CN106117069A - Method for preparing L-glutamic acid chelated potassium monohydrate - Google Patents

Method for preparing L-glutamic acid chelated potassium monohydrate Download PDF

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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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potassium
glutamic acid
monohydrate
method
reaction
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CN201610429682.7A
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席日新
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宜兴市前成生物有限公司
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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 method for preparing L-glutamic acid chelated potassium monohydrate. The method comprises the following steps of performing a reaction by using potassium carbonate or potassium hydroxide, and L-glutamic acid as raw materials, and by using water of which the temperature is 70-80 DEG C as a solvent, clarifying a solution, adjusting the pH value of reaction liquid to 7.5-8.5, continuing a reaction at 80-85 DEG C for 2-4 hours, decoloring reaction liquid, performing filtration, performing concentration to a Baume degree of 36-38 degree Be, and then performing cooling to 15-20 DEG C; and adding L-glutamic acid chelated potassium monohydrate crystals as seed crystals to concentrated liquid, maintaining the temperature to be 15-20 DEG C, performing stirring for crystallization, performing discharging, performing centrifugation so as to obtain crude products, rinsing every 100 kg of the crude products with 5-10 L of deionized water, and drying solids so as to obtain products of which the chelating degree is 95% or above. According to the method disclosed by the invention, an organic solvent is not used, so that the safety coefficient of production environment is increased, and the cost of the raw materials is substantially reduced; the products are free from solvent residues, and moisture is easy to control; and besides, investment on equipment and sites can be reduced.

Description

技术领域 FIELD

[0001 ]本发明属于化学合成领域,具体涉及一种制备L-谷氨酸螯合钾一水物的方法。 [0001] The present invention belongs to the field of chemical synthesis, particularly the method relates to a monohydrate L- glutamic acid chelated potassium prepared. 一种制备L-谷氨酸螯合钾一水物的方法 The method of L- glutamic acid monohydrate for the preparation of chelated potassium

背景技术 Background technique

[0002] L-谷氨酸螯合钾一水物,是一种医药中间体,可用作食品添加剂和生物化学研究制剂,在调节心肌功能及电生理和治疗心脑血管疾病、低血钾等各种心率失常、肝炎、肝功能不全等方面有显著疗效。 [0002] L- glutamic acid monohydrate, potassium chelate, a pharmaceutical intermediates, can be used as a food additive formulation and biochemical research, and in the regulation of myocardial function and electrophysiological treatment of cardiovascular and cerebrovascular diseases, hypokalemia arrhythmia and other aspects of hepatitis, liver failure and other significant effect. 现有的生产工艺配料、浓缩完全一样,差异之处主要是提取方法的差异。 Ingredients conventional production process, was concentrated exactly the same, the main difference is the difference extraction method. 目前生产工艺中的提取L-谷氨酸螯合钾一水物工艺为:采用有机溶剂改变溶剂极性,从而使产品析出或者采用喷雾干燥的方法,直接获得成品。 Extraction L- present production process of potassium glutamate monohydrate process is a chelated: a polar organic solvent, changing the solvent, so that the product precipitated or spray drying, the finished product obtained directly. 第一种方法:使用有机溶剂, 降低了生产环境的安全系数,且所获得的产品中易残留有机溶剂,同时使用有机溶剂提取会增加生产成本。 The first method: using an organic solvent, reducing the safety factor of the production environment, and the products obtained tend to remain in the organic solvent, while an organic solvent extraction will increase production costs. 同时由于使用有机溶剂在产品烘干过程中产品的外观由于溶剂挥发带走少量结晶水而导致无光泽、流动性差;第二种提取方法设备、场地投大、生产成本高;所获得产品是粉末,毫无颗粒和流动性可言,水分含量不稳定,不易控制。 At the same time the use of organic solvents in the product during the drying process due to the appearance of the product took a few crystals solvent evaporation resulting in dull water, poor fluidity; second extraction equipment, facilities investment, high production costs; the product obtained is a powder , flowability and no particles at all, the moisture content is unstable and difficult to control.

发明内容 SUMMARY

[0003] 本发明的目的在于提供一种制备L-谷氨酸螯合钾一水物的方法。 [0003] The object of the present invention is to provide a method of chelated potassium L- glutamate monohydrate prepared.

