CN102617379A - Processing method for lysine-containing solution - Google Patents
Processing method for lysine-containing solution Download PDFInfo
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- CN102617379A CN102617379A CN2012100506118A CN201210050611A CN102617379A CN 102617379 A CN102617379 A CN 102617379A CN 2012100506118 A CN2012100506118 A CN 2012100506118A CN 201210050611 A CN201210050611 A CN 201210050611A CN 102617379 A CN102617379 A CN 102617379A
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Abstract
The invention discloses a processing method for a lysine-containing solution. The processing method includes that the lysine-containing solution is enabled to sequentially pass one or more groups of positive ion exchange resin column groups which are in serial connection sequentially until the concentration of lysine in liquid flowed from ends of the one or more groups of positive ion exchange resin column groups is not larger than 0.1g/dL, each group of positive ion exchange resin column groups comprises one or more positive ion exchange resin columns which are in a parallel connection, and positive ion exchange resin columns with lysine are subjected to elution with an alkaline solution to obtain a lysine-containing elution. The processing method for the lysine-containing solution is characterized in that the lysine-containing solution passes the positive ion exchange resin column groups under the condition that the pH is 1.0-2.0 or the concentration of lysine is not lower than 1.0g/dL. The invention further discloses a circulating processing method for the lysine-containing solution. The processing method can improve the yield of the lysine, and be widely applied to industrial production.
Description
Technical field
The present invention relates to a kind of treatment process that contains lysine solution.
Background technology
Methionin is one of eight kinds of primary amino acids (claim indispensable amino acid again, they are Methionin, Threonine, leucine, Isoleucine, methionine(Met), Xie Ansuan, phenylalanine(Phe) and tryptophane) of needed by human.The solubleness of Methionin in water is very big, and is prone to absorb carbon dioxide in air, is difficult to obtain its crystallization.Therefore it often occurs with the form of mono-hydrochloric salts as commodity.Methionin is of many uses, is mainly used in following industry: foodstuffs industry, preparation nutrition-fortifying agent, tasty agents, sweeting agent; Fodder industry, the preparation nutrition-fortifying agent; Medicine industry, preparation amino acid transfusion, amino acid derivative, amino acid salts; Chemical industry, preparing washing agent, skin care item, leatheroid; Agricultural, preparation public nuisance-free agricultural chemicals etc.At present, the Methionin product more than 90% is used for fodder industry, as adding an amount of Methionin in the feed, can increase the synthetic of animal body internal protein, promotes animal growth.
Lysine hydrochloride is general to adopt following method to prepare: strain fermentation obtains fermented liquid; Adding a large amount of vitriol oils in the fermented liquid transfers pH to 2.0-3.0 to carry out acidifying; Remove thalline through metallic membrane or ceramic membrane filter after the acidifying; Obtain Methionin membrane filtration liquid and promptly contain lysine solution, contain lysine solution and adopt strongly acidic cation-exchange to adsorb exchange, wash-out is carried out with weak ammonia in the saturated back of resin absorption; The Methionin that elutes obtains the lysine hydrochloride finished product through concentrated, salt acid for adjusting pH value, crystallization, solid-liquid separation, oven dry.
Raising along with modernization level; At present generally adopt large chemical equipment ISEP system to contain the IX purification Methionin of lysine solution; Principle is: make to contain lysine solution and carry out ion-exchange chromatography with many groups cation exchange resin column groups of contact and separate; Every group of cation exchange resin column group comprises the cation exchange resin column of one or more parallel connections; Every group of cation exchange resin column group led district and breeding blanket through adsorption zone, back filled region, alkali successively and circularly, so that the cation exchange resin column group exchanges absorption successively and circularly, purifies and absorption once more, desorb and regeneration, obtains elutriant after the desorb.Methionin mainly exists with the monovalent cation form, and the ion exchange reaction formula of adsorption and desorption is following:
R-H+HLysH
+→R-HLysH+H
+
R-HLysH+NH
4 ++OH
-→R-NH
4+HLys+H
2O
As shown in Figure 1; The technology of using at present generally comprises: at adsorption zone; The cation exchange resin column group is connected in series successively, contains lysine solution and introduces from the upper end that is in the first cation exchange resin column group of adsorption zone, respectively organizes the cation exchange resin column group in this adsorption zone of flowing through successively; And flow out from the lower end that is in adsorption zone omega-cation exchange resin column group and to obtain waste liquid, the said Methionin of part at least that contains in the lysine solution is adsorbed onto on the Zeo-karb; In the back filled region, with the part elutriant backfill cation exchange resin column that obtains, make cation exchange resin column purify with and be tending towards adsorbing saturated; Lead the district at alkali, make the basic soln cation exchange resin column of flowing through, make the Methionin desorb that is adsorbed onto on the Zeo-karb obtain elutriant; In the breeding blanket; Use earlier the hot wash cation exchange resin column, with the air compression leg water in the cation exchange resin column is discharged again, in the waste liquid that adsorption zone obtains, add the sulfuric acid adjust pH then to 1.0-1.2; With the waste liquid backfill cation exchange resin column behind the adjust pH; Cation exchange resin column is made the transition, and cation exchange resin column returns adsorption zone again and adsorbs then, accomplishes once circulation.
