CN106117069A - A kind of method preparing L glutamate chelate potassium one water thing - Google Patents

A kind of method preparing L glutamate chelate potassium one water thing Download PDF

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Publication number
CN106117069A
CN106117069A CN201610429682.7A CN201610429682A CN106117069A CN 106117069 A CN106117069 A CN 106117069A CN 201610429682 A CN201610429682 A CN 201610429682A CN 106117069 A CN106117069 A CN 106117069A
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pidolidone
potassium
water
chelating
water thing
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席日新
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YIXING QIANCHENG BIOLOGICAL CO Ltd
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YIXING QIANCHENG BIOLOGICAL CO Ltd
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    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C227/00Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
    • C07C227/14Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof
    • C07C227/18Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton from compounds containing already amino and carboxyl groups or derivatives thereof by reactions involving amino or carboxyl groups, e.g. hydrolysis of esters or amides, by formation of halides, salts or esters
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C227/00Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
    • C07C227/38Separation; Purification; Stabilisation; Use of additives
    • C07C227/40Separation; Purification
    • C07C227/42Crystallisation
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07BGENERAL METHODS OF ORGANIC CHEMISTRY; APPARATUS THEREFOR
    • C07B2200/00Indexing scheme relating to specific properties of organic compounds
    • C07B2200/13Crystalline forms, e.g. polymorphs

Abstract

The invention discloses a kind of method preparing L glutamate chelate potassium one water thing, including: with potassium carbonate or potassium hydroxide, L glutamic acid as raw material, react with the water that temperature is 70~80 DEG C for solvent, the pH value of solution clarification post-equalization reactant liquor is to 7.5~8.5, continue to react 2~4 hours at 80~85 DEG C, by reactant liquor decolorization filtering, to be concentrated into mother-in-law U.S. degree be 36~38 ° of B é, is cooled to 15~20 DEG C;Adding L glutamate chelate potassium one water thing crystal in concentrated solution to be centrifuged to obtain crude product as crystal seed, maintenance temperature 15~20 DEG C, stirred crystallization, blowing, every 100kg crude product uses 5~10L deionized waters rinsings, and solid obtains chelating degree after drying and reaches the product of more than 95%.The present invention does not use organic solvent, improves the safety coefficient of production environment, considerably reduces cost of material;And product no solvent residue, moisture is easy to control;And equipment, place input can be reduced.

