CN102617379B - A kind for the treatment of process containing lysine solution - Google Patents
A kind for the treatment of process containing lysine solution Download PDFInfo
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- CN102617379B CN102617379B CN201210050611.8A CN201210050611A CN102617379B CN 102617379 B CN102617379 B CN 102617379B CN 201210050611 A CN201210050611 A CN 201210050611A CN 102617379 B CN102617379 B CN 102617379B
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Abstract
The invention discloses a kind for the treatment of process containing lysine solution, described method comprises: make containing lysine solution successively by cation exchange resin column group that one or more groups is connected successively, to the liquid that the end of the cation exchange resin column group of connecting successively from this one or more groups flows out, lysine concentration is not higher than 0.1g/dL, often organize the cation exchange resin column that cation exchange resin column group comprises one or more parallel connection, then basic solution is used to carry out wash-out to the cation exchange resin column after absorption Methionin, obtain the elutriant containing Methionin, it is characterized in that, described containing lysine solution be under the condition of 1.0-2.0 in pH value or be not less than the condition of 1.0g/dL at lysine concentration under by described cation exchange resin column group.The invention also discloses a kind for the treatment of process of the circulation containing lysine solution.The inventive method can improve the yield of Methionin, can be widely used in industrial production.
Description
Technical field
The present invention relates to a kind for the treatment of process containing lysine solution.
Background technology
Methionin is one of eight kinds of primary amino acids (also known as indispensable amino acid, they are Methionin, Threonine, leucine, Isoleucine, methionine(Met), α-amino-isovaleric acid, phenylalanine and tryptophane) of needed by human.The solubleness of Methionin in water is very large, and easily absorbs the carbonic acid gas in air, is difficult to obtain its crystallization.Therefore as commodity, it often occurs with the form of mono-hydrochloric salts.Methionin is of many uses, is mainly used in following industry: foodstuffs industry, prepares nutrition-fortifying agent, tasty agents, sweeting agent; Fodder industry, prepares nutrition-fortifying agent; Medicine industry, Preparation of amino acid transfusion, amino acid derivative, amino acid salts; Chemical industry, making detergent, skin care product, leatheroid; Agricultural, prepares public nuisance-free agricultural chemicals etc.At present, the lysine product of more than 90% is used for fodder industry, as added appropriate Methionin in feed, can increase the synthesis of animal body internal protein, promotes animal growth.
Lysine hydrochloride is generally adopted and is prepared with the following method: strain fermentation obtains fermented liquid, adding a large amount of vitriol oils in fermented liquid adjusts pH to 2.0-3.0 to carry out acidifying, through metallic membrane or ceramic membrane filter removing thalline after acidifying, obtain Methionin membrane filtration liquid namely containing lysine solution, adopt strongly acidic cation-exchange to carry out absorption containing lysine solution to exchange, the saturated rear weak ammonia of resin absorption carries out wash-out, the Methionin eluted, through concentrated, salt acid for adjusting pH value, crystallization, solid-liquid separation, oven dry, obtains lysine hydrochloride finished product.
Along with the raising of modernization level, large chemical equipment ISEP system is generally adopted to carry out containing the ion exchange purification Methionin of lysine solution at present, principle is: make to contact containing lysine solution carry out ion exchange mechansim with cation exchange resin column group of organizing more, often organize the cation exchange resin column that cation exchange resin column group comprises one or more parallel connection, often organize cation exchange resin column group successively and cyclically through adsorption zone, back filled region, Jian Dao district and breeding blanket, to make cation exchange resin column group successively and cyclically to carry out exchange adsorption, purify and again adsorb, desorb and regeneration, elutriant is obtained after desorb.Methionin mainly exists with monovalent cation form, and the ion exchange reaction formula of adsorption and desorption is as follows:
R-H+HLysH
+→R-HLysH+H
+
R-HLysH+NH
4 ++OH
-→R-NH
4+HLys+H
2O
As shown in Figure 1, the technique of current use generally comprises: in adsorption zone, cation exchange resin column group is sequentially connected in series, introduce containing the upper end of lysine solution from the cation exchange resin column group being in first place, adsorption zone, flow through each group of cation exchange resin column group in this adsorption zone successively, and obtain waste liquid from the lower end outflow of the cation exchange resin column group being in position, end, adsorption zone, make the described at least part of Methionin contained in lysine solution be adsorbed onto on Zeo-karb; In back filled region, with obtain elution fractions backfill cation exchange resin column, make cation exchange resin column purify and and be tending towards absorption saturated; In Jian Dao district, make basic solution flow through cation exchange resin column, make the Methionin desorb be adsorbed onto on Zeo-karb obtain elutriant; In breeding blanket, first use hot wash cation exchange resin column, with air compression leg, the water in cation exchange resin column is discharged again, then sulfuric acid adjust pH is added to 1.0-1.2 in the waste liquid obtained to adsorption zone, with the waste liquid backfill cation exchange resin column after adjust pH, cation exchange resin column is made the transition, and then cation exchange resin column returns to adsorption zone again and adsorbs, and completes and once circulates.