The ISEP system adopts the technology of using at present, though use the pH value as the waste liquid of 1.0-1.2 cation exchange resin column to be made the transition, remains in the H in the cation exchange resin column after transition
+Amount limited; At adsorption zone; Contain the pH value of lysine solution through the first cation exchange resin column group of adsorption zone still for about 2.0-3.0, when there was the cation exchange resin column group that at least two groups are connected in series successively simultaneously in adsorption zone, containing lysine solution, to pass through the pH value of cation exchange resin column group of back higher; Thereby cation exchange resin column is lower to the adsorptive power that contains lysine solution, thereby the Methionin yield is low.
Summary of the invention
The objective of the invention is for the low defective of Methionin yield in the technology that overcomes present use, a kind of new treatment process that contains lysine solution is provided.
Contriver of the present invention is unexpected under study for action to be found; Make and contain lysine solution and exchange absorption through one or more groups placed in-line successively cation exchange resin column group successively; Lysine concentration is not higher than under the situation of 0.1g/dL from the terminal effusive liquid of one or more groups placed in-line successively cation exchange resin column group making, and contains lysine solution and can improve the yield of Methionin through the cation exchange resin column group in the pH value under for the condition that is not less than 1.0g/dL under the condition of 1.0-2.0 or at lysine concentration.
Therefore; To achieve these goals; On the one hand; The invention provides a kind of treatment process that contains lysine solution; Said method comprises: make the said lysine solution that contains successively through one or more groups placed in-line successively cation exchange resin column group, be adsorbed to that lysine concentration is not higher than 0.1g/dL from the terminal effusive liquid of this one or more groups placed in-line successively cation exchange resin column group so that contain Methionin in the lysine solution, every group of cation exchange resin column group comprises the cation exchange resin column of one or more parallel connections; Cation exchange resin column after using basic soln to absorption Methionin then carries out wash-out; Obtain containing the elutriant of Methionin, it is characterized in that, said contain lysine solution the pH value for the condition that is not less than 1.0g/dL under the condition of 1.0-2.0 or at lysine concentration under through said cation exchange resin column group.
Preferably, said contain lysine solution the pH value for the condition that is not less than 1.0g/dL under the condition of 1.8-2.0 or at lysine concentration under through said cation exchange resin column group.
On the other hand; The present invention also provides a kind of treatment process that contains lysine solution, it is characterized in that, said method comprises: make the said lysine solution that contains carry out ion-exchange chromatography with many groups cation exchange resin column groups of contact and separate; Every group of cation exchange resin column group led district and breeding blanket through adsorption zone, alkali successively and circularly; So that the cation exchange resin column group exchanges absorption, desorb and regeneration successively and circularly, obtain elutriant after the desorb, said every group of cation exchange resin column group comprises the cation exchange resin column of one or more parallel connections; Wherein
One or more groups placed in-line successively cation exchange resin column group is in adsorption zone simultaneously; The said lysine solution that contains is introduced from the upper end that is in the first cation exchange resin column group of adsorption zone; In the pH value for respectively organizing the cation exchange resin column group in this adsorption zone of flowing through successively under the condition of 1.0-2.0 or under lysine concentration is not less than the condition of 1.0g/dL; Flow out from the lower end that is in adsorption zone omega-cation exchange resin column group then; The said Methionin of part at least that contains in the lysine solution is adsorbed onto on the Zeo-karb, and makes the lysine concentration in the effusive liquid not be higher than 0.1g/dL; Lead the district at alkali, make the basic soln said cation exchange resin column of flowing through, make the Methionin desorb that is adsorbed onto on the Zeo-karb obtain said elutriant; In the breeding blanket, water and air make cation exchange resin column be able to regeneration successively through cation exchange resin column.
Preferably; The said lysine solution that contains is introduced from the upper end that is in the first cation exchange resin column group of adsorption zone;, flow out from the lower end that is in adsorption zone omega-cation exchange resin column group then for respectively organizing the cation exchange resin column group in this adsorption zone of flowing through successively under the condition of 1.8-2.0 or under lysine concentration is not less than the condition of 1.0g/dL in the pH value.
The treatment process that contains lysine solution provided by the invention; Improved the yield of Methionin; Shown in embodiment 1 and Comparative Examples 1; The lysine concentration of embodiment 1 from the effusive liquid in lower end of adsorption zone omega-cation exchange resin column group is 0.04g/dL, and the content of the Methionin of Comparative Examples 1 from the effusive liquid in lower end of adsorption zone omega-cation exchange resin column group is 0.08g/dL; Every group of cation exchange resin column group provided by the invention led the method for district and breeding blanket successively and circularly through adsorption zone, alkali; Owing to contain lysine solution passes through adsorption zone under for the condition that is not less than 1.0g/dL under the condition of 1.0-2.0 or at lysine concentration in pH value cation exchange resin column group; Saved the step of using sulfuric acid to transfer the waste liquor PH value cation exchange resin column to be made the transition in the breeding blanket as 1.0-1.2; Under the identical situation of the cation exchange resin column group mode of connection of adsorption zone; Save the sulfuric acid consumption greatly, reduced production cost.The treatment process that contains lysine solution provided by the invention can be widely used in industrial production.
Other features and advantages of the present invention will partly specify in embodiment subsequently.
Description of drawings
Fig. 1 contains the process flow sheet of lysine solution for ISEP system handles in the technology of using at present;
Fig. 2 is for containing the process flow sheet of lysine solution according to the ISEP system handles of the inventive method.
Embodiment
Be elaborated below in conjunction with the accompanying drawing specific embodiments of the invention.Should be understood that embodiment described herein only is used for explanation and explains the present invention, is not limited to the present invention.