Description

A kind of method preparing Pidolidone chelating potassium one water thing
Technical field
The invention belongs to the field of chemical synthesis, be specifically related to a kind of method preparing Pidolidone chelating potassium one water thing.
Background technology
Pidolidone chelating potassium one water thing, is a kind of medicine intermediate, can be used as food additive and biochemical research Preparation, in regulation myocardial function and various arrhythmias, hepatitis, the liver function such as electro physiology and treatment cardiovascular and cerebrovascular disease, hypokalemia Congruent aspect can not there is significant curative effect.Existing production technology dispensing, concentrate just the same, mainly extracting method in place of difference Difference.Extraction Pidolidone chelating potassium one water thing technique in production technology is at present: use organic solvent to change solvent pole Property, so that product separates out or use the method being spray-dried, directly obtain finished product.First method: use organic solvent, Reduce easy residual organic solvent in the safety coefficient of production environment, and the product obtained, use organic solvent extraction simultaneously Production cost can be increased.Simultaneously because use organic solvent outward appearance of product in product drying course to take away owing to solvent volatilizees A small amount of water of crystallization and cause tarnish, poor fluidity;The second extracting method equipment, place throw big, production cost height;Obtained Product is powder, has no granule and mobility can be sayed, moisture is unstable, wayward.
Summary of the invention
It is an object of the invention to provide a kind of method preparing Pidolidone chelating potassium one water thing.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of method preparing Pidolidone chelating potassium one water thing, comprises the following steps:
Step (1), with potassium carbonate or potassium hydroxide, Pidolidone as raw material, with water that temperature is 70~80 DEG C as solvent Reacting, the pH value of solution clarification post-equalization reactant liquor, to 7.5~8.5, continues reaction 2~4 hours at 80~85 DEG C, so After by reactant liquor decolorization filtering, to be concentrated into mother-in-law U.S. degree be 36~38 ° of B é, concentrated solution is cooled to temperature 15~20 DEG C;
Step (2), concentrated solution after cooling add Pidolidone chelating potassium one water thing crystal as crystal seed, maintain temperature Spend 15~20 DEG C, stirred crystallization 36~48 hours, blowing is centrifugal to obtain Pidolidone chelating potassium crude product, every 100kg crude product use 5~ 10L deionized water rinses, and solid is dried at 80~85 DEG C and within 6~10 hours, obtains Pidolidone chelating potassium one water produce product.
In step (1), the quality of described Pidolidone is the 20~25% of the quality of water, preferably 20%;L-paddy ammonia Acid is 2:1~1.1, preferably 2:1.005 with the ratio of the amount of the material of potassium carbonate;The amount of the material of Pidolidone and potassium hydroxide Ratio be 1:1~1.1, preferably 1:1.01.
In step (1), preferably react with the water that temperature is 75 DEG C for solvent.
In step (2), the w/v of described crystal seed Pidolidone chelating potassium one water thing crystal and concentrated solution be 1~ 5:100 (g:mL or kg:L), preferably 3:100.Pidolidone chelating potassium one water thing crystal is not specially required, only by the present invention If qualified products can serve as crystal seed.
In step (2), every 100kgL-glutamate chelate potassium crude product uses 6~8L deionized water rinsings.
As prepare Pidolidone chelating potassium one water thing preferred version, comprise the following steps:
Step (1), with potassium carbonate or potassium hydroxide, Pidolidone as raw material, carry out with the water that temperature is 75 DEG C for solvent Reaction, the pH value of solution clarification post-equalization reactant liquor, to 8.0-8.5, continues to react 2~4 hours at 85 DEG C;Then will reaction Loss of thick fluid chromogenic filter, to be concentrated into mother-in-law U.S. degree be 36-38 ° of B é, and concentrated solution is cooled to temperature 15-20 DEG C.
Step (2), concentrated solution add Pidolidone chelating potassium one water thing crystal as crystal seed, Pidolidone chelating potassium one The w/v of water thing crystal and concentrated solution is 3:100, maintenance temperature 16~18 DEG C, stirred crystallization 40 hours, and blowing is centrifuged Obtaining Pidolidone chelating potassium crude product, every 100kg crude product uses 6~8L deionized waters rinsings, the most box 80~85 DEG C of solid to do Within dry about 8 hours, obtain Pidolidone chelating potassium one water produce product.
Beneficial effects of the present invention:
Using the inventive method to prepare Pidolidone chelating potassium one water thing, chelating degree has reached more than 95%, has well solved Determine client's demand for height chelating degree Monopotassium L-Glutamate one water thing.
Client is more and more higher to the requirement of dissolvent residual, and not using solvent is trend of the times, and the present invention does not use organic molten Agent, improves the safety coefficient of production environment, does not use organic solvent that cost of material can also be greatly lowered simultaneously, reduces into These about 6000 yuan/ton;Guaranteeing product no solvent residue, moisture is easy to control simultaneously;And the program relative to spray drying method, if Standby, place puts into smaller, can reduce the equipment investment of about 20%.
