CN106349131B - A kind of isolation and purification method of methionine - Google Patents
A kind of isolation and purification method of methionine Download PDFInfo
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- CN106349131B CN106349131B CN201610743198.1A CN201610743198A CN106349131B CN 106349131 B CN106349131 B CN 106349131B CN 201610743198 A CN201610743198 A CN 201610743198A CN 106349131 B CN106349131 B CN 106349131B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/26—Separation; Purification; Stabilisation; Use of additives
- C07C319/28—Separation; Purification
Abstract
The invention discloses a kind of isolation and purification method of methionine, concretely comprise the following steps:1) methionine salt is acidified with acid to, cooled down, crystallized, filtered and to obtain filtrate and methionine crystal, methionine crystal is further washed and obtains washing lotion and methionine wet product;) filtrate that obtains step 1), washing lotion be merged into mixed liquor, mixed liquor is concentrated into the mother liquor that salt content is 10 28wt%, methionine content is 2% 5%, mother liquor enters homogeneous membrane electrodialysis after decolorization by accurate filter, carries out desalting processing until the salt in light room is reduced to 3 7wt%;3) solution in the light room after step 2) processing is subjected to out-phase membrane electrodialysis deep desalting again, until the salt in light room decreases below 0.1wt%, obtains methionine aqueous solution, the further condensing crystallizing of methionine aqueous solution is obtained into methionine product.Salt feed liquid containing methionine need not be diluted by this method;Concentration is repeated also without by the inorganic salts filtrate containing methionine, causes methionine that thermal decomposition occurs and generates foul gas.
Description
Technical field
The invention belongs to chemical field, and in particular to a kind of isolation and purification method of methionine.
Background technology
D, L-Methionine also known as methionine, are one of base units for forming protein, are unique in necessary amino acid
Amino acid containing sulphur, except participating in the transfer of methyl, the metabolism of phosphorus and adrenaline, the synthesis of choline, creatine in animal body
Outside, or the raw material of synthetic protein and cystine.
Methionine is widely used in the fields such as medicine, food, feed and cosmetics, wherein as feed addictive volume, use
Amount is very big, and the demand of global methionine has reached 1,800,000 tons/year, and Chinese 2015 annual requirement of methionine has exceeded 160,000
Ton, and at present China except Ningxia purple light Tian Hua methionine Co., Ltd 100,000 tons of methionine go into operation in addition to, China
Methionine is also needed to largely from external import.
There are win wound, An Disu, Sumitomo, An Disu, Ningxia purple light day in the whole world using the company that glycolylurea method prepares methionine
And Russian volga.The maximum difference of these company's glycolylurea method synthetic methionine techniques is embodied in two aspects;(1) cyanogen source
Difference, that is, it is all using 2- 2-hydroxy-4-methylthio fourths made from hydrogen cyanide and methylthiopropionaldehyde reaction to win wound, Sumitomo, An Disu
Nitrile (abbreviation cyanalcohol) produces 5- (2-methylmercaptoethyl)-hydantoins (abbreviation glycolylurea) for raw material, so as to obtain glycolylurea aqueous solution;
And Ningxia purple light day and volga then use rowland-Planck production technology, with Cymag, methylthiopropionaldehyde, ammonia, titanium dioxide
The aqueous solution of carbon produces 5- (2-methylmercaptoethyl)-hydantoins (abbreviation glycolylurea) for raw material, so as to obtain containing sodium carbonate
Glycolylurea aqueous solution;(2) alkali for hydrolyzing glycolylurea is different.Winning the hydrolysis use of glycolylurea in wound, the methionine production technology of Sumitomo is
Potassium carbonate or potassium hydroxide aqueous solution, carbon dioxide acidifying, potassium carbonate recycle, and production technology is cleaner;And pacify enlightening
Soviet Union, Ningxia purple light day, the methionine production technology of volga are all derived from the production technology of French rowland-Planck, because
The hydrolysis of this glycolylurea is all to use sodium hydrate aqueous solution, sulfuric acid acidifying, by-product sodium sulphate.