On the one hand; The invention provides a kind of treatment process that contains lysine solution; This method comprises: make to contain lysine solution successively through one or more groups placed in-line successively cation exchange resin column group; Be adsorbed to that lysine concentration is not higher than 0.1g/dL from the terminal effusive liquid of this one or more groups placed in-line successively cation exchange resin column group so that contain Methionin in the lysine solution; Every group of cation exchange resin column group comprises the cation exchange resin column of one or more parallel connections; Use basic soln that the cation exchange resin column of absorption behind the Methionin carried out wash-out then, obtain containing the elutriant of Methionin, contain lysine solution in pH value for perhaps being not less than under the condition of 1.0g/dL through said cation exchange resin column group under the condition of 1.0-2.0 at lysine concentration.
In the fermentative prepn Methionin process; Strain fermentation obtains fermented liquid; Add a large amount of vitriol oils in the fermented liquid and transfer pH to 2.0-3.0 to carry out acidifying, remove thalline through metallic membrane or ceramic membrane filter after the acidifying and obtain Methionin membrane filtration liquid, among the present invention; Contain lysine solution and comprise this Methionin membrane filtration liquid, the concentration of Methionin is generally 14.0-18.0g/dL in the Methionin membrane filtration liquid.
According to the present invention, through said cation exchange resin column group can realize the object of the invention in the pH value under for the condition that is not less than 1.0g/dL under the condition of 1.0-2.0 or at lysine concentration although contain lysine solution, promptly improve the yield of Methionin.But under the preferable case, contain lysine solution the pH value for the condition that is not less than 1.0g/dL under the condition of 1.8-2.0 or at lysine concentration under through said cation exchange resin column group, can be under the situation that improves the Methionin yield further saving sulfuric acid consumption.
Among the present invention, the cation exchange resin column group is preferably three groups, and every group of cation exchange resin column group preferably includes the cation exchange resin column of 3-6 parallel connection.
Among the present invention; Zeo-karb in the cation exchange resin column can be used for adsorbing the cationic various Zeo-karbs of Methionin or Methionin for this area; But be preferably sulfonic group strong-acid type cation exchange resin; The total exchange capacity of Zeo-karb is preferably greater than 5mmol/g, further is preferably 6-15mmol/g, further is preferably 6-10mmol/g.
Among the present invention, the pH value is preferably regulated through adding sulfuric acid.
Among the present invention; Methionin is eluted from the easy cation exchange resin column behind the absorption Methionin and make things convenient for cation exchange resin column regenerated aspect to consider; Basic soln is preferably ammoniacal liquor, and the pH value is preferably 10.0-14.0, more preferably 11.0-12.5.
On the other hand; The invention provides a kind of treatment process that contains lysine solution; This method comprises: make to contain lysine solution and carry out ion-exchange chromatography with many groups cation exchange resin column groups of contact and separate, every group of cation exchange resin column group led district and breeding blanket through adsorption zone, alkali successively and circularly, so that the cation exchange resin column group exchanges absorption, desorb and regeneration successively and circularly; Obtain elutriant after the desorb; Every group of cation exchange resin column group comprises the cation exchange resin column of one or more parallel connections, wherein
One or more groups placed in-line successively cation exchange resin column group is in adsorption zone simultaneously; Containing lysine solution introduces from the upper end that is in the first cation exchange resin column group of adsorption zone; In the pH value for respectively organizing the cation exchange resin column group in this adsorption zone of flowing through successively under the condition of 1.0-2.0 or under lysine concentration is not less than the condition of 1.0g/dL; Flow out from the lower end that is in adsorption zone omega-cation exchange resin column group then; The Methionin of part at least that contains in the lysine solution is adsorbed onto on the Zeo-karb, and makes the lysine concentration in the effusive liquid not be higher than 0.1g/dL; Lead the district at alkali, make the basic soln cation exchange resin column of flowing through, make the Methionin desorb that is adsorbed onto on the Zeo-karb obtain elutriant; In the breeding blanket, water and air make cation exchange resin column be able to regeneration successively through cation exchange resin column.
According to the present invention; Although containing lysine solution introduces from the upper end that is in the first cation exchange resin column group of adsorption zone; In the pH value for respectively organizing the cation exchange resin column group in this adsorption zone of flowing through successively under the condition of 1.0-2.0 or under lysine concentration is not less than the condition of 1.0g/dL; Flow out from the lower end that is in adsorption zone omega-cation exchange resin column group then, can realize the object of the invention, promptly improve the yield of Methionin.But under the preferable case; Containing lysine solution introduces from the upper end that is in the first cation exchange resin column group of adsorption zone; In the pH value for respectively organizing the cation exchange resin column group in this adsorption zone of flowing through successively under the condition of 1.8-2.0 or under lysine concentration is not less than the condition of 1.0g/dL; Flow out from the lower end that is in adsorption zone omega-cation exchange resin column group then, can under the situation that improves the Methionin yield, further save the sulfuric acid consumption.
Among the present invention; When adopting the placed in-line successively cation exchange resin column group of many groups; For the intravital pressure of the post that alleviates cation exchange resin column, increase the work-ing life of cylinder and resin, under the preferable case; Between the two adjacent groups cation exchange resin column group of adsorption zone, be provided with the transfer jar, two adjacent groups cation exchange resin column group is connected in series through the transfer jar.
Among the present invention, the pH value is preferably regulated through adding sulfuric acid.
