CN104177280A - Production process of methionine - Google Patents

Production process of methionine Download PDF

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Publication number
CN104177280A
CN104177280A CN201310194709.5A CN201310194709A CN104177280A CN 104177280 A CN104177280 A CN 104177280A CN 201310194709 A CN201310194709 A CN 201310194709A CN 104177280 A CN104177280 A CN 104177280A
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China
Prior art keywords
methionine
met
solution
reverse osmosis
inorganic salt
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Pending
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CN201310194709.5A
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Chinese (zh)
Inventor
卢伯福
陈洪景
虞美辉
李振峰
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XIAMEN STARMEM FILM TECHNOLOGY Co Ltd
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XIAMEN STARMEM FILM TECHNOLOGY Co Ltd
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Priority to CN201310194709.5A priority Critical patent/CN104177280A/en
Publication of CN104177280A publication Critical patent/CN104177280A/en
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Abstract

The invention discloses a production process of methionine. The production process is characterized by comprising the following steps of (1) separating a methionine crystallization mother liquor through a continuous chromatographic separation system filled with a sodium or potassium type chromatography resin to obtain a methionine solution and an inorganic salt solution or a sodium chloride solution; and (2) concentrating the methionine solution by using a reverse osmosis system to obtain a methionine reverse osmosis concentrate, and returning the methionine reverse osmosis concentrate to a crystallization process. With the above technical solution, the production process of methionine comprises the steps of subjecting the crystallization mother liquor to continuous chromatographic separation and reverse osmosis concentration successively and returning the concentrate to the crystallization process. The production process has the advantages of simple process, good separation effect, high methionine purity and low concentration cost.