[0004] 本发明的目的可以通过以下技术方案实现: [0004] The object of the present invention can be achieved by the following technical solution:

[0005] -种制备L-谷氨酸螯合钾一水物的方法,包括以下步骤: [0005] - Preparation of L- glutamic acid species chelated potassium monohydrate, comprising the steps of:

[0006] 步骤(1)、以碳酸钾或氢氧化钾、L-谷氨酸为原料,以温度为70~80°C的水为溶剂进行反应,溶液澄清后校正反应液的pH值至7.5~8.5,继续在80~85 °C下反应2~4小时,然后将反应液脱色过滤、浓缩至婆美度为36~38° Βέ,浓缩液冷却至温度15~20°C; [0006] Step (1), potassium carbonate or potassium hydroxide, L- glutamic acid as raw materials and the reaction temperature solvent is water 70 ~ 80 ° C, the correction of the pH of the reaction solution after the solution is clarified to 7.5 to 8.5, reaction was continued for 2 to 4 hours at 80 ~ 85 ° C, then the reaction solution was decolorized filtered and concentrated to a degree of PO US 36 ~ 38 ° Βέ, it was cooled and concentrated to a temperature of 15 ~ 20 ° C;

[0007] 步骤(2)、向降温后的浓缩液中加入L-谷氨酸螯合钾一水物晶体作为晶种,维持温度15~20°C,搅拌结晶36~48小时,放料离心得L-谷氨酸螯合钾粗品,每IOOkg粗品使用5~ IOL去离子水漂洗,固体在80~85°C干燥6~10小时得到L-谷氨酸螯合钾一水物产品。 [0007] Step (2), was added potassium chelate L- glutamate monohydrate crystals after cooling of the concentrated solution as a seed crystal, maintaining the temperature 15 ~ 20 ° C, crystallization was stirred 36 to 48 hours, from the discharge Reviews L- chelating crude potassium glutamate, each IOOkg used crude 5 ~ IOL rinsed with deionized water, the solid was dried 80 ~ 85 ° C 6 to 10 hours to give L- potassium glutamate monohydrate chelated products.

[0008] 步骤(1)中,所述的L-谷氨酸的质量为水的质量的20~25%,优选为20% ;L-谷氨酸与碳酸钾的物质的量之比为2:1~1.1,优选为2:1.005;L-谷氨酸与氢氧化钾的物质的量之比为1:1~1.1,优选为1:1.01。 [0008] Step (1), the mass of L- glutamic acid was 20 to 25% by weight of water, preferably 20%; the amount of L- glutamic acid and potassium carbonate material ratio of 2 : 1 to 1.1, preferably from 2: 1.005; and the amount of substance L- glutamic acid and potassium hydroxide is 1: 1 to 1.1, preferably 1: 1.01.

[0009] 步骤(1)中,优选以温度为75°C的水为溶剂进行反应。 [0009] Step (1), preferably at a temperature of 75 ° C water is a solvent for the reaction.

[0010] 步骤(2)中,所述的晶种L-谷氨酸螯合钾一水物晶体和浓缩液的重量体积比为1~ 5:100(g:mL或kg:L),优选为3:100。 [0010] Step (2), the weight ratio of the volume of the seed chelated potassium glutamate, L- monohydrate crystals and the concentrate is 1 ~ 5: 100 (g: mL or kg: L), preferably 3: 100. 本发明对L-谷氨酸螯合钾一水物晶体没有特别要求,只要是合格产品就可以作为晶种。 The present invention is not particularly required for L- potassium glutamate monohydrate crystals chelate, as long as the product can be qualified as a seed crystal.

[0011] 步骤(2)中,每IOOkgL-谷氨酸螯合钾粗品使用6~8L去离子水漂洗。 [0011] Step (2), each IOOkgL- chelated potassium glutamate used crude 6 ~ 8L deionized water rinse.

[0012]作为制备L-谷氨酸螯合钾一水物的优选方案,包括以下步骤: [0012] As a preferred embodiment the preparation of L- glutamic acid chelated potassium monohydrate, comprising the steps of:

[0013]步骤(1)、以碳酸钾或氢氧化钾、L-谷氨酸为原料,以温度为75 °C的水为溶剂进行反应,溶液澄清后校正反应液的pH值至8.0-8.5,继续在85 °C下反应2~4小时;然后将反应液脱色过滤、浓缩至婆美度为36-38°Βέ,浓缩液冷却至温度15-20°C。 [0013] Step (1), potassium carbonate or potassium hydroxide, L- glutamic acid as raw materials, the reaction is carried out at a temperature of 75 ° C the solvent is water, the correction of the reaction solution is then clarified solution to pH 8.0-8.5 , reaction was continued for 2 to 4 hours at 85 ° C; the reaction was then decolorized filtered and concentrated to a degree of beauty woman 36-38 ° Βέ, was cooled and concentrated to a temperature of 15-20 ° C.

