CN103739508B - Extraction technology of 98.5% lysine hydrochloride - Google Patents
Extraction technology of 98.5% lysine hydrochloride Download PDFInfo
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- CN103739508B CN103739508B CN201410024471.6A CN201410024471A CN103739508B CN 103739508 B CN103739508 B CN 103739508B CN 201410024471 A CN201410024471 A CN 201410024471A CN 103739508 B CN103739508 B CN 103739508B
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention belongs to the technical field of lysine production, and particularly relates to an extraction technology of 98.5% lysine hydrochloride. The extraction technology of 98.5% lysine hydrochloride comprises the following steps: (1) ceramic membrane separation; (2) continuous ion exchange; (3) acid concentration; (4) crystallization; (5) baking, namely baking wet crystals obtained in the step (4) through a dryer until the moisture content is smaller than or equal to 1.5%, then removing small particles in a multi-stage swinging screening manner, re-dissolving excessive overtails and siftage and then returning to the step (4) to crystallize. The technology is reasonable in design, and the extracted 98.5% lysine hydrochloride is regular in crystal shape, uniform in size and strong in compressive capacity.
Description
Technical field
The invention belongs to the technical field that Methionin is produced, be specifically related to a kind of extraction process of 98.5% lysine hydrochloride.
Background technology
Methionin is that eight kinds of primary amino acids of needed by human are (also known as indispensable amino acid, one of they are Methionin, Threonine, leucine, Isoleucine, methionine(Met), α-amino-isovaleric acid, phenylalanine and tryptophane), because health oneself can not produce it, it must be obtained by diet and nutritional supplement.As a seed amino acid, it is the requisite integral part of protein, as everyone knows, protein is the major ingredient forming human body cell, through digesting first breaks down into amino acids after protein in food enters human body, then human body utilize again the new human body protein of these amino acid resynthesis (as immune antibody, digestive ferment, plasma proteins, tethelin etc. be all synthesis after human body protein).In each seed amino acid of synthetic protein, 1B is most important one, has lacked it, and other amino acid is just restricted or is not used, and scientist claims it to be human body first indispensable amino acid.
1B, clear crystal, fusing point 224.5 DEG C (decomposition), is slightly soluble in ethanol, is insoluble to ether.Methionin is at water
In solubleness very large, and easily absorb the carbonic acid gas in air, be difficult to obtain its crystallization, therefore as commodity, it often occurs with the form of mono-hydrochloric salts or vitriol, and outward appearance is light brown particle, because containing two amino in molecule, a carboxyl, in alkalescence, belongs to basic aminoacids.
1B tool has been widely used, and such as food aspect can be used as food enrichment, food reodorant; Medicine
Aspect can be used as the ancillary drug of diuretic(s), and treat the lead poisoning phenomenon caused because muriate in blood reduces, also can generate salt with acidic drug (as Whitfield's ointment etc.) alleviates untoward reaction, share with methionine(Met), and severe hypertension can be suppressed sick; Feed aspect is current, and the 1B product of more than 90% is used for fodder industry, the effect that as added appropriate Methionin in feed, can meet animal needs, promoting growth of animal, improve amino acid balance, improve efficiency of feed utilization, save protein resource.
Existing 98.5% lysine hydrochloride extraction process adopts traditional Plate Filtration, filtered liquid is of poor quality, only adopt filter cloth and super-cell, even if adopt multiple filtering technology, the suspension solid substance in material and soluble proteins can not be removed completely, and these suspension solid substances and soluble proteins are once dialysis, can make follow-up from skill process result degrades of handing over, the whole production cycle shortens, reason is that these suspension solid substances and soluble proteins wrap up ion exchange resin surface, do not have real exchange interaction, not only affect production efficiency, and in regenerative process, need a large amount of washing water to rinse, add the consumption of water and regenerator.Traditional sheet frame execute-in-place environment adopts open design, the possibility of material crossed contamination is very big, the external world is easy to bring foreign material into and enters in material with other foreign matters, affect quality product, moreover owing to adopting open structure, execute-in-place environment is dirty, and steam rising phenomenon in operating space is serious, affects the healthy of operator; General conventional film filtration process, core component filtering membrane tube, by affected by high, is easy to damage, causes material thoroughly to filter, affect quality product; And general conventional film filtration process is short for cycling time, and cycles of concentration is on the low side, and integral membrane flux is little.