ISEP system adopts the technique used at present, although make the transition to cation exchange resin column with the waste liquid that pH value is 1.0-1.2, remains in the H in cation exchange resin column after transition
+amount limited, in adsorption zone, the pH value passing through the cation exchange resin column group of first place, adsorption zone containing lysine solution is still about 2.0-3.0, when there is the cation exchange resin column group that at least two groups are sequentially connected in series in adsorption zone simultaneously, higher by the pH value of cation exchange resin column group below containing lysine solution, thus cation exchange resin column is lower to the adsorptive power containing lysine solution, thus Methionin yield is low.
Summary of the invention
The object of the invention is the defect that in the technique in order to overcome use at present, Methionin yield is low, a kind for the treatment of process containing lysine solution is newly provided.
The present inventor surprisingly finds under study for action, the cation exchange resin column group of being connected successively by one or more groups successively containing lysine solution is made to carry out exchange adsorption, when the liquid that the end of the cation exchange resin column group making to connect successively from one or more groups flows out, lysine concentration is not higher than 0.1g/dL, containing lysine solution be under the condition of 1.0-2.0 in pH value or be not less than 1.0g/dL at lysine concentration condition under can be improved the yield of Methionin by cation exchange resin column group.
Therefore, to achieve these goals, on the one hand, the invention provides a kind for the treatment of process containing lysine solution, described method comprises: make described containing lysine solution successively by cation exchange resin column group that one or more groups is connected successively, the liquid flowed out to make the end being adsorbed to the cation exchange resin column group of connecting successively from this one or more groups containing the Methionin in lysine solution, lysine concentration is not higher than 0.1g/dL, often organize the cation exchange resin column that cation exchange resin column group comprises one or more parallel connection, then basic solution is used to carry out wash-out to the cation exchange resin column after absorption Methionin, obtain the elutriant containing Methionin, it is characterized in that, described containing lysine solution be under the condition of 1.0-2.0 in pH value or be not less than the condition of 1.0g/dL at lysine concentration under by described cation exchange resin column group.
Preferably, described containing lysine solution be under the condition of 1.8-2.0 in pH value or be not less than the condition of 1.0g/dL at lysine concentration under by described cation exchange resin column group.
On the other hand, present invention also offers a kind for the treatment of process containing lysine solution, it is characterized in that, described method comprises: make described contact containing lysine solution carry out ion exchange mechansim with cation exchange resin column group of organizing more, often organize cation exchange resin column group successively and cyclically through adsorption zone, Jian Dao district and breeding blanket, to make cation exchange resin column group successively and cyclically to carry out exchange adsorption, desorb and regeneration, elutriant is obtained after desorb, the described cation exchange resin column often organized cation exchange resin column group and comprise one or more parallel connection, wherein,
One or more groups cation exchange resin column group of connecting successively is in adsorption zone simultaneously, the described lysine solution that contains is introduced from the upper end of the cation exchange resin column group being in first place, adsorption zone, be be not less than each group of cation exchange resin column group flowed through successively under the condition of 1.0g/dL in this adsorption zone under the condition of 1.0-2.0 or at lysine concentration in pH value, then flow out from the lower end of the cation exchange resin column group being in position, end, adsorption zone, the described at least part of Methionin contained in lysine solution is made to be adsorbed onto on Zeo-karb, and make lysine concentration in the liquid of outflow not higher than 0.1g/dL, in Jian Dao district, make basic solution flow through described cation exchange resin column, make the Methionin desorb be adsorbed onto on Zeo-karb obtain described elutriant, in breeding blanket, with water and air successively by cation exchange resin column, cation exchange resin column is regenerated.
Preferably, the described lysine solution that contains is introduced from the upper end of the cation exchange resin column group being in first place, adsorption zone, be be not less than each group of cation exchange resin column group flowed through successively under the condition of 1.0g/dL in this adsorption zone under the condition of 1.8-2.0 or at lysine concentration in pH value, then flow out from the lower end of the cation exchange resin column group being in position, end, adsorption zone.
Treatment process containing lysine solution provided by the invention, improve the yield of Methionin, as shown in embodiment 1 and comparative example 1, embodiment 1 is 0.04g/dL from the lysine concentration the liquid that the lower end of the cation exchange resin column group of position, end, adsorption zone is flowed out, and comparative example 1 is 0.08g/dL from the content of the Methionin the liquid that the lower end of the cation exchange resin column group of position, end, adsorption zone is flowed out; Provided by the invention often organize cation exchange resin column group successively and cyclically through adsorption zone, the method for Jian Dao district and breeding blanket, due to containing lysine solution in pH value be 1.0-2.0 condition under or be not less than 1.0g/dL at lysine concentration condition under by the cation exchange resin column group of adsorption zone, eliminate and adjust waste liquid pH value to be the step that 1.0-1.2 makes the transition to cation exchange resin column at breeding blanket sulfuric acid, when the cation exchange resin column group mode of connection of adsorption zone is identical, greatly save sulfuric acid dosage, reduce production cost.Treatment process containing lysine solution provided by the invention, can be widely used in industrial production.
