CN105503630A - Method for purifying lysine hydrochloride - Google Patents
Method for purifying lysine hydrochloride Download PDFInfo
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- CN105503630A CN105503630A CN201510896726.2A CN201510896726A CN105503630A CN 105503630 A CN105503630 A CN 105503630A CN 201510896726 A CN201510896726 A CN 201510896726A CN 105503630 A CN105503630 A CN 105503630A
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
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Abstract
The invention relates to a method for extracting lysine hydrochloride from lysine hydrochloride fermenting liquid. The method comprises the following steps: filtering the lysine hydrochloride fermenting liquid by a microporous ceramic membrane to obtain micro-filtrate and a membrane dense phase; decoloring the micro-filtrate by activated carbon to obtain decolored liquid; carrying vacuum concentration, acid regulation and cooling crystallization on the decolored liquid to obtain wet crystal and crystallized mother liquor; carrying out further centrifugal drying on the wet crystal to obtain lysine hydrochloride crystal; merging the membrane dense phase and the crystallized mother liquor, and carrying out vacuum concentration and spray drying on the obtained mixed liquid to obtain the lysine hydrochloride with the content of more than 65%. After the method is used for extracting the lysine hydrochloride, the extraction rate is high, and the high-purity lysine hydrochloride can be prepared; furthermore, the extraction technology is simple in operation and environment-friendly.
Description
Technical field
The present invention relates to lysine hydrochloride and extract field, specifically provide a kind of method extracting lysine hydrochloride from lysine hydrochloride fermented liquid.
Background technology
Methionin is synthesis cranial nerve, biomass cells nucleoprotein and the indispensable composition of oxyphorase, is that animal self can not be synthesized, one of the amino acid that must absorb from food, and nutritionist is classified as it " the first lack amino acid "." first limiting amino acid " of vegetable protein.Lysine hydrochloride, chemistry 2,6-hydrochloride diaminocaproate by name, molecular formula is: C
6h
14n
2o
2hCL.
Methionin function in vivo has: participate in body protein as the synthesis of skeletal muscle, enzyme and polypeptide hormone; Be one of ketogenic amino acid, when lacking available carbohydrate, it participates in the metabolism generating ketoboidies and glucose; Maintain acid base equilibrium in body; As the precursor of synthesis carnitine, participate in metabolism of fat; In addition Methionin can also improve body opposing stress ability.
Along with the development of science and technology and people are to more understandings of healthcare knowledge, people have recognized the importance of Methionin in people's life, and the demand in Methionin market is also increasing.The development in market has made Methionin move towards field of food health care and field of medicaments from field of animal feed.The lysine hydrochloric acid product salt annual production of the current world reaches 1,000,000 tons, and wherein about 90% be used as fodder additives, 10% for food and medicine intermediate.Therefore it is very important for increasing value-added content of product.
Though the production of Methionin is flourish both at home and abroad at present, the lysine salt product that market is sold is mainly lysine hydrochloride crystal and purity is the lysine sulfate of about 65%.Wherein, high purity lysine hydrochloride mainly adopts resin adsorption method to purify and obtains, but in purification process, there are some defects: the Metastable zone of example hydrochloric acid Methionin crystallization is narrower; Lysine hydrochloride is because of the large not easily crystallization of solvability in aqueous, and easily lumps in high temperature environments; Purification process energy consumption is high; Mother liquor direct discharge-ring environment pollution is large.
Given this, special proposition the present invention.
Summary of the invention
The present invention aims to provide a kind of method of purification of lysine hydrochloride of easy, efficient, environmental protection.Adopt method of purification of the present invention, improve further purity and the yield of lysine hydrochloride, solve the technological difficulties of lysine hydrochloride not easily crystallization in aqueous; Lysine hydrochloride in film concentrated phase and crystalline mother solution is fully extracted simultaneously, effectively promote the utility value of lysine hydrochloride fermented liquid, and avoid crystalline mother solution and directly discharge brought problem of environmental pollution.