Description

A kind of methionine(Met) production technique
Technical field
The present invention relates to methionine(Met) field, particularly a kind of methionine(Met) production technique.
Background technology
At present the conventional method of preparing methionine(Met) is mainly that the solution that Sodium L-methioninate obtains after being neutralized by acid mainly contains methionine(Met) and inorganic salt, is then separated and obtains methionine(Met) with crystalline form by crystallization by under acidic conditions and Sodium L-methioninate solution.In crystalline mother solution after crystallization, still contain a certain amount of methionine(Met) and inorganic salt, therefore, preferably by crystalline mother solution recycling.Conventional method is by all crystalline mother solution recyclings at present, but along with the impurity in circulating mother liquor (organic impurity in this mother liquor and sodium-chlor, sodium sulfate, salt of wormwood etc.) accumulation, need to discharge with specified amount.But the measure that has been not as discharging of waste liquid mother liquor because this has caused the methionine(Met) that wherein comprises and the loss of inorganic salt, and the cost disposing waste liquid and consumptive material very high, can increase environmental protection cost and reduce the yield of methionine(Met) and inorganic salt.
Method and the device of impurity in a kind of removal two grade methionine mother liquors are disclosed in the Chinese invention patent application " removing method and the device of impurity in two grade methionine mother liquors " that Luo Yuping, poplar equality are 201210317849.2 at application number: two grade methionine mother liquors are heated to 30 ~ 100 DEG C, then in every liter of two grade methionine mother liquors, add 1 ~ 10g sorbent material, insulation absorption 10min ~ 90min, two grade methionine mother liquors after last Filtration Adsorption, described sorbent material is diatomite, gac or atlapulgite; The inventive system comprises pending mother liquor holding tank, adsorption tanks, strainer and finished mother liquid storage tank, described pending mother liquor holding tank is communicated with the entrance of adsorption tanks, the outlet of described adsorption tanks is communicated with the entrance of strainer, and the filtrate outlet of described strainer is communicated with finished mother liquid storage tank; The present invention is compared with discharging the method for mother liquor in prior art, reduce the impurities accumulation in mother liquor, obtain the higher mother liquor of quality, thereby improved the yield of methionine(Met) and inorganic salt, reclaimed by the higher mother liquor of quality the methionine(Met) that obtains and the quality product of inorganic salt is optimized more simultaneously.But aforesaid method, adopt sorbent material in absorption impurity, also some methionine and inorganic salt have been adsorbed, affect the yield of product, and in prior art, from methionine(Met) and sulfuric acid mixture liquid, the method for separating inorganic salts still adopts the mode of evaporative crystallization, and which has the shortcomings such as concentrated cost height.
Summary of the invention
The object of the present invention is to provide a kind of good separating effect, methionine(Met) production technique that concentrated cost is low.
For achieving the above object, technical scheme proposed by the invention is: a kind of methionine(Met) production technique, it is characterized in that, and comprise the steps:
Step 1: methionine(Met) crystalline mother solution is separated by the continuous chromatography separation system that is filled with sodium type or potassium type chromatography resin, obtain methionine solution and inorganic salt solution;
Step 2: adopt reverse osmosis system to concentrate to obtain methionine(Met) reverse osmosis concentrated liquid methionine solution, the methionine(Met) reverse osmosis concentrated liquid obtaining is returned to Crystallization Procedure.
Further, also comprise that one obtains inorganic salt solution the step of inorganic salt crystal by evaporative crystallization.
The inorganic salt of the methionine(Met) that further, contains 2-4% massfraction in described methionine(Met) crystalline mother solution and 5-15% massfraction left and right.
Further, described inorganic salt are sodium sulfate or sodium-chlor.
Further, the purity of the middle methionine(Met) of the methionine solution after described continuous chromatography separation system separation is that more than 97% mass concentration is at 1-2%.
Further, the mass concentration of the middle inorganic salt of the inorganic salt solution after described continuous chromatography separation system separates is 5-7%, and purity is more than 95%.
Further, in described methionine(Met) reverse osmosis concentrated liquid, the mass concentration of methionine(Met) is 2-4%.
Adopt technique scheme, methionine(Met) production technique of the present invention, separates crystalline mother solution and reverse osmosis concentration by continuous chromatography successively, has the advantages such as technique is simple, good separating effect, and methionine(Met) purity is high, concentrated cost is low.
Embodiment
Below in conjunction with specific embodiment, the present invention will be further described.
Embodiment 1
Step 1: get methionine(Met) crystalline mother solution, contain the methionine(Met) of 3% massfraction and the sodium sulfate of 15% massfraction in crystalline mother solution, crystalline mother solution separates by the continuous chromatography separation system that is filled with sodium type chromatography resin, obtains methionine solution and inorganic salt solution; The purity of the middle methionine(Met) of the methionine solution of gained is 98%, and mass concentration is 1%; The mass concentration 10% of the middle sodium sulfate of metabisulfite solution, purity 95%;
Step 2: adopt reverse osmosis system to concentrate to obtain methionine(Met) reverse osmosis concentrated liquid methionine solution; In methionine(Met) reverse osmosis concentrated liquid, the mass concentration of methionine(Met) is 3%; The methionine(Met) reverse osmosis concentrated liquid obtaining is returned to Crystallization Procedure;
Preferably, can also be by metabisulfite solution by the step of the sodium sulfate crystal of evaporative crystallization.
Embodiment 2
Step 1: get methionine(Met) crystalline mother solution, contain the methionine(Met) of 2% massfraction and the sodium-chlor of 5% massfraction in crystalline mother solution, crystalline mother solution separates by the continuous chromatography separation system that is filled with potassium type chromatography resin, obtains methionine solution and sodium chloride solution; The purity of the middle methionine(Met) of the methionine solution of gained is 97%, and mass concentration is 2%; The mass concentration 7% of the middle sodium-chlor of sodium chloride solution, purity 96%;
Step 2: adopt reverse osmosis system to concentrate to obtain methionine(Met) reverse osmosis concentrated liquid methionine solution; In methionine(Met) reverse osmosis concentrated liquid, the mass concentration of methionine(Met) is 4%; The methionine(Met) reverse osmosis concentrated liquid obtaining is returned to Crystallization Procedure.
Embodiment 3
Step 1: get methionine(Met) crystalline mother solution, contain the methionine(Met) of 4% massfraction and the sodium sulfate of 10% massfraction in crystalline mother solution, crystalline mother solution separates by the continuous chromatography separation system that is filled with sodium type chromatography resin, obtains methionine solution and metabisulfite solution; The purity of the middle methionine(Met) of the methionine solution of gained is 99%, and mass concentration is 2%; The mass concentration 6% of the middle sodium sulfate of metabisulfite solution, purity 97%;
Step 2: adopt reverse osmosis system to concentrate to obtain methionine(Met) reverse osmosis concentrated liquid methionine solution; In methionine(Met) reverse osmosis concentrated liquid, the mass concentration of methionine(Met) is 4%; The methionine(Met) reverse osmosis concentrated liquid obtaining is returned to Crystallization Procedure.
In the above-described embodiments, only the present invention has been carried out to exemplary description, but those skilled in the art are reading after present patent application and can carry out various amendments to the present invention without departing from the spirit and scope of the present invention.