Other features and advantages of the present invention are described in detail in embodiment part subsequently.
Accompanying drawing explanation
Fig. 1 is the process flow sheet that in the technique used at present, the process of ISEP system contains lysine solution;
Fig. 2 is the process flow sheet containing lysine solution according to the ISEP system process of the inventive method.
Embodiment
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described in detail.Should be understood that, embodiment described herein, only for instruction and explanation of the present invention, is not limited to the present invention.
On the one hand, the invention provides a kind for the treatment of process containing lysine solution, the method comprises: make containing lysine solution successively by cation exchange resin column group that one or more groups is connected successively, the liquid flowed out to make the end being adsorbed to the cation exchange resin column group of connecting successively from this one or more groups containing the Methionin in lysine solution, lysine concentration is not higher than 0.1g/dL, often organize the cation exchange resin column that cation exchange resin column group comprises one or more parallel connection, then basic solution is used to carry out wash-out to the cation exchange resin column after absorption Methionin, obtain the elutriant containing Methionin, by described cation exchange resin column group under the condition containing lysine solution being under the condition of 1.0-2.0 in pH value or be not less than 1.0g/dL at lysine concentration.
In preparing lysine through fermentation process, strain fermentation obtains fermented liquid, adding a large amount of vitriol oils in fermented liquid adjusts pH to 2.0-3.0 to carry out acidifying, Methionin membrane filtration liquid is obtained through metallic membrane or ceramic membrane filter removing thalline after acidifying, in the present invention, comprise this Methionin membrane filtration liquid containing lysine solution, in Methionin membrane filtration liquid, the concentration of Methionin is generally 14.0-18.0g/dL.
According to the present invention, although be under the condition of 1.0-2.0 in pH value containing lysine solution or object of the present invention can be realized by described cation exchange resin column group be not less than the condition of 1.0g/dL at lysine concentration under, namely improve the yield of Methionin.But under preferable case, containing lysine solution be under the condition of 1.8-2.0 in pH value or be not less than 1.0g/dL at lysine concentration condition under by described cation exchange resin column group, sulfuric acid dosage can be saved further when improving Methionin yield.
In the present invention, cation exchange resin column group is preferably three groups, often organizes the cation exchange resin column that cation exchange resin column group preferably includes 3-6 parallel connection.
In the present invention, Zeo-karb in cation exchange resin column can be used for the cationic various Zeo-karb that can adsorb 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, more preferably 6-15mmol/g, is further preferably 6-10mmol/g.
In the present invention, pH value regulates preferably by adding sulfuric acid.
In the present invention, from easy cation exchange resin column after absorption Methionin, Methionin is eluted and the aspect facilitating cation exchange resin column to regenerate consideration, basic solution is preferably ammoniacal liquor, and pH value is preferably 10.0-14.0, is more preferably 11.0-12.5.
On the other hand, the invention provides a kind for the treatment of process containing lysine solution, the method comprises: make to contact containing lysine solution carry out ion exchange mechansim with cation exchange resin column group of organizing more, often organize cation exchange resin column group successively and cyclically through adsorption zone, Jian Dao district and breeding blanket, to make cation exchange resin column group successively and cyclically to carry out exchange adsorption, desorb and regeneration, elutriant is obtained after desorb, often organize the cation exchange resin column that cation exchange resin column group comprises one or more parallel connection, wherein
One or more groups cation exchange resin column group of connecting successively is in adsorption zone simultaneously, introduce containing the upper end of lysine solution from the cation exchange resin column group being in first place, adsorption zone, be be not less than each group of cation exchange resin column group flowed through successively under the condition of 1.0g/dL in this adsorption zone under the condition of 1.0-2.0 or at lysine concentration in pH value, then flow out from the lower end of the cation exchange resin column group being in position, end, adsorption zone, make to be adsorbed onto on Zeo-karb containing at least part of Methionin in lysine solution, and make lysine concentration in the liquid of outflow not higher than 0.1g/dL, in Jian Dao district, make basic solution flow through cation exchange resin column, make the Methionin desorb be adsorbed onto on Zeo-karb obtain elutriant, in breeding blanket, with water and air successively by cation exchange resin column, cation exchange resin column is regenerated.
According to the present invention, although introduce containing the upper end of lysine solution from the cation exchange resin column group being in first place, adsorption zone, be be not less than each group of cation exchange resin column group flowed through successively under the condition of 1.0g/dL in this adsorption zone under the condition of 1.0-2.0 or at lysine concentration in pH value, then flow out from the lower end of the cation exchange resin column group being in position, end, adsorption zone, object of the present invention can be realized, namely improve the yield of Methionin.But under preferable case, introduce containing the upper end of lysine solution from the cation exchange resin column group being in first place, adsorption zone, be be not less than each group of cation exchange resin column group flowed through successively under the condition of 1.0g/dL in this adsorption zone under the condition of 1.8-2.0 or at lysine concentration in pH value, then flowing out from the lower end of the cation exchange resin column group being in position, end, adsorption zone, sulfuric acid dosage can be saved further when improving Methionin yield.