Among the present invention, the cation exchange resin column group that is in adsorption zone simultaneously is preferably three groups, every group of cation exchange resin column that comprises 3-6 parallel connection.In order not only to reach the good adsorption effect but also further save the vitriolic consumption; Under the preferable case; Contain lysine solution under the condition of adjust pH not through being in the first and deputy cation exchange resin column group of adsorption zone; Making through the lysine concentration in the liquid after the cation exchange resin column group of adsorption zone first place and before the deputy cation exchange resin column group of process adsorption zone is being 1.0-2.0g/dL, is through being in adsorption zone omega-cation exchange resin column group under the condition of 1.8-2.0 in the pH value.
In the pH value is through being in the implementation method of adsorption zone omega-cation exchange resin column group under the condition of 1.8-2.0; Can be in the process of adsorption zone omega-cation exchange resin column group absorption; In adsorption zone omega-cation exchange resin column group, add the sulphur acid for adjusting pH value; Also can in the transfer jar before being in adsorption zone omega-cation exchange resin column group, add the sulphur acid for adjusting pH value; In order to make pH value condition more stable, be preferably that adjust pH is 1.8-2.0 in the transfer jar before being in adsorption zone omega-cation exchange resin column group.
It will be understood by those skilled in the art that generally speaking cation exchange resin column is saturated through all not adsorbing behind the adsorption zone; And when containing lysine solution and flowing through the cation exchange resin column group; The small amount of impurities that contains in the lysine solution also can remain in the cation exchange resin column, therefore, and in order to reduce the impurity that remains in the cation exchange resin column; Also in order to make cation exchange resin column absorption be tending towards saturated; The inventive method comprises also that preferably cation exchange resin column is through after the adsorption zone, before alkali leads the district, also through the back filled region, in the back filled region; With part elutriant backfill cation exchange resin column, cation exchange resin column is purified and absorption once more.
Owing to from the effusive liquid of said cation exchange resin column, contain Methionin after the backfill; Therefore, under the preferable case, return adsorption zone from the effusive liquid of cation exchange resin column after the backfill; Mix as the said lysine solution that contains with Methionin membrane filtration liquid; Therefore, the said lysine solution that contains is formed from the effusive liquid two portions of cation exchange resin column after by Methionin membrane filtration liquid and backfill, contains that the concentration of Methionin is generally 10.0-15.0g/dL in the lysine solution.
Zeo-karb and basic soln are addressed in preamble, repeat no more at this.
Because the present invention is with respect to the improvement of prior art; At adsorption zone, limit containing the lysine concentration and the pH value condition of lysine solution through the cation exchange resin column group, and in the breeding blanket; Saved the step of regulating waste liquor PH value backfill cation exchange resin column with sulfuric acid; Therefore, otherwise parameter and numerical value thereof do not have particular requirement, all can be with reference to prior art.For example; Contain time and temperature, the flow velocity of back filled region part elutriant and flow velocity and temperature, the flow velocity of breeding blanket water and the air pressure and the temperature of temperature and air that temperature, alkali are led district's basic soln that lysine solution contacts with Zeo-karb for adsorption zone and do not have particular requirement; Can adopt this area condition commonly used; For example, the condition of absorption comprises that temperature is 40-60 ℃; Containing the time that lysine solution contacts with Zeo-karb under the condition of adjust pH not is 17-20min, is that the time that contacts with Zeo-karb under the condition of 1.0-2.0 is 8-10min at adjust pH; The condition that purifies with absorption once more comprises, the flow velocity of part elutriant be 2.0-4.0 times of column volume/hour, temperature is 40-60 ℃; The condition of desorb comprises, the flow velocity of basic soln be 4.0-8.0 times of column volume/hour, temperature is 40-60 ℃; The regenerated condition comprises, the flow velocity of water be 4.5-8.5 times of column volume/hour, temperature is 40-60 ℃, the air pressure of air is 0.07-0.15MPa, temperature is 15-30 ℃.
Among the present invention, the consumption of the part elutriant of every cation exchange resin column of backfill is preferably 0.4-0.6 times of column volume; The consumption of basic soln does not have particular requirement, as long as the Methionin of absorption is eluted; In the breeding blanket, the consumption of the water of every cation exchange resin column use is preferably 0.35-0.65 times of column volume, and the consumption of the air of 0.07-0.15MPa does not have particular requirement, as long as the water in the cation exchange resin column is discharged.
Among the present invention, waste liquid refers to from the lower end of adsorption zone omega-cation exchange resin column group and flows out the liquid that obtains.