[0014] 步骤(2)、浓缩液中加入L-谷氨酸螯合钾一水物晶体作为晶种,L-谷氨酸螯合钾一水物晶体和浓缩液的重量体积比为3:100,维持温度16~18°C,搅拌结晶40小时,放料离心得L-谷氨酸螯合钾粗品,每IOOkg粗品使用6~8L去离子水漂洗,固体普通箱式80~85°C干燥8小时左右得到L-谷氨酸螯合钾一水物产品。 [0014] Step (2), the concentrate was added potassium chelate L- glutamate monohydrate crystals as a seed, L- chelated potassium glutamate monohydrate crystals and the weight ratio of the concentrate volume ratio of 3: 100, maintaining the temperature 16 ~ 18 ° C, crystallization was stirred for 40 hours centrifuged to discharge L- glutamic acid chelated potassium crude each IOOkg used crude 6 ~ 8L deionized water rinse, ordinary solid box 80 ~ 85 ° C left dried for 8 hours to give L- chelated potassium glutamate monohydrate product.

[0015] 本发明的有益效果: [0015] Advantageous effects of the invention:

[0016]采用本发明方法制备L-谷氨酸螯合钾一水物,螯合度达到了95%以上,很好的解决了客户对于高螯合度L-谷氨酸钾一水物的需求。 [0016] L- glutamic acid was prepared using the method of the present invention chelated potassium monohydrate, chelating reaches 95% or more, a good solution to the needs of customers for high chelating L- potassium glutamate monohydrate thereof.

[0017] 客户对溶剂残留的要求越来越高,不使用溶剂是大势所趋,本发明不使用有机溶剂,提高了生产环境的安全系数,同时不使用有机溶剂也可以大幅度降低原料成本,降低成本约6000元/吨;同时确保产品无溶剂残留,水分易控制;且该方案的相对于喷雾干燥法,设备、场地投入比较小,可以降低约20%的设备投入。 [0017] customer requirements for increasingly high residual solvent, no solvent is the trend, the present invention does not use an organic solvent to improve the safety factor production environment, without the use of organic solvents may significantly reduce raw material costs, reduce costs about 6,000 yuan / ton; while ensuring that no solvent residue products, easy to control water; and with the regimen for a spray-drying method, equipment, facilities investment is relatively small and can be reduced by about 20% of equipment investment.

[0018] 具体表现为: [0018] Specific performance:

[0019] 1)体系pH偏碱性,同时维持反应3小时,使L-谷氨酸螯合钾一水物的螯合度由65% ~70%提高到了95%以上。 [0019] 1) System alkaline pH, while maintaining the reaction for 3 hours so that a chelate of chelate-L- potassium glutamate monohydrate is from 65% to 70% to 95%.

[0020] 2)投入1~5%的L-谷氨酸螯合钾一水物晶体作为晶种,诱导L-谷氨酸螯合钾结晶。 [0020] 2) 1 to 5% into L- chelated potassium glutamate monohydrate crystals as a seed, L- glutamic acid chelated potassium induce crystallization.

[0021] 3)维持结晶温度15~20°C,是确保L-谷氨酸螯合钾尽可能多的结晶出来,同时维持36~48小时是确保产品结晶形态好,物料表面所含母液少,这样可以直接采用普通烘箱烘干。 [0021] 3) maintaining the crystallization temperature is 15 ~ 20 ° C, to ensure that as much of L- glutamic acid chelated potassium crystallizes out, while maintaining 36 to 48 hours to ensure a good product is a crystalline form, the mother liquor contains less material surface such conventional oven drying can be used directly.

[0022] 4)固液离心分离时使用少量去离子水洗涤确保物料表面尽可能的少带母液,烘干后广品外观白壳、流动性好。 [0022] 4) the use of a small amount of solid-liquid separation by centrifugation of deionized water to ensure that the surface of the material as little as possible with the mother liquor, dried and wide Appearance white shell, fluidity.

具体实施方式 Detailed ways

[0023]下面通过具体实施方式对本发明的技术方案作进一步说明。 [0023] DETAILED DESCRIPTION by the following further description of the technical solution of the present invention.