In the present invention, during the cation exchange resin column group adopting many groups to connect successively, in order to alleviate the pressure in the cylinder of cation exchange resin column, increase the work-ing life of cylinder and resin, under preferable case, between the two adjacent groups cation exchange resin column group of adsorption zone, be provided with transfer tank, two adjacent groups cation exchange resin column group is connected in series through transfer tank.
In the present invention, pH value regulates preferably by adding sulfuric acid.
In the present invention, the cation exchange resin column group being simultaneously in adsorption zone is preferably three groups, and often group comprises the cation exchange resin column of 3-6 parallel connection.In order to not only reach good adsorption effect but also save the consumption of sulfuric acid further, under preferable case, containing lysine solution under the condition of not adjust pH by being in the first and deputy cation exchange resin column group in adsorption zone, making after the cation exchange resin column group of first place, adsorption zone and in the liquid before the deputy cation exchange resin column group in adsorption zone lysine concentration be 1.0-2.0g/dL, is by being in the cation exchange resin column group of position, end, adsorption zone in pH value under the condition of 1.8-2.0.
Be by being in the implementation method of the cation exchange resin column group of position, end, adsorption zone in pH value under the condition of 1.8-2.0, can in the process of the cation exchange resin column group absorption of position, end, adsorption zone, sulfuric acid adjust ph is added in the cation exchange resin column group of position, end, adsorption zone, also sulfuric acid adjust ph can be added in the transfer tank before the cation exchange resin column group being in position, end, adsorption zone, in order to make pH value condition more stable, being preferably adjust pH in the transfer tank before the cation exchange resin column group being in position, end, adsorption zone is 1.8-2.0.
What those skilled in the art should understand that is, generally, cation exchange resin column all can not adsorb saturated behind adsorption zone, and when flowing through cation exchange resin column group containing lysine solution, also can remain in cation exchange resin column containing a small amount of impurity in lysine solution, therefore, in order to reduce the impurity remained in cation exchange resin column, also be tending towards saturated to make cation exchange resin column adsorb, the inventive method preferably also comprises cation exchange resin column after adsorption zone, before Jian Dao district, also through back filled region, in back filled region, cation exchange resin column is backfilled with elution fractions, cation exchange resin column is made to carry out purification and again adsorb.
Owing to containing Methionin after backfill from the liquid that described cation exchange resin column flows out, therefore, under preferable case, the liquid flowed out from cation exchange resin column after backfill returns to adsorption zone, mix with Methionin membrane filtration liquid as described containing lysine solution, therefore, the described lysine solution that contains is made up of the liquid two portions flowed out from cation exchange resin column after Methionin membrane filtration liquid and backfill, is generally 10.0-15.0g/dL containing the concentration of Methionin in lysine solution.
Zeo-karb and basic solution are addressed in the preceding article, do not repeat them here.
Because the present invention is relative to the improvement of prior art, in adsorption zone, limited by the lysine concentration of cation exchange resin column group and pH value condition containing lysine solution, and in breeding blanket, eliminate the step regulating waste liquid pH value backfill cation exchange resin column with sulfuric acid, therefore, otherwise parameter and numerical value thereof, without particular requirement, all can refer to prior art.Such as, the time that adsorption zone is contacted with Zeo-karb containing lysine solution and temperature, the flow velocity of back filled region elution fractions and temperature, the flow velocity of Jian Dao district basic solution and temperature, the air pressure of the flow velocity of breeding blanket water and temperature and air and temperature are without particular requirement, the condition that this area is conventional can be adopted, such as, the condition of absorption comprises, temperature is 40-60 DEG C, the time contacted with Zeo-karb under the condition of not adjust pH containing lysine solution is 17-20min, be the time contacted with Zeo-karb under the condition of 1.0-2.0 at adjust pH be 8-10min, purification and the again condition of adsorbing comprise, the flow velocity of elution fractions be 2.0-4.0 times of column volume/hour, temperature is 40-60 DEG C, the condition of desorb comprises, the flow velocity of basic solution be 4.0-8.0 times of column volume/hour, temperature is 40-60 DEG C, the condition of regeneration comprises, the flow velocity of water be 4.5-8.5 times of column volume/hour, temperature is 40-60 DEG C, and the air pressure of air is 0.07-0.15MPa, and temperature is 15-30 DEG C.
In the present invention, the consumption backfilling the elution fractions of every root cation exchange resin column is preferably the 0.4-0.6 of column volume doubly; The consumption of basic solution without particular requirement, as long as the Methionin of absorption is eluted; In breeding blanket, the consumption of the water that every root cation exchange resin column uses is preferably the 0.35-0.65 of column volume doubly, the consumption of the air of 0.07-0.15MPa without particular requirement, as long as the water in cation exchange resin column is discharged.
In the present invention, waste liquid refers to and flows out from the lower end of the cation exchange resin column group of position, end, adsorption zone the liquid obtained.