Claims (7)

1. a methionine(Met) production technique, is characterized in that, comprises the steps:
Step 1: methionine(Met) crystalline mother solution is separated by the continuous chromatography separation system that is filled with sodium type or potassium type chromatography resin, obtain methionine solution and inorganic salt solution;
Step 2: adopt reverse osmosis system to concentrate to obtain methionine(Met) reverse osmosis concentrated liquid methionine solution; The methionine(Met) reverse osmosis concentrated liquid obtaining is returned to Crystallization Procedure.
2. a kind of methionine(Met) production technique according to claim 1, is characterized in that, also comprises that one obtains inorganic salt solution the step of inorganic salt crystal by evaporative crystallization.
3. a kind of methionine(Met) production technique according to claim 1, is characterized in that, described inorganic salt are sodium-chlor or sodium sulfate.
4. a kind of methionine(Met) production technique according to claim 1, is characterized in that, the methionine(Met) that contains 2-4% mass concentration in described methionine(Met) crystalline mother solution and the inorganic salt of 5-15% mass concentration.
5. a kind of methionine(Met) production technique according to claim 1, is characterized in that, the purity of the middle methionine(Met) of the methionine solution after described continuous chromatography separation system separates is more than 97%, and mass concentration is 1-2%.
6. a kind of methionine(Met) production technique according to claim 1, is characterized in that, the mass concentration 5-7% of the middle inorganic salt of the inorganic salt solution after described continuous chromatography separation system separates, and purity is more than 95%.
7. a kind of methionine(Met) production technique according to claim 1, is characterized in that, in described methionine(Met) reverse osmosis concentrated liquid, the mass concentration of methionine(Met) is 2-4%.
CN201310194709.5A 2013-05-23 2013-05-23 Production process of methionine Pending CN104177280A (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104926701A (en) * 2015-06-30 2015-09-23 西安蓝晓科技新材料股份有限公司 Purification process of methionine
CN106380433A (en) * 2016-08-26 2017-02-08 宁夏紫光天化蛋氨酸有限责任公司 Separation and purification method for N-acetyl-D, L-methionine
CN106432018A (en) * 2016-09-14 2017-02-22 宁夏紫光天化蛋氨酸有限责任公司 Method for environment-friendly clean production of D,L-methionine
CN106631855A (en) * 2016-12-09 2017-05-10 三达膜科技(厦门)有限公司 Method or recycling threonine from threonine crystallization mother solution
CN108623504A (en) * 2017-03-16 2018-10-09 诺华赛分离技术(上海)有限公司 Purify 2- hydroxyls -4- (methyl thio) butyric acid with chromatography
US10669233B2 (en) 2017-12-28 2020-06-02 Sunresin New Materials Co. Ltd., Xi'an Process of purifying methionine
CN112645357A (en) * 2020-12-22 2021-04-13 宁夏紫光天化蛋氨酸有限责任公司 Post-treatment method of sodium sulfate mother liquor
CN112679397A (en) * 2020-12-21 2021-04-20 宁夏紫光天化蛋氨酸有限责任公司 Preparation method of DL-methionine
US11242316B2 (en) * 2017-03-16 2022-02-08 Adisseo France S.A.S. Method for manufacturing 2-hydroxy-4-(methylthio)butyric acid
CN114057618A (en) * 2021-12-10 2022-02-18 宁夏紫光天化蛋氨酸有限责任公司 Methionine optimized preparation method based on sulfuric acid indirect acidification method