[0024] 实施例1 [0024] Example 1

[0025] 一种制备L-谷氨酸螯合钾一水物的方法,包括以下步骤: Method [0025] L- glutamic acid chelated potassium preparing a monohydrate, comprising the steps of:

[0026] (1)、反应釜中加入水,配备电机搅拌,加热至温度75°C,维持搅拌,加入L-谷氨酸后,逐步加入碳酸钾,碳酸钾需缓慢加入,以防泡沫过多料液溅出;其中L-谷氨酸的质量为水质量的20%,L-谷氨酸与碳酸钾的物质的量之比为2:1.005。 [0026] (1), water was added to the reaction kettle, equipped with a stirring machine, heated to a temperature of 75 ° C, stirring is maintained after addition of L- glutamic acid, was gradually added potassium carbonate, potassium carbonate was added slowly required to prevent excessive foam multi-feed liquid spill; wherein L- glutamic acid by mass of 20% by mass of water, the ratio of the amount of L- glutamic acid and potassium carbonate substance is 2: 1.005.

[0027] 溶液澄清后,取少量反应液过滤去杂后测试pH,并校正反应液pH为8.0;继续在85 °C下反应3小时;然后将反应液脱色过滤,真空浓缩至婆美度为37.6° Βέ,浓缩液冷却至温度18。 [0027] After the solution clarified, small amount of the reaction solution was filtered test pH after going heteroaryl, and corrects the reaction at pH 8.0; continued at 85 ° C for 3 hours; then the reaction solution was decolorized filtered, and concentrated in vacuo to a woman US degree 37.6 ° Βέ, was cooled and concentrated to a temperature of 18. . .

[0028] (2)、向降温后的浓缩液中加入L-谷氨酸螯合钾一水物晶体作为晶种,L-谷氨酸螯合钾一水物晶体和浓缩液的重量体积比为3:100,维持温度16~18°C,搅拌结晶40小时,放料离心得L-谷氨酸螯合钾粗品,每IOOkg粗品使用8L去离子水漂洗,固体普通箱式80~85°C 干燥8小时左右,水分合格后可以出料、装袋、密封。 [0028] (2) adding a water-L- glutamic acid chelated potassium crystals after cooling of the concentrated solution as the seed, the weight of the volume of L- glutamic acid chelated potassium monohydrate crystals and concentrated liquid ratio 3: 100, maintaining the temperature 16 ~ 18 ° C, crystallization was stirred for 40 hours centrifuged to discharge L- chelating crude potassium glutamate, each IOOkg used crude 8L deionized water rinse, ordinary solid box 80 ~ 85 ° C and dried about 8 hours, the feed water passing can, bagged, sealed.

[0029] 实施例2 [0029] Example 2

[0030] 一种制备L-谷氨酸螯合钾一水物的方法,包括以下步骤: Method [0030] L- glutamic acid chelated potassium preparing a monohydrate, comprising the steps of:

[0031] (1 )、反应釜中加入水,配备电机搅拌,加热至温度75 °C,维持搅拌,加入L-谷氨酸后,逐步加入氢氧化钾,氢氧化钾需缓慢加入,以防泡沫过多料液溅出;其中L-谷氨酸的质量为水质量的20%,L-谷氨酸与氢氧化钾的物质的量比为I: 1.0 l。 [0031] (1), water was added to the reaction kettle, equipped with a stirring machine, heated to a temperature of 75 ° C, stirring is maintained after addition of L- glutamic acid, potassium hydroxide was gradually added, was slowly added potassium hydroxide required to prevent excessive foam liquid spill; L- glutamic acid in which the mass is 20% by mass of water, the molar ratio of L- glutamic acid and potassium hydroxide to I: 1.0 l.

[0032] 溶液澄清后,取少量反应液过滤去杂后测试pH,并校正反应液pH为8.0;继续在85 °C下反应3小时;然后将反应液脱色过滤,真空浓缩至婆美度为37.2° Βέ,浓缩液冷却至温度18。 [0032] After the solution clarified, small amount of the reaction solution was filtered test pH after going heteroaryl, and corrects the reaction at pH 8.0; continued at 85 ° C for 3 hours; then the reaction solution was decolorized filtered, and concentrated in vacuo to a woman US degree 37.2 ° Βέ, was cooled and concentrated to a temperature of 18. . .