Therefore, it is directed to using sodium hydroxide hydrolysis glycolylurea, saponification liquor of the hydrolysis generation containing sodium carbonate and Sodium L-methioninate,
For saponification liquor after deamination and carbon dioxide, it is 5.0-5.5 to add sulfuric acid and be acidified to pH, is crystallized under the conditions of being cooled to 40 DEG C, point
From methionine, washing, obtains methionine product after drying;Wash water merges again dense by high temperature with the sulfuric acid mother liquid of sodium containing methionine
Contracting, is especially heated to 100 DEG C or so (at this time the solubility of methionine is maximum, and the solubility of sodium sulphate is low), then separates out big
The sodium sulphate of amount, centrifuges sodium sulphate while hot, and filtrate is cooled to 35 DEG C -40 DEG C, and methionine crystallization, washing, dries and obtain egg ammonia
Acid product, the concentration of sodium sulphate filtrate iterative cycles, cooling containing methionine take sodium sulphate and methionine respectively, in order to avoid egg
The loss of propylhomoserin, row's mother liquor not outer as far as possible, causes methionine in the case where being in thermophilic digestion for a long time, some methionine occurs
Thermal decomposition, generates dimethyl disulfide with foul smell or methyl mercaptan (as shown in Figure 1;CN104693082A), these
Material can be remained in the cooling water that sulfuric acid mother liquid of sodium neutralizes outer row, and the sulfuric acid mother liquid of sodium for causing to circulate for a long time has stench
Taste, sodium sulphate plant operations bad environments, influences surrounding enviroment, and also results in methionine decomposed, the mother solution C OD of outer row
It is higher, it is difficult to carry out biochemical treatment, and sulfuric acid mother liquid of sodium constantly circulates, a small amount of sodium formate, sodium acetate in mother liquor, third
Sour sodium can constantly be accumulated, these materials cause the decline of follow-up methionine product quality, its decline the reason for be mainly:Its
One, the decomposition of methionine and the polymerization of methionine especially form the dimer of methionine, and methionine decompose after having
Machine impurity is accumulated in system, causes the methionine of crystallization to have niff;Second, the sodium formate of saponification liquor generation, second
The accumulation in system such as sour sodium, sodium propionate, 2-Hydroxy-4-methylthiobutyric acid sodium, so as to have impact on the quality of methionine product.
The outstanding problem that the above factor results in the methionine production technology maximums such as An Disu, Chongqing purple light day, volga is
Environmental issue.It is to burn to solve the problems, such as this best bet at present, this inevitably consumes more energy, increase methionine
Loss and production cost.Patent CN104693082A discloses a kind of method that methionine is isolated and purified using continuous chromatography,
This method is exactly using sulfuric acid mother liquid of sodium of the continuous chromatography processing containing methionine, achievees the purpose that desalination, but the problem of maximum
Have at 2 points:First is, chromatography investment is big;Second be the methionine and sodium sulphate obtained after chromatographic isolation concentration it is all dilute
Release twice, in follow-up concentration except water consumption is higher.
Although out-phase membrane electrodialysis can carry out desalting processing, it is low that this desalination is often merely able to removing salt content
Feed liquid, has strict requirements to the salt content in processing feed liquid, if salt content is excessive, can cause the electrodialytic desalination of heterogeneous membrane
The problem of power consumption is high, salt rejection rate is low, methionine rejection is low.
Therefore, develop another production D, L-Methionine new process is to be highly desirable, especially methionine with it is inorganic
Salt isolates and purifies.
The content of the invention
In view of this, it is an object of the invention to provide a kind of isolation and purification method of methionine.The method need not
Salt feed liquid containing methionine is diluted, reduces the required energy consumption of subsequent purification concentration, easy to operate, gained methionine is pure
Degree is high;Concentration is repeated also without by the inorganic salts filtrate containing methionine in this method, causes methionine at long-time
Heat decomposition is issued in thermophilic digestion and generates foul gas, and this method is of low cost, gives up without substantial amounts of acid and stink
Water discharge, environmentally protective, by-product inorganic purity salt is high and can be used as commodity selling.