Therefore, as shown in Figure 2, a kind of preferred implementation according to the inventive method is: make to contact containing lysine solution carry out ion exchange mechansim with cation exchange resin column group of organizing more, often organize cation exchange resin column group successively and cyclically through adsorption zone, back filled region, Jian Dao district and breeding blanket, to make cation exchange resin column group successively and cyclically to carry out exchange adsorption, purification and Adsorption and desorption and regeneration again, elutriant is obtained, wherein after desorb
Three groups of cation exchange resin column groups of connecting successively are in adsorption zone simultaneously, often organize the cation exchange resin column that cation exchange resin column group preferably includes 3-6 parallel connection, Zeo-karb in cation exchange resin column is sulfonic group strong-acid type cation exchange resin, the total exchange capacity of Zeo-karb is greater than 5mmol/g, transfer tank is provided with between two adjacent groups cation exchange resin column group, two adjacent groups cation exchange resin column group is connected in series through transfer tank, concentration containing lysine solution is 10.0-15.0g/dL, temperature is 40-60 DEG C, introduce from the upper end of the cation exchange resin column group being in first place, adsorption zone, flow through each group of cation exchange resin column group in this adsorption zone successively, then flow out from the lower end of the cation exchange resin column group being in position, end, adsorption zone, and containing lysine solution under the condition of not adjust pH by being in the first and deputy cation exchange resin column group in adsorption zone, after the cation exchange resin column group of first place, adsorption zone and in the liquid before the deputy cation exchange resin column group in adsorption zone lysine concentration is made to be 1.0-2.0g/dL, the time contacted with Zeo-karb under the condition of not adjust pH is 17-20min, adding sulfuric acid adjust pH in transfer tank before the cation exchange resin column group being in position, end, adsorption zone is 1.8-2.0, be the time contacted with Zeo-karb under the condition of 1.8-2.0 at adjust pH be 8-10min, finally make from adsorption zone end position cation exchange resin column group lower end flow out liquid lysine concentration not higher than 0.1g/dL,
In back filled region, with elution fractions, temperature is 40-60 DEG C, with 2.0-4.0 times of column volume/hour flow velocity backfill cation exchange resin column, the consumption backfilling the elution fractions of every root cation exchange resin column is 0.4-0.6 times of column volume, the liquid flowed out from cation exchange resin column after backfill returns to adsorption zone, mixes containing lysine solution with described;
In Jian Dao district, make pH value be 11.0-12.5, temperature be 40-60 DEG C ammoniacal liquor with 4.0-8.0 times of column volume/hour flow velocity flow through cation exchange resin column, make the Methionin desorb be adsorbed onto on Zeo-karb obtain elutriant;
In breeding blanket, with temperature be 40-60 DEG C of water with 4.5-8.5 times of column volume/hour flow velocity flow through cation exchange resin column, the 0.35-0.65 that the consumption of the water that every root cation exchange resin column uses is column volume doubly, then make temperature be the air of 15-30 DEG C with the air pressure of 0.07-0.15MPa by cation exchange resin column, cation exchange resin column is regenerated.
Below the preferred embodiment of the present invention is described in detail by reference to the accompanying drawings; but; the present invention is not limited to the detail in above-mentioned embodiment; within the scope of technical conceive 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.
It should be noted that in addition, each concrete technical characteristic described in above-mentioned embodiment, in reconcilable situation, can be combined by any suitable mode, in order to avoid unnecessary repetition, the present invention illustrates no longer separately to various possible array mode.
In addition, also can carry out arbitrary combination between various different embodiment of the present invention, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Embodiment
The present invention is further illustrated for following embodiment, but therefore do not limit the present invention.
In following embodiment and comparative example:
The special strongly acidic cation-exchange of WD-2 type Methionin is sulfonic group strong-acid type cation exchange resin, is purchased from Chuzhou City Guan Dong Chemical Co., Ltd. of Anhui Province.
According to GB10794-89 standard detection lysine concentration (in lysine hydrochloride).