Traditional extraction technique adopts continuous evaporative crystallization, adopts recycle pump pump circulation stimulating method, although control certain degree of supersaturation, but because the Different Size Fractions in forceful motion is subject to mutual collision, friction, generate plane of crystal crystal formation coarse, out-of-shape, pseudo-brilliant and cluster crystal quantity is many, particle is tiny, make crystal and mother liquor separation difficulty, during washing, dissolution of crystals amount is also large, and crystal loss is serious, follow-up moisture dries difficulty, and product easily lumps.
Traditional evaporation technology adopts following current evaporation, concentrated, does not have primary heater unit, steam and heat utilization ratio low, use of flash steam weak effect, refrigeration cycle water consumption is large, and evaporation performance falls behind.
The screening that traditional extraction technique adopts requires not tight, and the uneven granularity of size is mingled with mutually, and product is easy to caking.
Summary of the invention
The object of the invention is to the defect for above-mentioned existence and provide a kind of extraction process of 98.5% lysine hydrochloride, this technological design is reasonable, extracts 98.5% Lysine hydrochloride crystal regular shape of gained, and size is even, and anti-pressure ability is strong.
Technical scheme of the present invention is: a kind of extraction process of 98.5% lysine hydrochloride, comprises the following steps:
(1) ceramic membrane separation: first the lysine fermentation liquor of gained is placed in fermented liquid storage tank, then by stage pump, lysine fermentation liquor is pumped into ceramic film component by storage tank, the dialyzate of gained is placed in membrane filtration flow container, and gained trapped substance is placed in film concentrated phase tank;
(2) continuous ionic exchanges: the membrane filtration liquid in step (1) membrane filtration flow container is injected ISEP continuous ionic exchange system, adsorb and resolve, finally obtain new elutriant to Methionin ion;
(3) acid is concentrated: by the elutriant of step (2) gained first through deammoniation tower deamination, then evaporate through quadruple effect evaporator, triple-effect evaporator, 1st effective evaporator and 2nd effect evaporator successively, improve the concentration of Methionin, finally obtained liquid and be placed in liquid bath;
(4) crystallization: the liquid that completes of step (3) gained is neutralized into lysine hydrochloric acid salts solution with hydrochloric acid in neutralization bucket, this solution is placed in crystallization cylinder and lowers the temperature crystallization, is separated obtains wet crystal and mother liquor through centrifuge; Mother liquor low-temperature evaporation crystallization in mother liquor crystallization device after concentrated, then delivers to neutralization bucket through the isolated wet crystal material of mother liquor whizzer, is separated the secondary mother liquid obtained and delivers to ISEP continuous ionic exchange system;
(5) dry: the wet crystallization of step (4) gained is less than or equal to 1.5% by drying machine drying to water content, then waves screening through multistage, remove small-particle; Step (4) crystallization is returned after unnecessary sieve dissolves again with screen underflow.
The pH value of the lysine fermentation liquor in described step (1) controls 3.6 ~ 4.1, and temperature controls at 65 ~ 70 DEG C; The one-level mould difference of described ceramic film component is 1.6bar, and secondary membrane pressure reduction is 2.4bar.
ISEP continuous ionic exchange system in described step (2) comprises decolouring section, Yu Xi district, adsorption zone, wash-out back filled region, Jian Dao district, breeding blanket and protective belt; Membrane filtration liquid is injected decolorizer, ion exchange column as upper prop liquid, is rotated ion exchange column to adsorption zone, adsorb Methionin ion by fixing rotating disk, the waste liquid that fractionation by adsorption is got off gets rid of cylinder; Adsorb saturated cylinder by fixing rotating disk, ion exchange column to be rotated to wash-out back filled region, by the waste water in elutriant backfill extrusion cylinder and impurity; Cylinder after wash-out backfill rotates into Jian Dao district, and resolve through ammonia neutralization and by Methionin ion and obtain new elutriant and be placed in wash-out flow container through protective belt purifying, ion exchange column becomes actifier column; Actifier column rotates to breeding blanket, after dilute sulphuric acid makes the transition, reach optimal adsorption ability.
Described fixing rotating disk is fixed with at least three ion exchange columns.
It is 580 ~ 700m that upper fluid injection in described step (2) controls flow
3/ h, temperature is 48 ~ 52 DEG C, and pH value is 3 ~ 4.2; Waste liquid controls flow for being more than or equal to 32 m
3/ h, temperature is 48 ~ 54 DEG C, and pH value is 1.0 ~ 1.2.
Quadruple effect evaporator, triple-effect evaporator, 1st effective evaporator and 2nd effect evaporator in described step (3) are thin-film evaporator.
Be equipped with sparger in quadruple effect evaporator, triple-effect evaporator, 1st effective evaporator and 2nd effect evaporator in described step (3), vapor pressure all controls at 0.3 ~ 0.4MPa, and the effect temperature wherein in 1st effective evaporator controls at 82 ~ 88 DEG C.