Methionine Thermal Decomposition Mechanism is have studied first to solve foregoing invention purpose, it is true by being confirmed with compounds GC-MS
The product for having determined methionine thermal decomposition is dimethyl disulfide, allylamine, 3- methyl mercaptos propylamine and carbon dioxide, its mechanism is:
Methionine is decomposed into 3- methyl mercaptos propylamine and carbon dioxide, that is to say, that decarboxylation first when heated first;3- methyl mercapto propylamine
Continue to be heated and be decomposed into dimethyl disulfide and allylamine, as shown in Figure 1.
To reach above-mentioned purpose, the present invention specifically provides following technical solution:
A kind of isolation and purification method of methionine, described method includes following steps:
1) mother liquor containing methionine and salt is entered into homogeneous membrane electrodialysis by filter, carries out desalting processing until light
Salt in room is reduced to 3-7wt%;
2) solution in the light room after step 1) processing is subjected to out-phase membrane electrodialysis deep desalting again, until in light room
Salt decreases below 0.1wt%, obtains methionine aqueous solution and the saline solution of dense room in light room.
Further, the mother liquor containing methionine and salt obtains as follows:Methionine salt is acidified with acid, is cold
But, crystallize, filter to obtain filtrate and methionine crystal, further wash methionine crystal and obtain washing lotion and methionine wet product, by step
1) filtrate that obtains, washing lotion are merged into mixed liquor, by mixed liquor be concentrated into salt content be 10-28wt%, methionine content be
The mother liquor of 2%-5%.
Further, the methionine salt is made for 5- (2-methylmercaptoethyl)-hydantoins through basic hydrolysis, and the alkali is
One or more in sodium hydroxide, sodium carbonate, potassium hydroxide, potassium carbonate, saleratus, ammonia.
Further, the methionine salt includes Sodium L-methioninate and sodium carbonate.
Further, the methionine salt further includes the one or more in sodium formate, sodium acetate, sodium propionate.
Further, acid is inorganic acid used in the acidifying, and it is 4.0-7.0 that methionine salt, which is acidified with acid to pH,.
Further, the inorganic acid is sulfuric acid, hydrochloric acid or phosphoric acid, and it is 4.0-7.0 that methionine salt, which is acidified with acid to pH,.
Further, the inorganic acid is sulfuric acid, mass fraction 90%-98%.
Further, the temperature of water is 30 DEG C -45 DEG C used in step 1) washing methionine crystal.
Further, the method further includes step 3):Methionine aqueous solution is further concentrated to give methionine product, will be dense
The saline solution of room is further concentrated to give inorganic salts.
Beneficial effects of the present invention:Compared with prior art, the isolation and purification method of methionine provided by the invention is profit
Reasonably combined with homogeneous membrane electrodialysis and out-phase membrane electrodialysis and solve methionine and organic-inorganic salinity in traditional processing technology
The problem of from difficulty, compared with its single use homogeneous membrane or out-phase membrane electrodialysis, both combinations carry out desalination, overcome two
The applied defect of person in itself.Homogeneous membrane electrodialysis and out-phase membrane electrodialysis are used for methionine desalination field, have high selectivity,
Separating degree is high, and with chromatography desalination project, the sodium sulphate feed liquid of homogeneous membrane electrodialysis and heterogeneous membrane electrodialysis process containing methionine is not
Need the salt feed liquid containing methionine being diluted, reduce the required energy consumption of subsequent purification concentration, easy to operate, gained egg ammonia
Sour purity is high;Concentration is repeated also without by the inorganic salts filtrate containing methionine in this method, causes methionine when long
Between be in thermophilic digestion and issue heat and decompose and generate foul gas, and this method it is of low cost, without substantial amounts of acid and smelly
Taste discharge of wastewater, environmentally protective, by-product inorganic purity salt is high and can be used as commodity selling.
Brief description of the drawings
In order to make the purpose of the present invention, technical solution and beneficial effect clearer, the present invention provides drawings described below:
Fig. 1 is methionine by Thermal Decomposition Mechanism figure;
Fig. 2 is the basic arrangement mode schematic diagram of electrodialysis.
Embodiment
The preferred embodiment of the present invention is described in detail below.The experiment side of actual conditions is not specified in embodiment
Method, usually according to normal condition or according to the condition proposed by manufacturer.
The basic arrangement mode schematic diagram of electrodialysis is as shown in Figure 2.