To achieve these goals, the present invention adopts following technical scheme:
A method of purification for lysine hydrochloride, comprises following steps:
Step (1): adopt microporous membrane to filter lysine hydrochloride fermented liquid, obtain micro-filtrate and film concentrated phase;
Step (2): adopt gac to decolour described micro-filtrate, obtain destainer;
Step (3): by gained destainer through vacuum concentration, acid adjustment, decrease temperature crystalline, obtains wet crystal and crystalline mother solution; The further centrifugal oven dry of wherein said wet crystal, obtains lysine hydrochloride crystal;
Step (4): step (1) gained film concentrated phase and step (3) gained crystalline mother solution are merged, gained mixed solution, through vacuum concentration, spraying dry, obtains the lysine hydrochloride of content more than 65%.
In method of purification of the present invention, in step (1), described microporous membrane intake pressure is 0.2 ~ 0.3MPa, and inlet and outlet pressure difference is 0.05MPa; Described membrane flux is 50 ~ 70LMH; The aperture of described microporous membrane is 0.05 μm ~ 0.1 μm; Fermented liquid cycles of concentration is 5-7 times; Water-dialyzing addition is 30% ~ 35% (v/v) of fermented liquid charging cumulative volume; In this step, the yield of lysine hydrochloride reaches more than 96%.By the suitable selection to micropore ceramics membrane pore size, to the conservative control of microporous membrane inlet and outlet pressure and membrane flux, effectively can remove the impurity in fermented liquid and thalline, be beneficial to the operation of subsequent purification process, complete the filtration of lysine hydrochloride fermented liquid fast; And effectively avoid the excessive film distortion brought of film pressurized.In addition, the film concentrated phase after filtration can add water-dialyzing, carries out repeatedly micropore ceramics membrane filtration, thus improves filter effect.
In method of purification of the present invention, in step (2), described gac addition is 0.001 ~ 0.002g/mL micro-filtrate; Bleaching temperature is 60 ~ 70 DEG C, and the time is 30 ~ 60min, and the yield of lysine hydrochloride reaches more than 98%.The selection of discoloring agent and the control of decolorization condition can make micro-filtrate reach higher decolorizing efficiency and decolorizing effect.
In method of purification of the present invention, in step (3), described vacuum concentration condition is: vacuum tightness is-0.08 ~-0.09MPa, and temperature is 60 ~ 70 DEG C.
In method of purification of the present invention, in step (3), be that acid adjustment to pH value are 4.0 ~ 5.0 after 70 ~ 75% by destainer vacuum concentration to solid content.Acid adjustment process can adopt the conventional acid solution in this areas such as concentrated hydrochloric acid.
In method of purification of the present invention, in step (3), described decrease temperature crystalline concrete operation step is: be first cooled to 55 DEG C, 1 ~ 10% throws in lysine hydrochloride crystal seed by mass percentage, after growing the grain 2 ~ 4h, is down to 45 DEG C with the speed of 1 DEG C/h; Then 15 DEG C are down to the speed of 3 DEG C/h.Gained magma is separated by whizzer, with absolute ethanol washing, utilizes efficient ebullated bed in 50-60 DEG C of oven dry, obtain white needles, the lysine hydrochloride crystal of content >98.5%.In this process, by the control to rearing crystal time and cooling rate, the Metastable zone that can solve lysine hydrochloric acid salt-pepper noise is narrower, concentration there will be solidification too greatly, the too little technological difficulties generated without crystal of concentration, thus obtain the crystal of high-quality, improve crystallization yield.
In method of purification of the present invention, in step (4), described vacuum concentration condition is: vacuum tightness is at-0.08Mpa ~-0.09Mpa, and thickening temperature is 65 ~ 70 DEG C; Being concentrated into solid content is 30% ~ 40%, then carries out spraying dry, obtains low-purity lysine hydrochloride.
As one of preferred embodiment of the present invention, in described lysine hydrochloride fermented liquid, solid content is 22 ~ 25%, and pH value is 6.7 ~ 6.9, lysine hydrochloride content 15 ~ 20g/100mL.Prove that technical scheme of the present invention has better refining effect for the lysine hydrochloride under above-mentioned condition by experiment.In addition in method of purification of the present invention, be first heated to 80 DEG C after preferably lysine hydrochloride fermented liquid being put tank, insulation 10min, to realize better bacteria-eliminating efficacy.