[0033] (2 )、向降温后的浓缩液中加入L-谷氨酸螯合钾一水物晶体作为晶种,L-谷氨酸螯合钾一水物晶体和浓缩液的重量体积比为3:100,维持温度16~18°C,搅拌结晶40小时,放料离心得L-谷氨酸螯合钾粗品,每IOOkg粗品使用8L去离子水漂洗,固体普通箱式80~85°C 干燥8小时左右,水分合格后可以出料、装袋、密封。 [0033] (2) adding a water-L- glutamic acid chelated potassium crystals after cooling of the concentrated solution as the seed, the weight of the volume of L- glutamic acid chelated potassium monohydrate crystals and concentrated liquid ratio 3: 100, maintaining the temperature 16 ~ 18 ° C, crystallization was stirred for 40 hours centrifuged to discharge L- chelating crude potassium glutamate, each IOOkg used crude 8L deionized water rinse, ordinary solid box 80 ~ 85 ° C and dried about 8 hours, the feed water passing can, bagged, sealed.

[0034] 实施例3 [0034] Example 3

[0035] 一种制备L-谷氨酸螯合钾一水物的方法,包括以下步骤: Method [0035] L- glutamic acid chelated potassium preparing a monohydrate, comprising the steps of:

[0036] (1)、反应釜中加入水,配备电机搅拌,加热至温度75°C,维持搅拌,加入L-谷氨酸后,逐步加入碳酸钾,碳酸钾需缓慢加入,以防泡沫过多料液溅出;其中L-谷氨酸的质量为水质量的20%,L-谷氨酸与碳酸钾的物质的量比为2:1.005。 [0036] (1), water was added to the reaction kettle, equipped with a stirring machine, heated to a temperature of 75 ° C, stirring is maintained after addition of L- glutamic acid, was gradually added potassium carbonate, potassium carbonate was added slowly required to prevent excessive foam multi-feed liquid spill; wherein L- glutamic acid by mass of 20% by mass of water, the molar ratio of L- glutamic acid and potassium carbonate is 2: 1.005.

[0037] 溶液澄清后,取少量反应液过滤去杂后测试pH,并校正反应液pH为8.2;继续在85 °C下反应3小时;然后将反应液脱色过滤,真空浓缩至婆美度为37.6° Βέ,浓缩液冷却至温度16。 [0037] After the solution clarified, small amount of the reaction solution was filtered test pH after going heteroaryl, and corrects the reaction solution at pH 8.2; continued at 85 ° C for 3 hours; then the reaction solution was decolorized filtered, and concentrated in vacuo to a woman US degree 37.6 ° Βέ, was cooled and concentrated to a temperature of 16. . .

[0038] (2)、降温后的浓缩液中加入L-谷氨酸螯合钾一水物晶体作为晶种,L-谷氨酸螯合钾一水物晶体和浓缩液的重量体积比为5:100,维持温度16~18°C,搅拌结晶40小时,放料离心得L-谷氨酸螯合钾粗品,每IOOkg粗品使用6L去离子水漂洗,固体普通箱式80~85°C干燥8小时左右,水分合格后可以出料、装袋、密封。 [0038] (2), after cooling the concentrated solution was added potassium chelate L- glutamate monohydrate crystals as a seed, the weight ratio of the volume of L- glutamic acid chelated potassium monohydrate crystals and the concentrate of 5: 100, maintaining the temperature 16 ~ 18 ° C, crystallization was stirred for 40 hours centrifuged to discharge L- glutamic acid chelated potassium crude product, was used crude 6L each IOOkg rinsed with deionized water, ordinary solid box 80 ~ 85 ° C dried about 8 hours, the feed water passing can, bagged, sealed.

[0039] 对比例1 [0039] Comparative Example 1

[0040] (1)、反应釜中加入水,配备电机搅拌,加热至温度75°C,维持搅拌,加入L-谷氨酸后,逐步加入碳酸钾,碳酸钾需缓慢加入,以防泡沫过多料液溅出;其中L-谷氨酸的质量为水质量的20%,L-谷氨酸与碳酸钾的物质的量比为2:1.005。 [0040] (1), water was added to the reaction kettle, equipped with a stirring machine, heated to a temperature of 75 ° C, stirring is maintained after addition of L- glutamic acid, was gradually added potassium carbonate, potassium carbonate was added slowly required to prevent excessive foam multi-feed liquid spill; wherein L- glutamic acid by mass of 20% by mass of water, the molar ratio of L- glutamic acid and potassium carbonate is 2: 1.005.