Saponification liquor described in the present embodiment is by 5- (2-methylmercaptoethyl)-hydantoins or 5- (2- methylmercaptan ethyls
Base)-hydantoins and sodium carbonate mixed liquor add sodium hydroxide and be heated to 185 DEG C to being fully hydrolyzed, after deamination and carbon dioxide
It is made.Saponification liquor is composed of the following components:Mass percent be 15% ± 5% L, D- Sodium L-methioninates, mass percent 7%
± 5% sodium carbonate, sodium formate, sodium acetate and sodium propionate containing 0.1%-1.0%, and the aqueous medium of surplus.
After saponification liquor is carried out activated carbon decolorizing, then directly methionine isolation and purification method described in the present embodiment is
The sulfuric acid acidifying pH to 5.0-5.5 of 90%-98% is added, 35 DEG C -40 DEG C are cooled under stirring, is crystallized, is filtered, water
Wash, be dried to obtain methionine product, methionine extraction efficiency is 88%-92% (in terms of methionine total recovery), the purity of methionine
More than 99.4% can be reached;Wash water merges with sulfuric acid mother liquid of sodium, obtains the sulfuric acid mother liquid of sodium containing methionine, the mother liquor is through overrich
It is 20%-28% to be reduced to sodium sulphate content, and wherein methionine content is for 2%-4% or so, sodium formate, sodium acetate, sodium propionate etc.
Altogether about 1% or so.
Embodiment 1
It is 20wt% that sulfuric acid mother liquid of sodium process containing methionine is concentrated into sodium sulphate content, and wherein methionine content is
2wt% or so, sodium formate, sodium acetate, sodium propionate etc. amounts to about 1wt% or so, and material liquid pH 5.5, amounts to 10L.Contain egg ammonia
The sulfuric acid mother liquid of sodium of acid passes through accurate filter, and homogeneous membrane electrodialysis is entered under the conditions of maintaining the temperature at 35 DEG C and is carried out at desalination
Reason, homogeneous membrane electrodialysis has three Room, is pole liquid chamber, feed liquid room (light room) and receiving chamber (dense room) respectively, in desalination processes,
Since sodium sulphate is migrated to dense room, the pH in feed liquid room can have been raised, and sulfuric acid need to be added to keep pH 5.5 or so.When feed liquid room
In sodium sulphate when being reduced to 5%, the material in feed liquid room is transferred to heterogeneous membrane electrodialysis process system and carries out deep desalting, passes through
Electrodialysis desalination twice, the sodium sulphate content in feed liquid are less than 0.05%, methionine content 3.5%;By electrodialysis twice
After desalination, the rejection of methionine reaches 98.8%, and desalination rate reaches 99.5%.Respectively by aqueous sodium persulfate solution (content formic acid
Sodium, sodium acetate, sodium propionate), methionine aqueous solution (containing micro sodium sulphate) concentrated, respectively obtain sodium sulphate and egg ammonia
Acid product, the purity of methionine product are more than 99%.
Recycling Mother Solution after above-mentioned methionine aqueous solution condensing crystallizing is applied mechanically, when the salt accumulation of wherein residual minim is to influencing
During methionine product quality, Recycling Mother Solution to homogeneous membrane electrodialysis or heterogeneous membrane electrodialysis desalination part carry out desalting processing.
Embodiment 2
It is 25wt% that sulfuric acid mother liquid of sodium process containing methionine is concentrated into sodium sulphate content, and wherein methionine content is
2.4wt% or so, sodium formate, sodium acetate, sodium propionate etc. amounts to about 1wt% or so, and material liquid pH 5.2, amounts to 10L.Contain egg
The sulfuric acid mother liquid of sodium of propylhomoserin passes through accurate filter, and homogeneous membrane electrodialysis is entered under the conditions of maintaining the temperature at 35 DEG C and is carried out at desalination
Reason, homogeneous membrane electrodialysis has three Room, is pole liquid chamber, feed liquid room (light room) and receiving chamber (dense room) respectively, in desalination processes,
Since sodium sulphate is migrated to dense room, the pH in feed liquid room can have been raised, and sulfuric acid need to be added to keep pH 5.2 or so.When feed liquid room
In sodium sulphate when being reduced to 4%, the material in feed liquid room is transferred to heterogeneous membrane electrodialysis process system and carries out deep desalting, passes through
Electrodialysis desalination twice, the sodium sulphate content in feed liquid are less than 0.10%, methionine content 3.2%;By electrodialysis twice
After desalination, the rejection of methionine reaches 99%, and desalination rate reaches 99.0%.Respectively by aqueous sodium persulfate solution (content sodium formate,
Sodium acetate, sodium propionate), methionine aqueous solution (containing micro sodium sulphate) concentrated, respectively obtain sodium sulphate and methionine
Product, the purity of methionine product are more than 99%.