The present invention adopts advanced membrane separation process to instead of conventional resins absorption method to prepare Methionin technique, and by the concrete optimization to membrane separation process condition, the purity of further raising lysine hydrochloride and yield, solve the technological difficulties of lysine hydrochloride not easily crystallization in aqueous; Lysine hydrochloride in film concentrated phase and crystalline mother solution is fully extracted simultaneously, effectively promote the utility value of lysine hydrochloride fermented liquid, and avoid crystalline mother solution and directly discharge brought problem of environmental pollution.The extraction yield of the total lysine hydrochloride of gained of the present invention can up to more than 98%.
Embodiment
Embodiment for illustration of the present invention, but is not used for limiting the scope of the invention.
Concentration of the present invention is mass concentration, and solid content is mass content.
Lysine hydrochloride fermented liquid of the present invention is from Anhui Feng Yuan fermentation technique Engineering Co., Ltd.
Embodiment 1
The invention provides a kind of method extracting lysine hydrochloride from lysine hydrochloride fermented liquid, specifically comprise following steps:
Step (1): get lysine hydrochloride fermented liquid, wherein solid content is 22%, and pH value is 6.8, lysine hydrochloride content 15g/100mL.Adopt microporous membrane to filter described lysine hydrochloride fermented liquid, obtain micro-filtrate and film concentrated phase;
Described ceramic membrane aperture is 0.05 μm; Described microporous membrane intake pressure is 0.2MPa, and top hole pressure is 0.1MPa, and membrane flux is 50LMH.
Step (2): adopt Powdered Activated Carbon to decolour described micro-filtrate, obtain destainer; Described gac addition is the 0.001g/mL of micro-filtrate, and desolventing technology temperature is 60 DEG C, and the time is 30min.
Step (3): by dense for above-mentioned destainer vacuum concn, vacuum tightness is-0.08MPa, and temperature is 60 DEG C, and vacuum concentration is 70% to solid content, obtains concentrated solution.By above-mentioned concentrated solution adjust ph to 4.0.Above-mentioned concentrated solution is cooled to 50 DEG C, in concentrated solution, adds the lysine hydrochloride crystal seed of 1% (m/m), after growing the grain 2h, be down to 40 DEG C with the rate of temperature fall of 1 DEG C/h; Then be down to 10 DEG C with the rate of temperature fall of 3 DEG C/h, obtain magma.By described magma centrifugation, the wet crystal after centrifugal is washed with water, then with efficient ebullated bed 50 DEG C oven dry, obtain lysine hydrochloride crystal.
Step (4): step (1) gained film concentrated phase and step (3) gained crystalline mother solution are merged final vacuum and concentrate, vacuum tightness is at-0.08MPa, thickening temperature is 65 DEG C, vacuum concentration, to solid content 30% (m/m) spraying dry afterwards, obtains lysine hydrochloride mixture.
Wherein, in the present embodiment step (1), concentrated 5.9 times of lysine hydrochloride fermented liquid, concentrated phase lysine content 4.47g/100mL, solid content 13.3%.Cycles of concentration refers to the ratio of feed liquid and the concentrated phase after terminating except clearly mutually altogether entering ceramic membrane.
In the present embodiment step (3), gained lysine hydrochloride crystalline content 98.8% (in hydrochloride), ammonia-nitrogen content 0.025% (m/m), ash content 0.14% (m/m).
The present embodiment lysine hydrochloride crystal purity is 99.7%, and yield is 70%; In lysine hydrochloride mixture, lysine hydrochloride purity is 66%, and yield is 94%.The present embodiment lysine hydrochloride total recovery is 98.2%.
Embodiment 2
The invention provides a kind of method extracting lysine hydrochloride from lysine hydrochloride fermented liquid, specifically comprise following steps:
Step (1): get lysine hydrochloride fermented liquid, wherein solid content is 23%, and pH value is 6.7, lysine hydrochloride content 18g/100mL.Adopt microporous membrane to filter described lysine hydrochloride fermented liquid, obtain micro-filtrate and film concentrated phase;
Described ceramic membrane aperture is 0.08 μm; Described microporous membrane intake pressure is 0.25MPa, and top hole pressure is 0.15MPa, and membrane flux is 60LMH.