[00411 溶液澄清后,取少量反应液过滤去杂后测试pH,并校正反应液pH为8.1;继续在85 °C下反应3小时;然后将反应液脱色过滤,真空浓缩至婆美度为37.6° Βέ,浓缩液冷却至温度16。 [00411 solution was clarified small amount of the reaction solution was filtered test pH after going heteroaryl, and corrects the reaction solution at pH 8.1; the reaction was continued at 85 ° C 3 hours; then the reaction solution was decolorized filtered, and concentrated in vacuo to a woman Mido 37.6 ° Βέ, it was cooled and concentrated to a temperature of 16. . .

[0042] (2)、向反应釜中加入无水乙醇,浓缩液和无水乙醇的体积比为1:3,搅拌2日后逐步有L-谷氨酸螯合钾晶体析出,10小时后进行离心分离,在50-60°C真空烘箱中烘干取得L-谷氨酸螯合钾成品。 [0042] (2), was added to the kettle over anhydrous ethanol, the volume ratio of ethanol and the solution was concentrated to 1: 3, with a gradual stirring for 2 days L- glutamic acid crystals were precipitated potassium chelate, 10 hours centrifugal separation, and drying to obtain the finished product L- glutamic acid chelated potassium 50-60 ° C vacuum oven.

[0043] 对比例2 [0043] Comparative Example 2

[0044] (1)、反应釜中加入水,配备电机搅拌,加热至温度75°C,维持搅拌,加入L-谷氨酸后,逐步加入碳酸钾,碳酸钾需缓慢加入,以防泡沫过多料液溅出;其中L-谷氨酸的质量为水质量的20%,L-谷氨酸与碳酸钾的物质的量比为2:1.005。 [0044] (1), water was added to the reaction kettle, equipped with a stirring machine, heated to a temperature of 75 ° C, stirring is maintained after addition of L- glutamic acid, was gradually added potassium carbonate, potassium carbonate was added slowly required to prevent excessive foam multi-feed liquid spill; wherein L- glutamic acid by mass of 20% by mass of water, the molar ratio of L- glutamic acid and potassium carbonate is 2: 1.005.

[0045] 溶液澄清后,取少量反应液过滤去杂后测试pH,并校正反应液pH为8.0;继续在85 °C下反应3小时,然后将反应液脱色过滤,真空浓缩至婆美度为37.6° Βέ,浓缩液冷却至温度16 °C,此时物料极为粘稠,但无结晶析出。 [0045] The solution is then clarified, small amount of the reaction solution was filtered test pH after going heteroaryl, and corrects the reaction at pH 8.0; continued at 85 ° C for 3 hours, then the reaction solution was decolorized filtered, and concentrated in vacuo to a woman US degree 37.6 ° Βέ, was cooled and concentrated to a temperature of 16 ° C, this time is extremely viscous material, without crystallization.

[0046] (2)将上述粘稠物料在70_80°C直接进行喷雾干燥得L-谷氨酸螯合钾固体粉末。 [0046] (2) The above spray-drying sticky materials L- glutamate, potassium chelate solid powder directly 70_80 ° C.

[0047] 对比例3 [0047] Comparative Example 3

[0048] (I)、反应釜中加入水,配备电机搅拌,加热至温度75°C,维持搅拌,加入L-谷氨酸后,逐步加入碳酸钾,碳酸钾需缓慢加入,以防泡沫过多料液溅出;其中L-谷氨酸的质量为水质量的20%,L-谷氨酸与碳酸钾的物质的量比为2:1.005。 [0048] (I), water was added to the reaction kettle, equipped with a stirring machine, heated to a temperature of 75 ° C, stirring is maintained after addition of L- glutamic acid, was gradually added potassium carbonate, potassium carbonate was added slowly required to prevent excessive foam multi-feed liquid spill; wherein L- glutamic acid by mass of 20% by mass of water, the molar ratio of L- glutamic acid and potassium carbonate is 2: 1.005.

[0049]溶液澄清后,取少量反应液过滤去杂后测试pH,并校正反应液pH为7.0 ;将反应液脱色过滤,真空浓缩至婆美度为36-38° Βέ,浓缩液冷却至温度18°C。 [0049] After the solution was clarified by filtration small amount of the reaction solution after the pH was tested to miscellaneous, and corrects the reaction solution at pH 7.0; decolorized reaction solution was filtered, concentrated under vacuum to a degree of beauty woman 36-38 ° Βέ, was cooled to a temperature and concentrated 18 ° C.