Recycling Mother Solution after above-mentioned methionine aqueous solution condensing crystallizing is applied mechanically, when the salt accumulation of wherein residual minim is to influencing
During methionine product quality, Recycling Mother Solution to homogeneous membrane electrodialysis or heterogeneous membrane electrodialysis desalination part carry out desalting processing.
Embodiment 3
It is 28wt% that sulfuric acid mother liquid of sodium process containing methionine is concentrated into sodium sulphate content, and wherein methionine content is
3.0wt% or so, sodium formate, sodium acetate, sodium propionate etc. amounts to about 1wt% or so, and material liquid pH 5.1, amounts to 10L.Contain egg
The sulfuric acid mother liquid of sodium of propylhomoserin passes through accurate filter, and homogeneous membrane electrodialysis is entered under the conditions of maintaining the temperature at 35 DEG C and is carried out at desalination
Reason, homogeneous membrane electrodialysis has three Room, is pole liquid chamber, feed liquid room (light room) and receiving chamber (dense room) respectively, in desalination processes,
Since sodium sulphate is migrated to dense room, the pH in feed liquid room can have been raised, and sulfuric acid need to be added to keep pH 5.1 or so.When feed liquid room
In sodium sulphate when being reduced to 6%, the material in feed liquid room is transferred to heterogeneous membrane electrodialysis process system and carries out deep desalting, passes through
Electrodialysis desalination twice, the sodium sulphate content in feed liquid are less than 0.03%, methionine content 3.8%;By electrodialysis twice
After desalination, the rejection of methionine reaches 99%, and desalination rate reaches 99.6%.Respectively by aqueous sodium persulfate solution (content sodium formate,
Sodium acetate, sodium propionate), methionine aqueous solution (containing micro sodium sulphate) concentrated, respectively obtain sodium sulphate and methionine
Product, the purity of methionine product are more than 99%.
Recycling Mother Solution after above-mentioned methionine aqueous solution condensing crystallizing is applied mechanically, when the salt accumulation of wherein residual minim is to influencing
During methionine product quality, Recycling Mother Solution to homogeneous membrane electrodialysis or heterogeneous membrane electrodialysis desalination part carry out desalting processing.
Embodiment 4
It is 28wt% that sulfuric acid mother liquid of sodium process containing methionine is concentrated into sodium sulphate content, and wherein methionine content is
3.0wt% or so, sodium formate, sodium acetate, sodium propionate etc. amounts to about 1wt% or so, and material liquid pH 5.1, amounts to 10L, will be above-mentioned
The activated carbon (in terms of feed liquid quality) that feed liquid adds 0.5% carries out decolorization, and bleaching temperature is 45 DEG C, filters activated carbon, filter
Liquid is cooled to 35 DEG C or so.Sulfuric acid mother liquid of sodium containing methionine passes through accurate filter, under the conditions of maintaining the temperature at 35 DEG C into
Enter homogeneous membrane electrodialysis and carry out desalting processing, homogeneous membrane electrodialysis has three Room, is pole liquid chamber, feed liquid room (light room) respectively and connects
By room (dense room), in desalination processes, since sodium sulphate is migrated to dense room, the pH in feed liquid room can have been raised, and need to add sulfuric acid
PH is kept 5.1 or so.When the sodium sulphate in feed liquid room is reduced to 6%, the material in feed liquid room is transferred to out-phase membrane electrodialysis
Processing system carries out deep desalting, and by electrodialysis desalination twice, the sodium sulphate content in feed liquid is less than 0.03%, and methionine contains
Measure as 3.8%;After electrodialysis desalination twice, the rejection of methionine reaches 99%, and desalination rate reaches 99.6%.Respectively will
Aqueous sodium persulfate solution (content sodium formate, sodium acetate, sodium propionate), methionine aqueous solution (containing micro sodium sulphate) carry out dense
Contracting, respectively obtains sodium sulphate and methionine product, and the purity of methionine product is more than 99%.