Embodiment 1
Adopt the technique shown in Fig. 2, make to contact containing lysine solution carry out ion exchange mechansim with cation exchange resin column group of organizing more, often organize cation exchange resin column group successively and cyclically through adsorption zone, back filled region, Jian Dao district and breeding blanket, to make cation exchange resin column group successively and cyclically to carry out exchange adsorption, purification and Adsorption and desorption and regeneration again, elutriant is obtained after desorb, wherein
Three groups of cation exchange resin column groups of connecting successively are in adsorption zone simultaneously, often organize cation exchange resin column group to be made up of 4 cation exchange resin columns in parallel, Zeo-karb in cation exchange resin column is the special strongly acidic cation-exchange of WD-2 type Methionin, the total exchange capacity of Zeo-karb is 8mmol/g, transfer tank is provided with between two adjacent groups cation exchange resin column group, two adjacent groups cation exchange resin column group is connected in series through transfer tank, concentration containing lysine solution is 13.0g/dL, temperature is 50 DEG C, introduce from the upper end of the cation exchange resin column group being in first place, adsorption zone, flow through each group of cation exchange resin column group in this adsorption zone successively, then flow out from the lower end of the cation exchange resin column group being in position, end, adsorption zone, and containing lysine solution under the condition of not adjust pH by being in the first and deputy cation exchange resin column group in adsorption zone, after the cation exchange resin column group of first place, adsorption zone and lysine concentration in the liquid before the deputy cation exchange resin column group in adsorption zone is 1.5g/dL, the time contacted with Zeo-karb under the condition of not adjust pH is 17min, adding sulfuric acid adjust pH in transfer tank before the cation exchange resin column group being in position, end, adsorption zone is 2.0, be the time contacted with Zeo-karb under the condition of 2.0 at adjust pH be 8.5min, result is 0.04g/dL from the lysine concentration the liquid that the lower end of the cation exchange resin column group of position, end, adsorption zone is flowed out,
In back filled region, every root cation exchange resin column elution fractions (0.525 times for column volume), temperature is 50 DEG C, with 3.5 times of column volumes/hour flow velocity backfill cation exchange resin column, the liquid flowed out from cation exchange resin column after backfill returns to adsorption zone, mixes containing lysine solution with described;
In Jian Dao district, make pH value be 11.5, temperature be 50 DEG C ammoniacal liquor with 6.0 times of column volumes/hour flow velocity flow through cation exchange resin column, make the Methionin desorb be adsorbed onto on Zeo-karb obtain elutriant;
In breeding blanket, every root cation exchange resin column temperature be 50 DEG C of water (0.45 times for column volume) with 6.0 times of column volumes/hour flow velocity flow through cation exchange resin column, then make temperature be the air of 20 DEG C with the air pressure of 0.12MPa by cation exchange resin column, cation exchange resin column is regenerated.
Embodiment 2
Adopt the technique shown in Fig. 2, make to contact containing lysine solution carry out ion exchange mechansim with cation exchange resin column group of organizing more, often organize cation exchange resin column group successively and cyclically through adsorption zone, back filled region, Jian Dao district and breeding blanket, to make cation exchange resin column group successively and cyclically to carry out exchange adsorption, purification and Adsorption and desorption and regeneration again, elutriant is obtained after desorb, wherein
Three groups of cation exchange resin column groups of connecting successively are in adsorption zone simultaneously, often organize cation exchange resin column group to be made up of 3 cation exchange resin columns in parallel, Zeo-karb in cation exchange resin column is the special strongly acidic cation-exchange of WD-2 type Methionin, the total exchange capacity of Zeo-karb is 8mmol/g, transfer tank is provided with between two adjacent groups cation exchange resin column group, two adjacent groups cation exchange resin column group is connected in series through transfer tank, concentration containing lysine solution is 10.0g/dL, temperature is 40 DEG C, introduce from the upper end of the cation exchange resin column group being in first place, adsorption zone, flow through each group of cation exchange resin column group in this adsorption zone successively, then flow out from the lower end of the cation exchange resin column group being in position, end, adsorption zone, and containing lysine solution under the condition of not adjust pH by being in the first and deputy cation exchange resin column group in adsorption zone, after the cation exchange resin column group of first place, adsorption zone and lysine concentration in the liquid before the deputy cation exchange resin column group in adsorption zone is 1.0g/dL, the time contacted with Zeo-karb under the condition of not adjust pH is 19min, adding sulfuric acid adjust pH in transfer tank before the cation exchange resin column group being in position, end, adsorption zone is 1.8, be the time contacted with Zeo-karb under the condition of 1.8 at adjust pH be 9.5min, result is 0.02g/dL from the lysine concentration the liquid that the lower end of the cation exchange resin column group of position, end, adsorption zone is flowed out,
In back filled region, every root cation exchange resin column elution fractions (0.5 times for column volume), temperature is 40 DEG C, with 3.0 times of column volumes/hour flow velocity backfill cation exchange resin column, the liquid flowed out from cation exchange resin column after backfill returns to adsorption zone, mixes containing lysine solution with described;
In Jian Dao district, make pH value be 11.0, temperature be 40 DEG C ammoniacal liquor with 4.8 times of column volumes/hour flow velocity flow through cation exchange resin column, make the Methionin desorb be adsorbed onto on Zeo-karb obtain elutriant;
In breeding blanket, every root cation exchange resin column temperature be 40 DEG C of water (0.375 times for column volume) with 4.5 times of column volumes/hour flow velocity flow through cation exchange resin column, then make temperature be the air of 15 DEG C with the air pressure of 0.15MPa by cation exchange resin column, cation exchange resin column is regenerated.