Completing liquid-tight degree in described step (3) is 1050 ~ 1100kg/m
3.
PH value in neutralization bucket in described step (4) controls 4.6 ~ 4.8.
Temperature in described step (4) in mother liquor crystallization device controls at 38 ~ 55 DEG C, and vacuum degree control is at-0.99 ~-0.90bar.
Beneficial effect of the present invention is: the pH value of lysine fermentation liquor controlled 3.6 ~ 4.1, microorganism finally to be lost activity by the extraction process of 98.5% lysine hydrochloride of the present invention before ceramic membrane separation, produces acid and stagnates.For ensureing enough membrane fluxs, adopting the multistage pressure reduction of ceramic film component to control and classified filtering technique, farthest utilizing film thoroughly to filter usefulness, ensure the clarity of filtrate simultaneously, and traditional Plate Filtration, filtered liquid is of poor quality, and execute-in-place environment is dirty; Conventional film filtration process, filtering membrane tube is by affected by high, and be easy to damage, cycling time is short, and membrane flux is low.
The present invention adopts the fixed-bed process ratio of ISEP continuous ionic exchange system and routine, and resin demand is only 30% of fixed bed, and the decline 85% of water consumption, acid and alkali consumption is only 40% of fixed bed.Because adopting rotating circulating design, whole simulation moving-bed utilization ratio strengthens greatly, and whole production cost reduces nearly 30%.Yield improves 5 ~ 8%.The heavy metal content of products obtained therefrom is less than < 3ppm.For fully ensureing the adsorption effect of ion exchange resin to zwitterion, before ion-exchange, designing decolouring system, fully ensureing the operating capacity of resin, and adding Yu Xi district and protective belt, guaranteeing that feed liquid quality control is in normal range.
Traditional technique adopts continuous evaporative crystallization, the plane of crystal crystal formation produced is coarse, irregular, puppet is brilliant and cluster crystal is many, moisture dries difficulty, product easily lumps and size distribution is irregular, and the present invention adopts cross-flow evaporation, elevating membrane circulation, board-like preheating, secondary steam to recycle, evaporation performance is higher by more than 30% than traditional mode evaporation, and steam consumption reduces by 40%, the plane of crystal of described explained hereafter is bright and clean, regular shape, size is even, and crystal anti-pressure ability is strong, moisture is dried easily, and product is not easy caking.
Technique employing of the present invention is multistage waves screening, removes small-particle, effectively controls product caking, return front road art breading after unnecessary sieve dissolves again with screen underflow, and traditional technology classification is thin, granularity size is uneven, be mingled with mutually, caking phenomenon is obvious.
Embodiment
Below by specific embodiment, the present invention will be described in detail.
An extraction process for 98.5% lysine hydrochloride, comprises the following steps:
(1) ceramic membrane separation: first the lysine fermentation liquor of gained is placed in fermented liquid storage tank, control the pH value of lysine fermentation liquor 3.6 ~ 4.1, temperature controls at 65 ~ 70 DEG C; Then by stage pump, lysine fermentation liquor is successively pumped into ceramic film component to the multistage distribution of suspension by storage tank by clear liquid, the one-level mould difference of ceramic film component is 1.6bar, secondary membrane pressure reduction is 2.4bar, the dialyzate of gained is placed in membrane filtration flow container, and gained trapped substance is placed in film concentrated phase tank;
(2) continuous ionic exchanges: the membrane filtration liquid in step (1) membrane filtration flow container is injected ISEP continuous ionic exchange system, to relying
Propylhomoserin ion carries out adsorbing and resolving, and finally obtains new elutriant; ISEP continuous ionic in described step (2) exchanges system
Turnkey draws together decolouring section, Yu Xi district, adsorption zone, wash-out back filled region, Jian Dao district, breeding blanket and protective belt; Membrane filtration liquid is injected decolorizer, ion exchange column as upper prop liquid, and in control, fluid injection flow is 580 ~ 700m
3/ h, temperature is 48 ~ 52 DEG C, and pH value is 3 ~ 4.2; Rotated ion exchange column to Yu Xi district and adsorption zone by fixing rotating disk, adsorb Methionin ion, the waste liquid that fractionation by adsorption is got off gets rid of cylinder, controls waste liquid flow for being more than or equal to 32 m
3/ h, temperature is 48 ~ 54 DEG C, and pH value is 1.0 ~ 1.2; Adsorb saturated cylinder by fixing rotating disk, ion exchange column to be rotated to wash-out back filled region, by the waste water in elutriant backfill extrusion cylinder and impurity; Cylinder after wash-out backfill rotates into Jian Dao district, to resolve to obtain new elutriant after the purifying of protective belt and be placed in elutriant tank through ammonia neutralization and by Methionin ion, and ion exchange column becomes actifier column; Actifier column rotates to breeding blanket and protective belt, after dilute sulphuric acid makes the transition, reach optimal adsorption ability.Described fixing rotating disk is fixed with at least three ion exchange columns.