Recycling Mother Solution after above-mentioned methionine aqueous solution condensing crystallizing is applied mechanically, when the salt accumulation of wherein residual minim is to influencing
During methionine product quality, Recycling Mother Solution to homogeneous membrane electrodialysis or heterogeneous membrane electrodialysis desalination part carry out desalting processing.
To sum up it can be shown that, compared with prior art, the isolation and purification method of methionine provided by the invention is using homogeneous
Membrane electrodialysis and out-phase membrane electrodialysis reasonably separate difficulty with reference to methionine in solution traditional processing technology with organic-inorganic salt
The problem of, compared with its single use homogeneous membrane or out-phase membrane electrodialysis, both combinations carry out desalination, overcome both in itself
Applied defect.Homogeneous membrane electrodialysis and out-phase membrane electrodialysis are used for methionine desalination field, there is high selectivity, separating degree
Height, with chromatography desalination project, the sodium sulphate feed liquid of homogeneous membrane electrodialysis and heterogeneous membrane electrodialysis process containing methionine need not incite somebody to action
Salt feed liquid containing methionine is diluted, and reduces energy consumption, easy to operate, gained methionine purity needed for subsequent purification concentration
It is high;Concentration is repeated also without by the inorganic salts filtrate containing methionine in this method, causes methionine to be in for a long time
Thermophilic digestion issues heat and decomposes and generate foul gas, and this method is of low cost, the substantial amounts of acid and stink waste water of nothing
Discharge, environmentally protective, by-product inorganic purity salt is high and can be used as commodity selling.
Finally illustrate, preferred embodiment above is merely illustrative of the technical solution of the present invention and unrestricted, although logical
Cross above preferred embodiment the present invention is described in detail, however, those skilled in the art should understand that, can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (9)
1. a kind of isolation and purification method of methionine, it is characterised in that described method includes following steps:
1)Mother liquor containing methionine and salt is entered into homogeneous membrane electrodialysis by filter, carries out desalting processing until in light room
Salt be reduced to 3-7wt%;
2)Will be through step 1)Solution after processing in light room carries out out-phase membrane electrodialysis deep desalting again, until the salt drop in light room
As low as it is less than 0.1wt%, obtains methionine aqueous solution and the saline solution of dense room in light room;
The mother liquor containing methionine and salt obtains as follows:Methionine salt is acidified with acid, cool down, crystallize, is taken out
Filtrate and methionine crystal are filtered to obtain, methionine crystal is further washed and obtains washing lotion and methionine wet product, by step 1)Obtained filter
Liquid, washing lotion are merged into mixed liquor, and mixed liquor is concentrated into the mother liquor that salt content is 10-28wt%, methionine content is 2%-5%.
2. a kind of isolation and purification method of methionine according to claim 1, it is characterised in that the methionine salt is 5-
(2-methylmercaptoethyl)- hydantoins is made through basic hydrolysis, and the alkali is sodium hydroxide, sodium carbonate, potassium hydroxide, carbonic acid
One or more in potassium, saleratus, ammonia.
3. a kind of isolation and purification method of methionine according to claim 2, it is characterised in that the methionine salt includes egg
Propylhomoserin sodium and sodium carbonate.
4. a kind of isolation and purification method of methionine according to claim 3, it is characterised in that the methionine salt further includes
One or more in sodium formate, sodium acetate, sodium propionate.
5. a kind of isolation and purification method of methionine according to claim 1, it is characterised in that acid is nothing used in the acidifying
Machine acid, it is 4.0-7.0 that methionine salt, which is acidified with acid to pH,.
A kind of 6. isolation and purification method of methionine according to claim 5, it is characterised in that the inorganic acid for sulfuric acid,
Hydrochloric acid or phosphoric acid, it is 4.0-7.0 that methionine salt, which is acidified with acid to pH,.