Embodiment 3
Adopt the technique shown in Fig. 2, make to contact containing lysine solution carry out ion exchange mechansim with cation exchange resin column group of organizing more, often organize cation exchange resin column group successively and cyclically through adsorption zone, back filled region, Jian Dao district and breeding blanket, to make cation exchange resin column group successively and cyclically to carry out exchange adsorption, purification and Adsorption and desorption and regeneration again, elutriant is obtained after desorb, wherein
Three groups of cation exchange resin column groups of connecting successively are in adsorption zone simultaneously, often organize cation exchange resin column group to be made up of 6 cation exchange resin columns in parallel, Zeo-karb in cation exchange resin column is the special strongly acidic cation-exchange of WD-2 type Methionin, the total exchange capacity of Zeo-karb is 8mmol/g, transfer tank is provided with between two adjacent groups cation exchange resin column group, two adjacent groups cation exchange resin column group is connected in series through transfer tank, concentration containing lysine solution is 15.0g/dL, temperature is 60 DEG C, introduce from the upper end of the cation exchange resin column group being in first place, adsorption zone, flow through each group of cation exchange resin column group in this adsorption zone successively, then flow out from the lower end of the cation exchange resin column group being in position, end, adsorption zone, and containing lysine solution under the condition of not adjust pH by being in the first and deputy cation exchange resin column group in adsorption zone, after the cation exchange resin column group of first place, adsorption zone and lysine concentration in the liquid before the deputy cation exchange resin column group in adsorption zone is 2.0g/dL, the time contacted with Zeo-karb under the condition of not adjust pH is 17min, adding sulfuric acid adjust pH in transfer tank before the cation exchange resin column group being in position, end, adsorption zone is 1.9, be the time contacted with Zeo-karb under the condition of 1.9 at adjust pH be 8.5min, result is 0.05g/dL from the lysine concentration the liquid that the lower end of the cation exchange resin column group of position, end, adsorption zone is flowed out,
In back filled region, every root cation exchange resin column elution fractions (0.6 times for column volume), temperature is 60 DEG C, with 4.0 times of column volumes/hour flow velocity backfill cation exchange resin column, the liquid flowed out from cation exchange resin column after backfill returns to adsorption zone, mixes containing lysine solution with described;
In Jian Dao district, make pH value be 12.5, temperature be 60 DEG C ammoniacal liquor with 5.5 times of column volumes/hour flow velocity flow through cation exchange resin column, make the Methionin desorb be adsorbed onto on Zeo-karb obtain elutriant;
In breeding blanket, every root cation exchange resin column temperature be 60 DEG C of water (0.5 times for column volume) with 6.5 times of column volumes/hour flow velocity flow through cation exchange resin column, then make temperature be the air of 30 DEG C with the air pressure of 0.07MPa by cation exchange resin column, cation exchange resin column is regenerated.
Comparative example 1
According to the method process of embodiment 1 containing lysine solution, unlike, in adsorption zone, containing lysine solution under the condition of not adjust pH successively by being in connect successively three groups of cation exchange resin column groups of adsorption zone; In breeding blanket, make air by after cation exchange resin column, the pH value to 1.0 of the liquid flowed out from the lower end of the cation exchange resin column group of position, end, adsorption zone is regulated with sulfuric acid, then with the liquid after adjust ph with 3 times of column volumes/hour flow velocity backfill cation exchange resin column, the consumption backfilling the liquid after the adjust ph of every root cation exchange resin column is 0.45 times of column volume, and the cation exchange resin column after backfill enters adsorption zone again and carries out next round to the process containing lysine solution.The content recording the Methionin the liquid flowed out from the lower end of the cation exchange resin column group of position, end, adsorption zone is 0.08g/dL.
As can be seen from embodiment 1 and comparative example 1, embodiment 1 is 0.04g/dL from the lysine concentration the liquid that the lower end of the cation exchange resin column group of position, end, adsorption zone is flowed out, comparative example 1 is 0.08g/dL from the content of the Methionin the liquid that the lower end of the cation exchange resin column group of position, end, adsorption zone is flowed out, and the treatment process containing lysine solution of the present invention improves the yield of Methionin as seen.
Treatment process containing lysine solution provided by the invention, improves the yield of Methionin; Provided by the invention often organize cation exchange resin column group successively and cyclically through adsorption zone, the method for Jian Dao district and breeding blanket, due to containing lysine solution in pH value be 1.0-2.0 condition under or be not less than 1.0g/dL at lysine concentration condition under by the cation exchange resin column group of position, end, adsorption zone, eliminate and adjust waste liquid pH value to be the step that 1.0-1.2 makes the transition to cation exchange resin column at breeding blanket sulfuric acid, when the cation exchange resin column group mode of connection of adsorption zone is identical, greatly save sulfuric acid dosage, reduce production cost.Treatment process containing lysine solution provided by the invention, can be widely used in industrial production.
Claims (18)
1. the treatment process containing lysine solution, described method comprises: make described containing lysine solution successively by cation exchange resin column group that one or more groups is connected successively, the liquid flowed out to make the end being adsorbed to the cation exchange resin column group of connecting successively from this one or more groups containing the Methionin in lysine solution, lysine concentration is not higher than 0.1g/dL, often organize the cation exchange resin column that cation exchange resin column group comprises one or more parallel connection, then basic solution is used to carry out wash-out to the cation exchange resin column after absorption Methionin, obtain the elutriant containing Methionin, it is characterized in that, described is by described cation exchange resin column group in pH value under the condition of 1.0-2.0 containing lysine solution.