Therefore; As shown in Figure 2, according to a kind of preferred implementation of the inventive method be: make to contain lysine solution and carry out ion-exchange chromatography with many groups cation exchange resin column groups of contact and separate, every group of cation exchange resin column group led district and breeding blanket through adsorption zone, back filled region, alkali successively and circularly; So that the cation exchange resin column group exchanges absorption successively and circularly, purifies and absorption once more, desorb and regeneration; Obtain elutriant after the desorb, wherein
Three groups of placed in-line successively cation exchange resin column groups are in adsorption zone simultaneously; Every group of cation exchange resin column group preferably includes the cation exchange resin column of 3-6 parallel connection; Zeo-karb in the cation exchange resin column is a sulfonic group strong-acid type cation exchange resin; The total exchange capacity of Zeo-karb is greater than 5mmol/g; Be provided with the transfer jar between the two adjacent groups cation exchange resin column group; Two adjacent groups cation exchange resin column group is connected in series through the transfer jar; The concentration that contains lysine solution is 10.0-15.0g/dL, and temperature is 40-60 ℃, introduces from the upper end that is in the first cation exchange resin column group of adsorption zone; Flow through successively and respectively organize the cation exchange resin column group in this adsorption zone; Flow out from the lower end that is in adsorption zone omega-cation exchange resin column group then, and contain lysine solution under the condition of adjust pH not through be in adsorption zone the first with deputy cation exchange resin column group, making through the lysine concentration in the liquid after the first cation exchange resin column group of adsorption zone and before the deputy cation exchange resin column group of process adsorption zone is being 1.0-2.0g/dL; The time that under the condition of adjust pH not, contacts with Zeo-karb is 17-20min; Adding the sulfuric acid adjust pH in the transfer jar before being in adsorption zone omega-cation exchange resin column group is 1.8-2.0, is that the time that contacts with Zeo-karb under the condition of 1.8-2.0 is 8-10min at adjust pH, finally makes the lysine concentration from the effusive liquid in lower end of adsorption zone omega-cation exchange resin column group not be higher than 0.1g/dL;
In the back filled region; Use the part elutriant; Temperature is 40-60 ℃, with 2.0-4.0 times of column volume/hour flow velocity backfill cation exchange resin column, the consumption of the part elutriant of every cation exchange resin column of backfill be column volume 0.4-0.6 doubly; Return adsorption zone from the effusive liquid of cation exchange resin column after the backfill, mix with the said lysine solution that contains;
Lead the district at alkali, make the pH value for 11.0-12.5, temperature be 40-60 ℃ ammoniacal liquor with 4.0-8.0 times of column volume/hour the flow velocity cation exchange resin column of flowing through, make the Methionin desorb that is adsorbed onto on the Zeo-karb obtain elutriant;
In the breeding blanket; Use temperature as 40-60 ℃ of water with 4.5-8.5 times of column volume/hour the flow velocity cation exchange resin column of flowing through; The consumption of the water that every cation exchange resin column uses as the 0.35-0.65 of column volume doubly; Making temperature then is that 15-30 ℃ air is crossed cation exchange resin column with the Pneumatic pipe cleaner of 0.07-0.15MPa, makes cation exchange resin column be able to regeneration.
More than combine accompanying drawing to describe preferred implementation of the present invention in detail; But; The present invention is not limited to the detail in the above-mentioned embodiment; In technical conceive scope of the present invention, can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.
Need to prove in addition; Each concrete technical characterictic described in above-mentioned embodiment under reconcilable situation, can make up through any suitable manner; For fear of unnecessary repetition, the present invention is to the explanation no longer separately of various possible array modes.
In addition, also can carry out arbitrary combination between the various embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be regarded as the disclosed content of the present invention equally.
Embodiment
Following embodiment will be further described the present invention, but therefore not limit the present invention.
In following embodiment and Comparative Examples:
The special-purpose strongly acidic cation-exchange of WD-2 type Methionin is a sulfonic group strong-acid type cation exchange resin, purchases the Chuzhou City tabernaemontanus bulrush east chemical industry ltd in Anhui Province.
According to GB10794-89 standard detection lysine concentration (in lysine hydrochloride).
Embodiment 1
Adopt technology shown in Figure 2; Make and contain lysine solution and carry out ion-exchange chromatography with many groups cation exchange resin column groups of contact and separate; Every group of cation exchange resin column group led district and breeding blanket through adsorption zone, back filled region, alkali successively and circularly, so that the cation exchange resin column group exchanges absorption successively and circularly, purifies and absorption once more, desorb and regeneration, obtains elutriant after the desorb; Wherein
Three groups of placed in-line successively cation exchange resin column groups are in adsorption zone simultaneously; Every group of cation exchange resin column group is made up of the cation exchange resin column of 4 parallel connections; Zeo-karb in the cation exchange resin column is the special-purpose strongly acidic cation-exchange of WD-2 type Methionin; The total exchange capacity of Zeo-karb is 8mmol/g; Be provided with the transfer jar between the two adjacent groups cation exchange resin column group; Two adjacent groups cation exchange resin column group is connected in series through the transfer jar; The concentration that contains lysine solution is 13.0g/dL, and temperature is 50 ℃, introduces from the upper end that is in the first cation exchange resin column group of adsorption zone; Flow through successively and respectively organize the cation exchange resin column group in this adsorption zone; Flow out from the lower end that is in adsorption zone omega-cation exchange resin column group then, and contain lysine solution under the condition of adjust pH not through be in adsorption zone the first with deputy cation exchange resin column group, be 1.5g/dL through the lysine concentration in the liquid after the first cation exchange resin column group of adsorption zone and before the deputy cation exchange resin column group of process adsorption zone; The time that under the condition of adjust pH not, contacts with Zeo-karb is 17min; Adding the sulfuric acid adjust pH in the transfer jar before being in adsorption zone omega-cation exchange resin column group is 2.0, is that the time that contacts with Zeo-karb under 2.0 the condition is 8.5min at adjust pH, and the lysine concentration of result from the effusive liquid in lower end of adsorption zone omega-cation exchange resin column group is 0.04g/dL;
In the back filled region; Every cation exchange resin column is with part elutriant (be column volume 0.525 times); Temperature is 50 ℃; With 3.5 times of column volumes/hour flow velocity backfill cation exchange resin column, return adsorption zone from the effusive liquid of cation exchange resin column after the backfill, mix with the said lysine solution that contains;
Lead the district at alkali, making the pH value is 11.5, temperature be 50 ℃ ammoniacal liquor with 6.0 times of column volumes/hour the flow velocity cation exchange resin column of flowing through, make the Methionin desorb that is adsorbed onto on the Zeo-karb obtain elutriant;
In the breeding blanket; Every cation exchange resin column uses temperature be 50 ℃ of water (as 0.45 times of column volume) with 6.0 times of column volumes/hour the flow velocity cation exchange resin column of flowing through; Making temperature then is that 20 ℃ air is crossed cation exchange resin column with the Pneumatic pipe cleaner of 0.12MPa, makes cation exchange resin column be able to regeneration.