A kind of 7. isolation and purification method of methionine according to claim 6, it is characterised in that the inorganic acid is sulfuric acid,
Mass fraction is 90%-98%.
A kind of 8. isolation and purification method of methionine according to claim 1, it is characterised in that step 1)It is brilliant to wash methionine
The temperature of water used in body is 30 DEG C -45 DEG C.
9. a kind of isolation and purification method of methionine according to claim 1, it is characterised in that the method further includes step
3):Methionine aqueous solution is further concentrated to give methionine product, the saline solution of dense room is further concentrated to give inorganic salts.
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CN108794364A (en) * | 2017-05-02 | 2018-11-13 | 宁夏紫光天化蛋氨酸有限责任公司 | A kind of isolation and purification method of methionine |
CN108794363A (en) * | 2017-05-02 | 2018-11-13 | 宁夏紫光天化蛋氨酸有限责任公司 | A kind of methionine method for crystallising |
EP3406593A1 (en) | 2017-05-24 | 2018-11-28 | Evonik Degussa GmbH | Method for manufacturing methionine |
CN108658821B (en) * | 2017-06-13 | 2020-07-17 | 宁夏紫光天化蛋氨酸有限责任公司 | Clean production method of D, L-methionine and product thereof |
CN109232338A (en) * | 2018-11-09 | 2019-01-18 | 禄丰天宝磷化工有限公司 | A kind of isolation and purification method of methionine hydroxy analog |
CN109678768B (en) * | 2019-02-14 | 2020-12-22 | 天宝动物营养科技股份有限公司 | Method for producing methionine metal chelate by using methionine crystallization mother liquor |
CN112645357B (en) * | 2020-12-22 | 2023-08-01 | 宁夏紫光天化蛋氨酸有限责任公司 | Post-treatment method of sodium sulfate mother liquor |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3459650A (en) * | 1966-01-13 | 1969-08-05 | Sumitomo Chemical Co | Process for the purification of amino acids |
US4419198A (en) * | 1981-06-22 | 1983-12-06 | Monsanto Company | Purification of methioine hydroxy analogue hydrolyzate by electrodialysis |
US4454012A (en) * | 1980-02-19 | 1984-06-12 | Rhone-Poulenc Industries | Process for the preparation of methionine |
CN1560023A (en) * | 2004-02-16 | 2005-01-05 | 浙江大学 | Process of separating DL-alpha lactamic acid by ion membrane electric dialysis method |
CN104130169A (en) * | 2014-07-08 | 2014-11-05 | 重庆紫光化工股份有限公司 | Environment-friendly clean production method of D,L-methionine |
CN104693082A (en) * | 2015-04-03 | 2015-06-10 | 重庆紫光化工股份有限公司 | Method for preparing methionine |
-
2016
- 2016-08-26 CN CN201610743198.1A patent/CN106349131B/en active Active
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3459650A (en) * | 1966-01-13 | 1969-08-05 | Sumitomo Chemical Co | Process for the purification of amino acids |
US4454012A (en) * | 1980-02-19 | 1984-06-12 | Rhone-Poulenc Industries | Process for the preparation of methionine |
US4419198A (en) * | 1981-06-22 | 1983-12-06 | Monsanto Company | Purification of methioine hydroxy analogue hydrolyzate by electrodialysis |
CN1560023A (en) * | 2004-02-16 | 2005-01-05 | 浙江大学 | Process of separating DL-alpha lactamic acid by ion membrane electric dialysis method |
CN104130169A (en) * | 2014-07-08 | 2014-11-05 | 重庆紫光化工股份有限公司 | Environment-friendly clean production method of D,L-methionine |
CN104693082A (en) * | 2015-04-03 | 2015-06-10 | 重庆紫光化工股份有限公司 | Method for preparing methionine |
Non-Patent Citations (2)
Title |
---|
电渗析技术在氨基酸生产中的应用;陈艳 等;《水处理技术》;20111130;第37卷(第11期);第10-15页 * |
电渗析技术的原理及应用;李媛 等;《水处理技术与装备》;20151231(第5期);第16-22页 * |
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