(3) acid is concentrated: by the elutriant of step (2) gained first through deammoniation tower deamination, then cross-flow evaporation is carried out through quadruple effect evaporator, triple-effect evaporator, 1st effective evaporator and 2nd effect evaporator successively, combine simultaneously and adopt elevating membrane circulation, board-like preheating and secondary steam to recycle, improve the concentration of Methionin, finally obtained liquid and be placed in liquid bath; Described quadruple effect evaporator, triple-effect evaporator, 1st effective evaporator and 2nd effect evaporator are thin-film evaporator.Sparger is equipped with in quadruple effect evaporator, triple-effect evaporator, 1st effective evaporator and 2nd effect evaporator, the liquid that completes after deamination is assigned to uniformly in vaporizer tubulation after sparger, complete liquid under gravity, form membranaceous top-down flowing, film and tubulation outer wall steam generation thermal exchange simultaneously, the moisture in liquid has been made to be subject to thermal evaporation, to improve the concentration of Methionin, vapor pressure all controls at 0.3 ~ 0.4MPa, and the effect temperature wherein in 1st effective evaporator controls at 82 ~ 88 DEG C.
(4) crystallization: the liquid that completes of step (3) gained is neutralized into lysine hydrochloric acid salts solution with hydrochloric acid in neutralization bucket, this solution is placed in crystallization cylinder and lowers the temperature crystallization, is separated obtains wet crystal and mother liquor through centrifuge; Mother liquor low-temperature evaporation crystallization in mother liquor crystallization device after concentrated, then delivers to neutralization bucket through the isolated wet crystal material of mother liquor whizzer, is separated the secondary mother liquid obtained and delivers to ISEP continuous ionic exchange system.Temperature in described mother liquor crystallization device controls at 38 ~ 55 DEG C, and vacuum tightness all controls at-0.99 ~-0.90bar.
(5) dry: the wet crystallization of step (4) gained is less than or equal to 1.5% by drying machine drying to water content, then waves screening through multistage, remove small-particle, effectively control product caking.Front road art breading is returned after unnecessary sieve dissolves again with screen underflow.
Completing liquid-tight degree in described step (3) is 1050 ~ 1100kg/m
3.
Temperature in described step (4) in mother liquor crystallization device controls at 38 ~ 55 DEG C, and vacuum tightness all controls at-0.99 ~-0.90bar.
Claims (9)
1. an extraction process for 98.5% lysine hydrochloride, comprises the following steps:
(1) ceramic membrane separation: first the lysine fermentation liquor of gained is placed in fermented liquid storage tank, then by stage pump, lysine fermentation liquor is pumped into ceramic film component by storage tank, the dialyzate of gained is placed in membrane filtration flow container, and gained trapped substance is placed in film concentrated phase tank;
(2) continuous ionic exchanges: the membrane filtration liquid in step (1) membrane filtration flow container is injected ISEP continuous ionic exchange system, adsorb and resolve, finally obtain new elutriant to Methionin ion; Wherein said ISEP continuous ionic exchange system comprises decolouring section, Yu Xi district, adsorption zone, wash-out back filled region, Jian Dao district, breeding blanket and protective belt; Membrane filtration liquid is injected decolorizer, ion exchange column as upper prop liquid, is rotated ion exchange column to adsorption zone, adsorb Methionin ion by fixing rotating disk, the waste liquid that fractionation by adsorption is got off gets rid of cylinder; Adsorb saturated cylinder by fixing rotating disk, ion exchange column to be rotated to wash-out back filled region, by the waste water in elutriant backfill extrusion cylinder and impurity; Cylinder after wash-out backfill rotates into Jian Dao district, and resolve through ammonia neutralization and by Methionin ion and obtain new elutriant and be further purified through guard column and be placed in elutriant tank, ion exchange column becomes actifier column; Actifier column rotates to breeding blanket, after dilute sulphuric acid makes the transition, reach optimal adsorption ability;
(3) acid is concentrated: by the elutriant of step (2) gained first through deammoniation tower deamination, then cross-flow evaporation is carried out through quadruple effect evaporator, triple-effect evaporator, 1st effective evaporator and 2nd effect evaporator successively, improve the concentration of Methionin, finally obtained liquid and be placed in liquid bath;
(4) crystallization: the liquid that completes of step (3) gained is neutralized into lysine hydrochloric acid salts solution with hydrochloric acid in neutralization bucket, this solution is placed in crystallization cylinder and lowers the temperature crystallization, is separated obtains wet crystal and mother liquor through centrifuge; Mother liquor low-temperature evaporation crystallization in mother liquor crystallization device after concentrated, then delivers to neutralization bucket through the isolated wet crystal material of mother liquor whizzer, is separated the secondary mother liquid obtained and delivers to ISEP continuous ionic exchange system;
(5) dry: the wet crystallization of step (4) gained is less than or equal to 1.5% by drying machine drying to water content, then waves screening through multistage, remove small-particle; Step (4) crystallization is returned after unnecessary sieve dissolves again with screen underflow.