Embodiment 2
Adopt technology shown in Figure 2; Make and contain lysine solution and carry out ion-exchange chromatography with many groups cation exchange resin column groups of contact and separate; Every group of cation exchange resin column group led district and breeding blanket through adsorption zone, back filled region, alkali successively and circularly, so that the cation exchange resin column group exchanges absorption successively and circularly, purifies and absorption once more, desorb and regeneration, obtains elutriant after the desorb; Wherein
Three groups of placed in-line successively cation exchange resin column groups are in adsorption zone simultaneously; Every group of cation exchange resin column group is made up of the cation exchange resin column of 3 parallel connections; Zeo-karb in the cation exchange resin column is the special-purpose strongly acidic cation-exchange of WD-2 type Methionin; The total exchange capacity of Zeo-karb is 8mmol/g; Be provided with the transfer jar between the two adjacent groups cation exchange resin column group; Two adjacent groups cation exchange resin column group is connected in series through the transfer jar; The concentration that contains lysine solution is 10.0g/dL, and temperature is 40 ℃, introduces from the upper end that is in the first cation exchange resin column group of adsorption zone; Flow through successively and respectively organize the cation exchange resin column group in this adsorption zone; Flow out from the lower end that is in adsorption zone omega-cation exchange resin column group then, and contain lysine solution under the condition of adjust pH not through be in adsorption zone the first with deputy cation exchange resin column group, be 1.0g/dL through the lysine concentration in the liquid after the first cation exchange resin column group of adsorption zone and before the deputy cation exchange resin column group of process adsorption zone; The time that under the condition of adjust pH not, contacts with Zeo-karb is 19min; Adding the sulfuric acid adjust pH in the transfer jar before being in adsorption zone omega-cation exchange resin column group is 1.8, is that the time that contacts with Zeo-karb under 1.8 the condition is 9.5min at adjust pH, and the lysine concentration of result from the effusive liquid in lower end of adsorption zone omega-cation exchange resin column group is 0.02g/dL;
In the back filled region; Every cation exchange resin column is with part elutriant (be column volume 0.5 times); Temperature is 40 ℃; With 3.0 times of column volumes/hour flow velocity backfill cation exchange resin column, return adsorption zone from the effusive liquid of cation exchange resin column after the backfill, mix with the said lysine solution that contains;
Lead the district at alkali, making the pH value is 11.0, temperature be 40 ℃ ammoniacal liquor with 4.8 times of column volumes/hour the flow velocity cation exchange resin column of flowing through, make the Methionin desorb that is adsorbed onto on the Zeo-karb obtain elutriant;
In the breeding blanket; Every cation exchange resin column uses temperature be 40 ℃ of water (as 0.375 times of column volume) with 4.5 times of column volumes/hour the flow velocity cation exchange resin column of flowing through; Making temperature then is that 15 ℃ air is crossed cation exchange resin column with the Pneumatic pipe cleaner of 0.15MPa, makes cation exchange resin column be able to regeneration.
Embodiment 3
Adopt technology shown in Figure 2; Make and contain lysine solution and carry out ion-exchange chromatography with many groups cation exchange resin column groups of contact and separate; Every group of cation exchange resin column group led district and breeding blanket through adsorption zone, back filled region, alkali successively and circularly, so that the cation exchange resin column group exchanges absorption successively and circularly, purifies and absorption once more, desorb and regeneration, obtains elutriant after the desorb; Wherein
Three groups of placed in-line successively cation exchange resin column groups are in adsorption zone simultaneously; Every group of cation exchange resin column group is made up of the cation exchange resin column of 6 parallel connections; Zeo-karb in the cation exchange resin column is the special-purpose strongly acidic cation-exchange of WD-2 type Methionin; The total exchange capacity of Zeo-karb is 8mmol/g; Be provided with the transfer jar between the two adjacent groups cation exchange resin column group; Two adjacent groups cation exchange resin column group is connected in series through the transfer jar; The concentration that contains lysine solution is 15.0g/dL, and temperature is 60 ℃, introduces from the upper end that is in the first cation exchange resin column group of adsorption zone; Flow through successively and respectively organize the cation exchange resin column group in this adsorption zone; Flow out from the lower end that is in adsorption zone omega-cation exchange resin column group then, and contain lysine solution under the condition of adjust pH not through be in adsorption zone the first with deputy cation exchange resin column group, be 2.0g/dL through the lysine concentration in the liquid after the first cation exchange resin column group of adsorption zone and before the deputy cation exchange resin column group of process adsorption zone; The time that under the condition of adjust pH not, contacts with Zeo-karb is 17min; Adding the sulfuric acid adjust pH in the transfer jar before being in adsorption zone omega-cation exchange resin column group is 1.9, is that the time that contacts with Zeo-karb under 1.9 the condition is 8.5min at adjust pH, and the lysine concentration of result from the effusive liquid in lower end of adsorption zone omega-cation exchange resin column group is 0.05g/dL;
In the back filled region; Every cation exchange resin column is with part elutriant (be column volume 0.6 times); Temperature is 60 ℃; With 4.0 times of column volumes/hour flow velocity backfill cation exchange resin column, return adsorption zone from the effusive liquid of cation exchange resin column after the backfill, mix with the said lysine solution that contains;
Lead the district at alkali, making the pH value is 12.5, temperature be 60 ℃ ammoniacal liquor with 5.5 times of column volumes/hour the flow velocity cation exchange resin column of flowing through, make the Methionin desorb that is adsorbed onto on the Zeo-karb obtain elutriant;
In the breeding blanket; Every cation exchange resin column uses temperature be 60 ℃ of water (as 0.5 times of column volume) with 6.5 times of column volumes/hour the flow velocity cation exchange resin column of flowing through; Making temperature then is that 30 ℃ air is crossed cation exchange resin column with the Pneumatic pipe cleaner of 0.07MPa, makes cation exchange resin column be able to regeneration.