[0050] (2)、降温后的浓缩液中加入L-谷氨酸螯合钾一水物晶体作为晶种,L-谷氨酸螯合钾一水物晶体和浓缩液的重量体积比为3:100,维持温度16-18°C,搅拌结晶40小时,放料离心得L-谷氨酸螯合钾粗品,每IOOkg粗品使用8L去离子水漂洗,固体普通箱式80~85°C干燥8小时左右,水分合格后可以出料、装袋、密封。 [0050] (2), after cooling the concentrated solution was added potassium chelate L- glutamate monohydrate crystals as a seed, the weight ratio of the volume of L- glutamic acid chelated potassium monohydrate crystals and the concentrate of 3: 100, maintaining a temperature of 16-18 ° C, crystallization was stirred for 40 hours centrifuged to discharge L- glutamic acid chelated potassium crude product, was used crude each IOOkg 8L deionized water rinse, ordinary solid box 80 ~ 85 ° C dried about 8 hours, the feed water passing can, bagged, sealed.

[00511表1实施例1-3和对比例1-3制得的L-谷氨酸螯合钾的质量检测结果 [00511 Table 1 mass detection result and L- potassium glutamate 1-3 Comparative Examples 1-3 prepared chelating embodiment

Figure CN106117069AD00061

L0053J 结论:实施例1-3制得的L-谷氨酸螯合钾一水物晶体符合ϋ本味之素企业标准AJI97,制备过程中不使用有机溶剂,降低了生产过程中的安全系数,且L-谷氨酸螯合钾晶体中无有机溶剂残留,提高了产品的质量,晶体的含水量易于控制,实施例1-3制得的晶体的含水量稳定。 L0053J Conclusion: L- glutamic acid chelated potassium embodiments obtained in Example 1-3 monohydrate crystals meet ϋ present Ajinomoto AJI97 enterprise standards, without using an organic solvent in the preparation process, the safety factor is reduced in the production process, potassium glutamate and L- chelate crystals free of organic solvent residue, improved product quality, is easy to control the water content of the crystals, the water content of the crystals obtained in Example 1-3 stabilization system embodiments. 由于提取过程中不涉及有机溶剂及喷雾干燥的大型设备,占地小产品的成本有大幅降低。 Since the extraction process does not involve spray-drying organic solvent and a large equipment cost, small footprint products are significantly reduced.

[0054]按照对比例1所述的方法制备L-谷氨酸螯合钾一水物晶体有无水乙醇溶剂残留, 所制得的产品水分比较高,虽然合格,但是非常接近<8.0%的上限指标,同样也影响了其透光指标;对比例2制备的L-谷氨酸螯合钾,不同批次的产品的含水量不同,而且差别比较大,不稳定,且设备投入大,成本高,同样由于喷雾干燥温度较高,影响了成品的透光指标; 对比例3中待溶液澄清后即校正反应液pH为7.0、脱色过滤,偏低的pH和缺少螯合时间不利于提尚广品的整合度。 [0054] L- glutamic acid chelated potassium prepared according to the method described in Comparative Example 1 crystals have a water residual solvent ethanol, the product obtained is relatively high moisture, while passing, but very close to <8.0% Maximum index, which also affects the light-transmitting index; L- glutamic acid chelated potassium Comparative preparation 2, the water content of different batches of different products, and the difference is relatively large, unstable and a large equipment investment cost high, also due to the higher spray-drying temperature, the light-transmitting index of the finished product; Comparative Example 3, the reaction solution cleared after the correction of pH to 7.0, filter bleaching, low pH and lack of time is not conducive to chelating still mention wide degree of integration products.