It is embodied in:
1) system pH meta-alkalescence, maintains reaction 3 hours simultaneously, makes the chelating degree of Pidolidone chelating potassium one water thing by 65% ~70% brought up to more than 95%.
2) put into 1~5% Pidolidone chelating potassium one water thing crystal as crystal seed, induction Pidolidone chelating potassium knot Brilliant.
3) maintain crystallization temperature 15~20 DEG C, be to ensure that Pidolidone chelating potassium is as much as possible and crystallize out, tie up simultaneously Holding 36~48 hours and be to ensure that product crystal habit is good, mother solution contained by material surface is few, so can directly use a conventional oven Dry.
4) solid-liquid centrifugation uses a small amount of deionized water wash to guarantee material surface band mother solution as far as possible less when separating, and dries Rear product appearance is the brightest, good fluidity.
Detailed description of the invention
Below by detailed description of the invention, technical scheme is described further.
Embodiment 1
A kind of method preparing Pidolidone chelating potassium one water thing, comprises the following steps:
(1), reactor adds water, be equipped with motor stirring, be heated to temperature 75 DEG C, maintain stirring, add Pidolidone After, it being gradually added potassium carbonate, potassium carbonate need to be slowly added to, and spills with the too much feed liquid of foam-resistant;Wherein the quality of Pidolidone is The 20% of water quality, Pidolidone is 2:1.005 with the ratio of the amount of the material of potassium carbonate.
After solution clarification, take and test pH after a small amount of reacting liquid filtering roguing, and to correct reactant liquor pH be 8.0;Continue 85 React 3 hours at DEG C;Then by reactant liquor decolorization filtering, being concentrated in vacuo to mother-in-law U.S. degree is 37.6 ° of B é, and concentrated solution is cooled to temperature 18℃。
(2), the concentrated solution after cooling adds Pidolidone chelating potassium one water thing crystal as crystal seed, Pidolidone chela The w/v closing potassium one water thing crystal and concentrated solution is 3:100, maintenance temperature 16~18 DEG C, and stirred crystallization 40 hours is put Material is centrifugal that Pidolidone chelates potassium crude product, and every 100kg crude product uses the rinsing of 8L deionized water, the most box 80~85 DEG C of solid Be dried about 8 hours, after moisture is qualified can with discharging, pack, seal.
Embodiment 2
A kind of method preparing Pidolidone chelating potassium one water thing, comprises the following steps:
(1), reactor adds water, be equipped with motor stirring, be heated to temperature 75 DEG C, maintain stirring, add Pidolidone After, it being gradually added potassium hydroxide, potassium hydroxide need to be slowly added to, and spills with the too much feed liquid of foam-resistant;The wherein matter of Pidolidone 20% that amount is water quality, the amount of Pidolidone and the material of potassium hydroxide ratio is for 1:1.01.
After solution clarification, take and test pH after a small amount of reacting liquid filtering roguing, and to correct reactant liquor pH be 8.0;Continue 85 React 3 hours at DEG C;Then by reactant liquor decolorization filtering, being concentrated in vacuo to mother-in-law U.S. degree is 37.2 ° of B é, and concentrated solution is cooled to temperature 18℃。
(2), the concentrated solution after cooling adds Pidolidone chelating potassium one water thing crystal as crystal seed, Pidolidone chela The w/v closing potassium one water thing crystal and concentrated solution is 3:100, maintenance temperature 16~18 DEG C, and stirred crystallization 40 hours is put Material is centrifugal that Pidolidone chelates potassium crude product, and every 100kg crude product uses the rinsing of 8L deionized water, the most box 80~85 DEG C of solid Be dried about 8 hours, after moisture is qualified can with discharging, pack, seal.
Embodiment 3
A kind of method preparing Pidolidone chelating potassium one water thing, comprises the following steps:
(1), reactor adds water, be equipped with motor stirring, be heated to temperature 75 DEG C, maintain stirring, add Pidolidone After, it being gradually added potassium carbonate, potassium carbonate need to be slowly added to, and spills with the too much feed liquid of foam-resistant;Wherein the quality of Pidolidone is The 20% of water quality, the amount of Pidolidone and the material of potassium carbonate is than for 2:1.005.
After solution clarification, take and test pH after a small amount of reacting liquid filtering roguing, and to correct reactant liquor pH be 8.2;Continue 85 React 3 hours at DEG C;Then by reactant liquor decolorization filtering, being concentrated in vacuo to mother-in-law U.S. degree is 37.6 ° of B é, and concentrated solution is cooled to temperature 16℃。
(2), the concentrated solution after cooling adds Pidolidone chelating potassium one water thing crystal to chelate as crystal seed, Pidolidone The w/v of potassium one water thing crystal and concentrated solution is 5:100, maintenance temperature 16~18 DEG C, stirred crystallization 40 hours, blowing Centrifugal that Pidolidone chelates potassium crude product, every 100kg crude product uses the rinsing of 6L deionized water, and the most box 80~85 DEG C of solid is done Dry about 8 hours, after moisture is qualified can with discharging, pack, seal.
Comparative example 1
