qualified product (just in time being a water thing) exactly from the detected result mountain is exactly just in time to be about 8.9%, and be all 2.4-6.5% by the product moisture that spraying drying obtains, want just in time a water thing and be difficult to, can not realize substantially.And the weight of adding crystal seed is the 5%-12% of L-L-glutamic acid charging capacity, surpasses 12% products obtained therefrom mother liquor separation difficulty, and finished color is slightly yellow, does not meet quality standard, and the client does not accept.

Claims (5)

1. an induced crystallization method is separated the method for purification of L-potassium glutamate monohydrate, after in reaction vessel, adding deionized water and heating, drop into L-L-glutamic acid and salt of wormwood, pH value is proofreaied and correct in the clarification of question response liquid, add the proper amount of active carbon decolouring, press filtration, be concentrated to finite concentration, the reaction soln cooling is separated purification of L-potassium glutamate monohydrate, it is characterized in that: when separating purification of L-potassium glutamate monohydrate, after the reaction soln cooling, add L-Potassium glutamate crystal as crystal seed in reaction soln, the L-Potassium glutamate crystallization in the induced reaction solution forms the stable L-potassium glutamate monohydrate crystal of water content.
2. induced crystallization method according to claim 1 is separated the method for purification of L-potassium glutamate monohydrate, it is characterized in that: adding crystal seed L-Potassium glutamate crystalline weight is the 5%-12% of reactant L-L-glutamic acid input amount.
3. induced crystallization method according to claim 2 is separated the method for purification of L-potassium glutamate monohydrate, it is characterized in that: adding crystal seed L-Potassium glutamate crystalline weight is 10% of reactant L-L-glutamic acid input amount.
4. induced crystallization method according to claim 1 is separated the method for purification of L-potassium glutamate monohydrate, it is characterized in that: when adding crystal seed L-Potassium glutamate crystal, solution temperature is controlled at 20 ℃-48 ℃.
5. induced crystallization method according to claim 4 is separated the method for purification of L-potassium glutamate monohydrate, it is characterized in that: when adding crystal seed L-Potassium glutamate crystal, solution temperature is controlled at 45 ℃.
CN 201010214565 2010-06-30 2010-06-30 Method for separation and purification of L-potassium glutamate monohydrate Pending CN101863789A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102408347A (en) * 2011-10-31 2012-04-11 宜兴市前成生物有限公司 Method for preparing monopotassium L-aspartate dihydrate by separation process
CN106117069A (en) * 2016-06-17 2016-11-16 宜兴市前成生物有限公司 A kind of method preparing L glutamate chelate potassium one water thing

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RO76404A2 (en) * 1979-05-11 1981-05-30 Intreprinderea De Medicamente "Terapia",Ro PROCESS FOR OBTAINING POTASSIUM GLUTAMATE

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
RO76404A2 (en) * 1979-05-11 1981-05-30 Intreprinderea De Medicamente "Terapia",Ro PROCESS FOR OBTAINING POTASSIUM GLUTAMATE

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
《Chem. Ber.》 19901231 Hubert Schmidbaur等 Potassium Hydrogen L-Glutamate Monohydrate K(L-GluH)•H20 1001-1004 第123卷, *
《发酵科技通讯》 19811231 李益民 关于味精结晶的操作 43-46 , *

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102408347A (en) * 2011-10-31 2012-04-11 宜兴市前成生物有限公司 Method for preparing monopotassium L-aspartate dihydrate by separation process
CN102408347B (en) * 2011-10-31 2014-04-09 宜兴市前成生物有限公司 Method for preparing monopotassium L-aspartate dihydrate by separation process
CN106117069A (en) * 2016-06-17 2016-11-16 宜兴市前成生物有限公司 A kind of method preparing L glutamate chelate potassium one water thing

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Application publication date: 20101020