Claims (7)

1. 一种制备L-谷氨酸螯合钾一水物的方法,其特征在于包括以下步骤: 步骤(1)、以碳酸钾或氢氧化钾、L-谷氨酸为原料,以温度为70~80 °C的水为溶剂进行反应,溶液澄清后校正反应液的pH值至7.5~8.5,继续在80~85 °C下反应2~4小时,然后将反应液脱色过滤、浓缩至婆美度为36~38° Βέ,浓缩液冷却至温度15~20°C; 步骤(2)、向降温后的浓缩液中加入L-谷氨酸螯合钾一水物晶体作为晶种,维持温度15 ~20 °C,搅拌结晶36~48小时,放料离心得L-谷氨酸螯合钾粗品,每100kg粗品使用5~10L 去离子水漂洗,固体在80~85°C干燥6~10小时得到L-谷氨酸螯合钾一水物产品。 Method L- chelated potassium glutamate monohydrate for the preparation of, comprising the following steps: Step (1), potassium carbonate or potassium hydroxide, L- glutamic acid as raw materials, to a temperature of water 70 ~ 80 ° C is carried out for the reaction solvent, the correction of the reaction solution after the solution is clear to pH 7.5 to 8.5, the reaction was continued at 80 ~ 85 ° C 2 ~ 4 hours, then the reaction solution was decolorized filtered and concentrated to po Mido is 36 ~ 38 ° Βέ, was cooled and concentrated to a temperature of 15 ~ 20 ° C; step (2), was added potassium chelate L- glutamate monohydrate crystals after cooling of the concentrated solution as a seed crystal, maintaining the temperature 15 ~ 20 ° C, crystallization was stirred 36 to 48 hours, centrifuged to discharge L- glutamic acid chelated potassium crude product is used per 100kg crude 5 ~ 10L rinsed with deionized water, the solid was dried 80 ~ 85 ° C ~ 6 10 hours to give L- glutamic acid chelated potassium monohydrate product.
2. 根据权利要求1所述的制备L-谷氨酸螯合钾一水物的方法,其特征在于步骤(1)中, 所述的L-谷氨酸的质量为水的质量的20~25% ;L-谷氨酸与碳酸钾的物质的量之比为2:1 ~1.1 ;L-谷氨酸与氢氧化钾的物质的量之比为1:1~1.1。 The preparation of claim 1 L- potassium glutamate monohydrate chelate method as claimed in claim, wherein step (1), the mass of the mass of L- glutamic acid - water 20 25%; the amount of L- glutamic acid and potassium carbonate material ratio of 2: 1 to 1.1; the amount of the substance L- glutamic acid and potassium hydroxide is 1: 1 to 1.1.
3. 根据权利要求2所述的制备L-谷氨酸螯合钾一水物的方法,其特征在于步骤(1)中, 所述的L-谷氨酸的质量为水的质量的20% ;L-谷氨酸与碳酸钾的物质的量之比为2:1.005; L-谷氨酸与氢氧化钾的物质的量之比为1:1.01。 The preparation of L- glutamic acid chelated potassium 2 according to the method as claimed in claim monohydrate, wherein the step (1), the mass of L- glutamic acid of 20% by mass of water ; amount-of-substance ratio of L- glutamic acid and potassium carbonate is 2: 1.005; and the amount of substance of L- glutamic acid and potassium hydroxide is 1: 1.01.
4. 根据权利要求1所述的制备L-谷氨酸螯合钾一水物的方法,其特征在于步骤(1)中, 以温度为75 °C的水为溶剂进行反应。 The preparation of claim 1 L- potassium glutamate monohydrate chelate method as claimed in claim, wherein step (1) to a temperature of 75 ° C water as a solvent for the reaction.
5. 根据权利要求1所述的制备L-谷氨酸螯合钾一水物的方法,其特征在于步骤(2)中, 所述的晶种L-谷氨酸螯合钾一水物晶体和浓缩液的重量体积比为1~5:100。 The preparation of claim 1 L- potassium glutamate monohydrate chelate method as claimed in claim, wherein step (2), the seed L- chelated potassium glutamate monohydrate crystals and a concentrated liquid weight to volume ratio of 1 to 5: 100.
6. 根据权利要求5所述的制备L-谷氨酸螯合钾一水物的方法,其特征在于步骤(2)中, 所述的晶种L-谷氨酸螯合钾一水物晶体和浓缩液的重量体积比为3:100。 6. The method of producing L- potassium glutamate, 5 chelate monohydrate as claimed in claim, wherein step (2), the seed L- chelated potassium glutamate monohydrate crystals and the volume of concentrate weight ratio of 3: 100.
7. 根据权利要求1所述的制备L-谷氨酸螯合钾一水物的方法,其特征在于步骤(2)中, 每100kg L-谷氨酸螯合钾粗品使用6~8L去离子水漂洗。 The preparation of claim 1 L- potassium glutamate monohydrate chelate method as claimed in claim, wherein step (2) per 100kg L- glutamic acid chelate used crude potassium 6 ~ 8L deionized water rinse.
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