2. method according to claim 1, wherein, described is by described cation exchange resin column group in pH value under the condition of 1.8-2.0 containing lysine solution.
3. method according to claim 1 and 2, wherein, described cation exchange resin column group is three groups, and often group comprises the cation exchange resin column of 3-6 parallel connection.
4. method according to claim 1, wherein, the Zeo-karb in described cation exchange resin column is sulfonic group strong-acid type cation exchange resin, and the total exchange capacity of described Zeo-karb is greater than 5mmol/g.
5. method according to claim 1, wherein, pH value regulates by adding sulfuric acid.
6. method according to claim 1, wherein, described basic solution is ammoniacal liquor, and pH value is 10.0-14.0.
7. method according to claim 6, wherein, described pH value is 11.0-12.5.
8. the treatment process containing lysine solution, it is characterized in that, described method comprises: make described contact containing lysine solution carry out ion exchange mechansim with cation exchange resin column group of organizing more, often organize cation exchange resin column group successively and cyclically through adsorption zone, Jian Dao district and breeding blanket, to make cation exchange resin column group successively and cyclically to carry out exchange adsorption, desorb and regeneration, elutriant is obtained after desorb, the described cation exchange resin column often organized cation exchange resin column group and comprise one or more parallel connection, wherein
One or more groups cation exchange resin column group of connecting successively is in adsorption zone simultaneously, the described lysine solution that contains is introduced from the upper end of the cation exchange resin column group being in first place, adsorption zone, be each group of cation exchange resin column group flowed through successively under the condition of 1.0-2.0 in this adsorption zone in pH value, then flow out from the lower end of the cation exchange resin column group being in position, end, adsorption zone, make described to be adsorbed onto on Zeo-karb containing at least part of Methionin in lysine solution, and make lysine concentration in the liquid of outflow not higher than 0.1g/dL; In Jian Dao district, make basic solution flow through described cation exchange resin column, make the Methionin desorb be adsorbed onto on Zeo-karb obtain described elutriant; In breeding blanket, water and air is made to pass through cation exchange resin column successively, cation exchange resin column is regenerated, wherein, transfer tank is provided with between the two adjacent groups cation exchange resin column group of adsorption zone, two adjacent groups cation exchange resin column group is connected in series through described transfer tank, the cation exchange resin column group being simultaneously in adsorption zone is three groups, often group comprises the cation exchange resin column of 3-6 parallel connection, and in the transfer tank before the cation exchange resin column group being in position, end, adsorption zone, adjust pH is 1.8-2.0.
9. method according to claim 8, wherein, the described lysine solution that contains is introduced from the upper end of the cation exchange resin column group being in first place, adsorption zone, be each group of cation exchange resin column group flowed through successively under the condition of 1.8-2.0 in this adsorption zone in pH value, then flow out from the lower end of the cation exchange resin column group being in position, end, adsorption zone.
10. method according to claim 8, wherein, described containing lysine solution under the condition of not adjust pH by being in the first and deputy cation exchange resin column group in adsorption zone, making after the cation exchange resin column group of first place, adsorption zone and in the liquid before the deputy cation exchange resin column group in adsorption zone lysine concentration be 1.0-2.0g/dL, is by being in the cation exchange resin column group of position, end, adsorption zone in pH value under the condition of 1.8-2.0.
11. methods according to claim 8, wherein, the condition of described absorption comprises, temperature is 40-60 DEG C, the time contacted with Zeo-karb under the condition of not adjust pH containing lysine solution is 17-20min, be the time contacted with Zeo-karb under the condition of 1.0-2.0 is 8-10min at adjust pH; The condition of described desorb comprises, the flow velocity of described basic solution be 4.0-8.0 times of column volume/hour, temperature is 40-60 DEG C; The condition of described regeneration comprises, the flow velocity of described water be 4.5-8.5 times of column volume/hour, temperature is 40-60 DEG C, and the air pressure of described air is 0.07-0.15MPa, and temperature is 15-30 DEG C.
12. methods according to claim 8, wherein, described method also comprises described cation exchange resin column after adsorption zone, before Jian Dao district, also through back filled region, in back filled region, backfill described cation exchange resin column with the described elutriant of part, make described cation exchange resin column carry out purification and again adsorb.
13. methods according to claim 12, wherein, the liquid flowed out from described cation exchange resin column after backfill returns to adsorption zone, mixes containing lysine solution with described.
14. methods according to claim 12 or 13, wherein, described purification and the condition of again adsorbing comprise, the flow velocity of the described elutriant of described part be 2.0-4.0 times of column volume/hour, temperature is 40-60 DEG C.
15. methods according to claim 8, wherein, the Zeo-karb in described cation exchange resin column is sulfonic group strong-acid type cation exchange resin, and the total exchange capacity of described Zeo-karb is greater than 5mmol/g.
16. methods according to claim 8, wherein, pH value regulates by adding sulfuric acid.
17. methods according to claim 8, wherein, described basic solution is ammoniacal liquor, and pH value is 10.0-14.0.
18. methods according to claim 17, wherein, described pH value is 11.0-12.5.
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Citations (4)
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 |
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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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