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FR2772026A1 (en) * 1997-12-05 1999-06-11 Rhone Poulenc Nutrition Animal Preparation of methionine or its hydroxy analog using cation exchange resin
CN1950327A (en) * 2004-04-07 2007-04-18 旭化成化学株式会社 Method of purifying amino acid
CN101503366A (en) * 2009-03-11 2009-08-12 无锡晶海氨基酸有限公司 Method for extracting and separating L-valine by membrane separation and plant chromatography separation
CN101735135A (en) * 2009-12-02 2010-06-16 厦门世达膜科技有限公司 Method for concentrating 5-hydroxyl tryptophan
CN102688610A (en) * 2012-06-19 2012-09-26 华东理工大学 Chromatographic separation method of glycine and inorganic salt
CN102827045A (en) * 2012-08-31 2012-12-19 重庆紫光天化蛋氨酸有限责任公司 Method and apparatus for removing impurity in secondary methionine mother liquor

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
FR2772026A1 (en) * 1997-12-05 1999-06-11 Rhone Poulenc Nutrition Animal Preparation of methionine or its hydroxy analog using cation exchange resin
CN1950327A (en) * 2004-04-07 2007-04-18 旭化成化学株式会社 Method of purifying amino acid
CN101503366A (en) * 2009-03-11 2009-08-12 无锡晶海氨基酸有限公司 Method for extracting and separating L-valine by membrane separation and plant chromatography separation
CN101735135A (en) * 2009-12-02 2010-06-16 厦门世达膜科技有限公司 Method for concentrating 5-hydroxyl tryptophan
CN102688610A (en) * 2012-06-19 2012-09-26 华东理工大学 Chromatographic separation method of glycine and inorganic salt
CN102827045A (en) * 2012-08-31 2012-12-19 重庆紫光天化蛋氨酸有限责任公司 Method and apparatus for removing impurity in secondary methionine mother liquor

Cited By (15)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017000867A1 (en) * 2015-06-30 2017-01-05 西安蓝晓科技新材料股份有限公司 Process of purifying methionine
CN104926701A (en) * 2015-06-30 2015-09-23 西安蓝晓科技新材料股份有限公司 Purification process of methionine
CN106380433A (en) * 2016-08-26 2017-02-08 宁夏紫光天化蛋氨酸有限责任公司 Separation and purification method for N-acetyl-D, L-methionine
CN106380433B (en) * 2016-08-26 2018-04-20 宁夏紫光天化蛋氨酸有限责任公司 A kind of isolation and purification method of N acetyl D, L methionine
CN106432018A (en) * 2016-09-14 2017-02-22 宁夏紫光天化蛋氨酸有限责任公司 Method for environment-friendly clean production of D,L-methionine
CN106631855B (en) * 2016-12-09 2018-10-09 三达膜科技(厦门)有限公司 A method of recycling threonine from threonine crystallization mother liquid
CN106631855A (en) * 2016-12-09 2017-05-10 三达膜科技(厦门)有限公司 Method or recycling threonine from threonine crystallization mother solution
CN108623504A (en) * 2017-03-16 2018-10-09 诺华赛分离技术(上海)有限公司 Purify 2- hydroxyls -4- (methyl thio) butyric acid with chromatography
CN108623504B (en) * 2017-03-16 2020-09-01 诺华赛分离技术(上海)有限公司 Purification of 2-hydroxy-4- (methylthio) butanoic acid by chromatography
US11242316B2 (en) * 2017-03-16 2022-02-08 Adisseo France S.A.S. Method for manufacturing 2-hydroxy-4-(methylthio)butyric acid
US10669233B2 (en) 2017-12-28 2020-06-02 Sunresin New Materials Co. Ltd., Xi'an Process of purifying methionine
CN112679397A (en) * 2020-12-21 2021-04-20 宁夏紫光天化蛋氨酸有限责任公司 Preparation method of DL-methionine
CN112679397B (en) * 2020-12-21 2023-08-01 宁夏紫光天化蛋氨酸有限责任公司 Preparation method of DL-methionine
CN112645357A (en) * 2020-12-22 2021-04-13 宁夏紫光天化蛋氨酸有限责任公司 Post-treatment method of sodium sulfate mother liquor
CN114057618A (en) * 2021-12-10 2022-02-18 宁夏紫光天化蛋氨酸有限责任公司 Methionine optimized preparation method based on sulfuric acid indirect acidification method

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Application publication date: 20141203