(1), reactor adds water, be equipped with motor stirring, be heated to temperature 75 DEG C, maintain stirring, add Pidolidone After, it being gradually added potassium carbonate, potassium carbonate need to be slowly added to, and spills with the too much feed liquid of foam-resistant;Wherein the quality of Pidolidone is The 20% of water quality, the amount of Pidolidone and the material of potassium carbonate is than for 2:1.005.
After solution clarification, take and test pH after a small amount of reacting liquid filtering roguing, and to correct reactant liquor pH be 8.1;Continue 85 React 3 hours at DEG C;Then by reactant liquor decolorization filtering, being concentrated in vacuo to mother-in-law U.S. degree is 37.6 ° of B é, and concentrated solution is cooled to temperature 16℃。
(2), in reactor add dehydrated alcohol, the volume ratio of concentrated solution and dehydrated alcohol is 1:3, after stirring 2 by Step has Pidolidone chelating potassium crystal to separate out, and carries out centrifugation after 10 hours, and in 50-60 DEG C of vacuum drying oven, drying obtains L- Glutamate chelate potassium finished product.
Comparative example 2
(1), reactor adds water, be equipped with motor stirring, be heated to temperature 75 DEG C, maintain stirring, add Pidolidone After, it being gradually added potassium carbonate, potassium carbonate need to be slowly added to, and spills with the too much feed liquid of foam-resistant;Wherein the quality of Pidolidone is The 20% of water quality, the amount of Pidolidone and the material of potassium carbonate is than for 2:1.005.
After solution clarification, take and test pH after a small amount of reacting liquid filtering roguing, and to correct reactant liquor pH be 8.0;Continue 85 Reacting 3 hours at DEG C, then by reactant liquor decolorization filtering, being concentrated in vacuo to mother-in-law U.S. degree is 37.6 ° of B é, and concentrated solution is cooled to temperature 16 DEG C, now material extremely thickness, but nodeless mesh separates out.
(2) directly carry out being spray-dried to obtain Pidolidone chelating potassium pressed powder at 70-80 DEG C by above-mentioned sticky material.
Comparative example 3
(1), reactor adds water, be equipped with motor stirring, be heated to temperature 75 DEG C, maintain stirring, add Pidolidone After, it being gradually added potassium carbonate, potassium carbonate need to be slowly added to, and spills with the too much feed liquid of foam-resistant;Wherein the quality of Pidolidone is The 20% of water quality, the amount of Pidolidone and the material of potassium carbonate is than for 2:1.005.
After solution clarification, take and test pH after a small amount of reacting liquid filtering roguing, and to correct reactant liquor pH be 7.0;By reactant liquor Decolorization filtering, being concentrated in vacuo to mother-in-law U.S. degree is 36-38 ° of B é, and concentrated solution is cooled to temperature 18 DEG C.
(2), the concentrated solution after cooling adds Pidolidone chelating potassium one water thing crystal to chelate as crystal seed, Pidolidone The w/v of potassium one water thing crystal and concentrated solution is 3:100, maintain temperature 16-18 DEG C, stirred crystallization 40 hours, blowing from Gains in depth of comprehension Pidolidone chelating potassium crude product, every 100kg crude product uses the rinsing of 8L deionized water, and the most box 80~85 DEG C of solid is dried About 8 hours, after moisture is qualified can with discharging, pack, seal.
The quality measurements of the Pidolidone chelating potassium that table 1 embodiment 1-3 and comparative example 1-3 prepare
Detection project Embodiment 1 Embodiment 2 Embodiment 3 Comparative example 1 Comparative example 2 Comparative example 3
Outward appearance White particle White particle White particle White particle White powder White particle
Optical rotation 23.8° 23.7° 23.8° 23.5° 23.6° 23.4°
Light transmittance 99% 99% 99% 98.5% 98.6% 97%
Water content 6.5% 6.4% 6.5% 7.8% 6.0% 7.9%
Chelating degree 97.6% 98.4% 96.7% 95.4% 96.2% 68.5%
Dissolvent residual 0 0 0 0.06% 0 0
Conclusion: the Pidolidone chelating potassium one water thing crystal that embodiment 1-3 prepares meets Japan's aginomoto company standard AJI97, does not use organic solvent in preparation process, reduce the safety coefficient in production process, and Pidolidone chelating potassium is brilliant In body, organic solvent-free residual, improves the quality of product, and the water content of crystal is easily controllable, the crystal that embodiment 1-3 prepares Water content stable.Owing to being not related to the main equipment of organic solvent and spray drying during extracting, take up an area the one-tenth of miscellaneous goods Originally it is greatly reduced.
Preparing Pidolidone chelating potassium one water thing crystal according to the method described in comparative example 1 has anhydrous ethanol solvent to remain, Obtained product moisture is higher, although qualified, but the upper limit index of closely≤8.0%, the most also have impact on it Printing opacity index;The Pidolidone chelating potassium of comparative example 2 preparation, the water content of the product of different batches is different, and difference compares Greatly, unstable, and equipment investment is big, cost is high, also due to spray drying temperature is higher, have impact on the printing opacity index of finished product; Comparative example 3 i.e. corrects after solution is clarified reactant liquor pH be 7.0, decolorization filtering, pH on the low side and lack chelating disadvantage in time In the chelating degree improving product.