2. the extraction process of 98.5% lysine hydrochloride according to claim 1, is characterized in that, the pH value of the lysine fermentation liquor in described step (1) controls 3.6 ~ 4.1, and temperature controls at 65 ~ 70 DEG C; The one-level mould difference of described ceramic film component is 1.6bar, and secondary membrane pressure reduction is 2.4bar.
3. the extraction process of 98.5% lysine hydrochloride according to claim 1, is characterized in that, described fixing rotating disk is fixed with at least three ion exchange columns.
4. the extraction process of 98.5% lysine hydrochloride according to claim 1, is characterized in that, the upper prop hydraulic control flow in described step (2) is 580 ~ 700m
3/ h, temperature is 48 ~ 52 DEG C, and pH value is 3.0 ~ 4.2; Waste liquid controls flow for being more than or equal to 32 m
3/ h, temperature is 48 ~ 54 DEG C, and pH value is 1.0 ~ 1.2.
5. the extraction process of 98.5% lysine hydrochloride according to claim 1, is characterized in that, quadruple effect evaporator, triple-effect evaporator, 1st effective evaporator and 2nd effect evaporator in described step (3) are thin-film evaporator.
6. the extraction process of 98.5% lysine hydrochloride according to claim 1, it is characterized in that, sparger is equipped with in quadruple effect evaporator, triple-effect evaporator, 1st effective evaporator and 2nd effect evaporator in described step (3), vapor pressure all controls at 0.3 ~ 0.4MPa, and the effect temperature wherein in 1st effective evaporator controls at 82 ~ 88 DEG C.
7. the extraction process of 98.5% lysine hydrochloride according to claim 1, is characterized in that, completing liquid-tight degree in described step (3) is 1050 ~ 1100kg/m
3.
8. the extraction process of 98.5% lysine hydrochloride according to claim 1, is characterized in that, the pH value in the neutralization bucket in described step (4) controls 4.6 ~ 4.8.
9. the extraction process of 98.5% lysine hydrochloride according to claim 1, is characterized in that, the temperature in described step (4) in mother liquor crystallization device controls at 38 ~ 55 DEG C, and vacuum degree control is at-0.99 ~-0.90bar.
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| CN104163766B (en) * | 2014-07-29 | 2015-09-02 | 中粮生物化学（安徽）股份有限公司 | A kind of method preparing Lysine hydrochloride crystal |
| CN108084042A (en) * | 2017-12-23 | 2018-05-29 | 安徽名创新材料科技有限公司 | A kind of ceramic membrane separation purifies the method for lysine fermentation liquor |
| CN110590586B (en) * | 2019-09-16 | 2021-09-24 | 安徽丰原生物技术股份有限公司 | Method for separating and purifying lysine fermentation liquor |
| CN114181388B (en) * | 2021-11-30 | 2023-12-01 | 河北圣雪大成制药有限责任公司 | Method for extracting polylysine from fermentation liquor |
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Denomination of invention: A Extraction Process for 98.5% Lysine Hydrochloride Effective date of registration: 20230831 Granted publication date: 20150715 Pledgee: Shandong Zhucheng rural commercial bank Limited by Share Ltd. Pledgor: ZHUCHENG DONGXIAO BIOTECHNOLOGY Co.,Ltd. Registration number: Y2023980054774 |
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Address after: 262218 Xinxing Town, Zhucheng City, Weifang City, Shandong Province Patentee after: Dongxiao Biotechnology Co.,Ltd. Address before: 262218 Xinxing Town, Zhucheng City, Weifang City, Shandong Province Patentee before: ZHUCHENG DONGXIAO BIOTECHNOLOGY Co.,Ltd. |