Comparative Examples 1
Handle according to the method for embodiment 1 and to contain lysine solution, different is, at adsorption zone, contain lysine solution under the condition of adjust pH not successively through being in placed in-line successively three groups of cation exchange resin column groups of adsorption zone; In the breeding blanket; After making air pass through cation exchange resin column; Regulate from the pH value to 1.0 of the effusive liquid in lower end of adsorption zone omega-cation exchange resin column group with sulfuric acid; Then with regulate after the pH value liquid with 3 times of column volumes/hour flow velocity backfill cation exchange resin column; The consumption of the liquid after the adjusting pH value of every cation exchange resin column of backfill is 0.45 times of column volume, and the cation exchange resin column after the backfill gets into adsorption zone again and carries out next round to containing the processing of lysine solution.The content that records the Methionin from the effusive liquid in lower end of adsorption zone omega-cation exchange resin column group is 0.08g/dL.
Can find out with Comparative Examples 1 from embodiment 1; The lysine concentration of embodiment 1 from the effusive liquid in lower end of adsorption zone omega-cation exchange resin column group is 0.04g/dL; The content of the Methionin of Comparative Examples 1 from the effusive liquid in lower end of adsorption zone omega-cation exchange resin column group is 0.08g/dL, and the visible treatment process that contains lysine solution of the present invention has improved the yield of Methionin.
The treatment process that contains lysine solution provided by the invention has improved the yield of Methionin; Every group of cation exchange resin column group provided by the invention led the method for district and breeding blanket successively and circularly through adsorption zone, alkali; Pass through adsorption zone omega-cation exchange resin column group in pH value under for the condition that is not less than 1.0g/dL under the condition of 1.0-2.0 or at lysine concentration owing to contain lysine solution; Saved the step of using sulfuric acid to transfer the waste liquor PH value cation exchange resin column to be made the transition in the breeding blanket as 1.0-1.2; Under the identical situation of the cation exchange resin column group mode of connection of adsorption zone; Save the sulfuric acid consumption greatly, reduced production cost.The treatment process that contains lysine solution provided by the invention can be widely used in industrial production.
Claims (19)
1. treatment process that contains lysine solution; Said method comprises: make the said lysine solution that contains successively through one or more groups placed in-line successively cation exchange resin column group; Be adsorbed to that lysine concentration is not higher than 0.1g/dL from the terminal effusive liquid of this one or more groups placed in-line successively cation exchange resin column group so that contain Methionin in the lysine solution; Every group of cation exchange resin column group comprises the cation exchange resin column of one or more parallel connections; Cation exchange resin column after using basic soln to absorption Methionin then carries out wash-out; Obtain containing the elutriant of Methionin, it is characterized in that, said contain lysine solution the pH value for the condition that is not less than 1.0g/dL under the condition of 1.0-2.0 or at lysine concentration under through said cation exchange resin column group.
2. method according to claim 1, wherein, said contain lysine solution the pH value for the condition that is not less than 1.0g/dL under the condition of 1.8-2.0 or at lysine concentration under through said cation exchange resin column group.
3. method according to claim 1 and 2, wherein, said cation exchange resin column group is three groups, every group of cation exchange resin column that comprises 3-6 parallel connection.
4. according to any described method among the claim 1-3, wherein, the Zeo-karb in the said cation exchange resin column is a sulfonic group strong-acid type cation exchange resin, and the total exchange capacity of said Zeo-karb is greater than 5mmol/g.
5. according to any described method among the claim 1-4, wherein, the pH value is regulated through adding sulfuric acid.
6. according to any described method among the claim 1-5, wherein, said basic soln is an ammoniacal liquor, and the pH value is 10.0-14.0, is preferably 11.0-12.5.
7. treatment process that contains lysine solution; It is characterized in that; Said method comprises: make the said lysine solution that contains carry out ion-exchange chromatography with many groups cation exchange resin column groups of contact and separate, every group of cation exchange resin column group led district and breeding blanket through adsorption zone, alkali successively and circularly, so that the cation exchange resin column group exchanges absorption, desorb and regeneration successively and circularly; Obtain elutriant after the desorb; Said every group of cation exchange resin column group comprises the cation exchange resin column of one or more parallel connections, wherein
One or more groups placed in-line successively cation exchange resin column group is in adsorption zone simultaneously; The said lysine solution that contains is introduced from the upper end that is in the first cation exchange resin column group of adsorption zone; In the pH value for respectively organizing the cation exchange resin column group in this adsorption zone of flowing through successively under the condition of 1.0-2.0 or under lysine concentration is not less than the condition of 1.0g/dL; Flow out from the lower end that is in adsorption zone omega-cation exchange resin column group then; The said Methionin of part at least that contains in the lysine solution is adsorbed onto on the Zeo-karb, and makes the lysine concentration in the effusive liquid not be higher than 0.1g/dL; Lead the district at alkali, make the basic soln said cation exchange resin column of flowing through, make the Methionin desorb that is adsorbed onto on the Zeo-karb obtain said elutriant; In the breeding blanket, make water and air successively through cation exchange resin column, make cation exchange resin column be able to regeneration.