Claims (7)

1. the method preparing Pidolidone chelating potassium one water thing, it is characterised in that comprise the following steps:
Step (1), with potassium carbonate or potassium hydroxide, Pidolidone as raw material, carry out with the water that temperature is 70~80 DEG C for solvent Reaction, the pH value of solution clarification post-equalization reactant liquor, to 7.5~8.5, continues to react at 80~85 DEG C 2~4 hours, then will Reactant liquor decolorization filtering, to be concentrated into mother-in-law U.S. degree be 36~38 ° of B é, and concentrated solution is cooled to temperature 15~20 DEG C;
Step (2), concentrated solution after cooling add Pidolidone chelating potassium one water thing crystal as crystal seed, maintain temperature 15 ~20 DEG C, stirred crystallization 36~48 hours, blowing is centrifugal that Pidolidone chelates potassium crude product, and every 100kg crude product uses 5~10L Deionized water rinses, and solid is dried at 80~85 DEG C and within 6~10 hours, obtains Pidolidone chelating potassium one water produce product.
The method preparing Pidolidone chelating potassium one water thing the most according to claim 1, it is characterised in that in step (1), The quality of described Pidolidone is the 20~25% of the quality of water;Pidolidone is 2:1 with the ratio of the amount of the material of potassium carbonate ~1.1;Pidolidone is 1:1~1.1 with the ratio of the amount of the material of potassium hydroxide.
The method preparing Pidolidone chelating potassium one water thing the most according to claim 2, it is characterised in that in step (1), The quality of described Pidolidone is the 20% of the quality of water;Pidolidone is 2:1.005 with the ratio of the amount of the material of potassium carbonate; Pidolidone is 1:1.01 with the ratio of the amount of the material of potassium hydroxide.
The method preparing Pidolidone chelating potassium one water thing the most according to claim 1, it is characterised in that in step (1), React with the water that temperature is 75 DEG C for solvent.
The method preparing Pidolidone chelating potassium one water thing the most according to claim 1, it is characterised in that in step (2), Described crystal seed Pidolidone chelating potassium one water thing crystal and the w/v of concentrated solution are 1~5:100.
The method preparing Pidolidone chelating potassium one water thing the most according to claim 5, it is characterised in that in step (2), Described crystal seed Pidolidone chelating potassium one water thing crystal and the w/v of concentrated solution are 3:100.
The method preparing Pidolidone chelating potassium one water thing the most according to claim 1, it is characterised in that in step (2), Every 100kg Pidolidone chelating potassium crude product uses 6~8L deionized water rinsings.
CN201610429682.7A 2016-06-17 2016-06-17 A kind of method preparing L glutamate chelate potassium one water thing Pending CN106117069A (en)

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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
CN108516949A (en) * 2018-04-27 2018-09-11 宜兴市前成生物有限公司 It is a kind of to prepare the chelated calcium method of L-Glutimic acid

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CN108516949A (en) * 2018-04-27 2018-09-11 宜兴市前成生物有限公司 It is a kind of to prepare the chelated calcium method of L-Glutimic acid

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Application publication date: 20161116