8. method according to claim 7; Wherein, The said lysine solution that contains is introduced from the upper end that is in the first cation exchange resin column group of adsorption zone;, flow out from the lower end that is in adsorption zone omega-cation exchange resin column group then for respectively organizing the cation exchange resin column group in this adsorption zone of flowing through successively under the condition of 1.8-2.0 or under lysine concentration is not less than the condition of 1.0g/dL in the pH value.
9. according to claim 7 or 8 described methods, wherein, between the two adjacent groups cation exchange resin column group of adsorption zone, be provided with the transfer jar, two adjacent groups cation exchange resin column group is connected in series through said transfer jar.
10. according to any described method among the claim 7-9, wherein, the cation exchange resin column group that is in adsorption zone simultaneously is three groups, every group of cation exchange resin column that comprises 3-6 parallel connection.
11. method according to claim 10; Wherein, Said contain lysine solution under the condition of adjust pH not through being in the first and deputy cation exchange resin column group of adsorption zone; Making through the lysine concentration in the liquid after the cation exchange resin column group of adsorption zone first place and before the deputy cation exchange resin column group of process adsorption zone is being 1.0-2.0g/dL, is through being in adsorption zone omega-cation exchange resin column group under the condition of 1.8-2.0 in the pH value.
12. method according to claim 11, wherein, adjust pH is 1.8-2.0 in the transfer jar before being in adsorption zone omega-cation exchange resin column group.
13. according to any described method among the claim 7-12; Wherein, The condition of said absorption comprises; Temperature is 40-60 ℃, and containing the time that lysine solution contacts with Zeo-karb under the condition of adjust pH not is 17-20min, is that the time that contacts with Zeo-karb under the condition of 1.0-2.0 is 8-10min at adjust pH; The condition of said desorb comprises, the flow velocity of said basic soln be 4.0-8.0 times of column volume/hour, temperature is 40-60 ℃; Said regenerated condition comprises, the flow velocity of said water be 4.5-8.5 times of column volume/hour, temperature is 40-60 ℃, the air pressure of said air is 0.07-0.15MPa, temperature is 15-30 ℃.
14. according to any described method among the claim 7-13; Wherein, Said method comprises that also said cation exchange resin column is through after the adsorption zone, before alkali leads the district, also through the back filled region, in the back filled region; With the said cation exchange resin column of the said elutriant backfill of part, said cation exchange resin column is purified and absorption once more.
15. method according to claim 14 wherein, is returned adsorption zone from the effusive liquid of said cation exchange resin column after the backfill, mixes with the said lysine solution that contains.
16. according to claim 14 or 15 described methods, wherein, said purification and once more absorption condition comprise, the flow velocity of the said elutriant of said part be 2.0-4.0 times of column volume/hour, temperature is 40-60 ℃.
17. according to any described method among the claim 7-16, wherein, the Zeo-karb in the said cation exchange resin column is a sulfonic group strong-acid type cation exchange resin, the total exchange capacity of said Zeo-karb is greater than 5mmol/g.
18. according to any described method among the claim 7-17, wherein, the pH value is regulated through adding sulfuric acid.
19. according to any described method among the claim 7-18, wherein, said basic soln is an ammoniacal liquor, the pH value is 10.0-14.0, is preferably 11.0-12.5.
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| CN103497118A (en) * | 2013-09-30 | 2014-01-08 | 中粮生物化学（安徽）股份有限公司 | Treatment method for lysine-containing solution |
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| US4714767A (en) * | 1984-07-11 | 1987-12-22 | Ajinomoto Co., Inc. | Process for the separation of a basic amino acid from a fermentation broth using cation exchange resins |
| US4997754A (en) * | 1987-08-10 | 1991-03-05 | Ajinomoto Co., Inc. | Process for recovering L-amino acids from fermentation liquors containing them |
| US5279744A (en) * | 1990-09-25 | 1994-01-18 | Ajinomoto Co., Inc. | Method for purification of an amino acid using ion exchange resin |
| CN102206169A (en) * | 2011-03-25 | 2011-10-05 | 安徽丰原生物化学股份有限公司 | Purification method for lysine |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4714767A (en) * | 1984-07-11 | 1987-12-22 | Ajinomoto Co., Inc. | Process for the separation of a basic amino acid from a fermentation broth using cation exchange resins |
| US4997754A (en) * | 1987-08-10 | 1991-03-05 | Ajinomoto Co., Inc. | Process for recovering L-amino acids from fermentation liquors containing them |
| US5279744A (en) * | 1990-09-25 | 1994-01-18 | Ajinomoto Co., Inc. | Method for purification of an amino acid using ion exchange resin |
| CN102206169A (en) * | 2011-03-25 | 2011-10-05 | 安徽丰原生物化学股份有限公司 | Purification method for lysine |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103497118A (en) * | 2013-09-30 | 2014-01-08 | 中粮生物化学（安徽）股份有限公司 | Treatment method for lysine-containing solution |
| CN103497118B (en) * | 2013-09-30 | 2015-04-22 | 中粮生物化学（安徽）股份有限公司 | Treatment method for lysine-containing solution |
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