Step (2): adopt gac to decolour described micro-filtrate, obtain destainer; Described gac addition is the 0.0015g/mL of micro-filtrate, and desolventing technology temperature is 65 DEG C, and the time is 45min.
Step (3): by dense for above-mentioned destainer vacuum concn, vacuum tightness is-0.085MPa, and temperature is 65 DEG C, and vacuum concentration is 72% to solid content, obtains concentrated solution.By above-mentioned concentrated solution adjust ph to 4.5.Above-mentioned concentrated solution is cooled to 52 DEG C, in concentrated solution, adds the lysine hydrochloride crystal seed of 6% (m/m), after growing the grain 3h, be down to 42 DEG C with the rate of temperature fall of 1 DEG C/h; Then be down to 12 DEG C with the rate of temperature fall of 3 DEG C/h, obtain magma.The wet crystal efficient ebullated bed 55 DEG C oven dry of gained, obtains lysine hydrochloride crystal.
Step (4): step (1) gained film concentrated phase and step (3) gained crystalline mother solution merge final vacuum and concentrate, vacuum tightness is at-0.085MPa, thickening temperature is 67 DEG C, vacuum concentration, to solid content 35% (m/m) spraying dry afterwards, obtains lysine hydrochloride mixture.
Wherein, the present embodiment lysine hydrochloride crystal purity is 99%, yield 71%; In lysine mixture, lysine hydrochloride purity is 65.5%, and yield is 94%.The present embodiment lysine hydrochloride total recovery is 98.26%.
Embodiment 3
The invention provides a kind of method extracting lysine hydrochloride from lysine hydrochloride fermented liquid, specifically comprise following steps:
Step (1): get lysine hydrochloride fermented liquid, wherein solid content is 25%, and pH value is 6.8, lysine hydrochloride content 20g/100mL.Adopt microporous membrane to filter described lysine hydrochloride fermented liquid, obtain micro-filtrate and film concentrated phase;
Described ceramic membrane aperture is 0.1 μm; Described microporous membrane intake pressure is 0.3MPa, and top hole pressure is 0.2MPa, and membrane flux is 70LMH.
Step (2): adopt gac to decolour described micro-filtrate, obtain destainer; Described gac addition is the 0.002g/mL of micro-filtrate, and desolventing technology temperature is 70 DEG C, and the time is 60min.
Step (3): by dense for above-mentioned destainer vacuum concn, vacuum tightness is-0.09MPa, and temperature is 70 DEG C, and vacuum concentration is 75% to solid content, obtains concentrated solution.By above-mentioned concentrated solution adjust ph to 5.0.Above-mentioned concentrated solution is cooled to 55 DEG C, in concentrated solution, adds the lysine hydrochloride crystal seed of 10% (m/m), after growing the grain 4h, be down to 45 DEG C with the rate of temperature fall of 1 DEG C/h; Then be down to 15 DEG C with the rate of temperature fall of 3 DEG C/h, obtain magma.The wet crystal efficient ebullated bed 60 DEG C oven dry of gained, obtains lysine hydrochloride crystal.
Step (4): by step (1) gained film concentrated phase and step (3) gained crystalline mother solution mixture vacuum concentration, vacuum tightness is at-0.09MPa, thickening temperature is 70 DEG C, vacuum concentration, to solid content 40% (m/m) spraying dry afterwards, is prepared into 65.2% lysine hydrochloride.
Wherein, the present embodiment lysine hydrochloride crystal purity is 99.73%, and yield is 72.5%; In lysine hydrochloride mixture, lysine hydrochloride purity is 65.6%, and yield is 94.1%.The present embodiment lysine hydrochloride total recovery is 98.38%.
Embodiment 4
The invention provides a kind of method extracting lysine hydrochloride from lysine hydrochloride fermented liquid, specifically comprise following steps:
Step (1): get 500L and heat secondary fermentation liquid, solid content 25%, lysine content 19.5g/100mL, pH value 6.8.Fermented liquid uses 0.05 μm of ceramic membrane filter except thalline, film intake pressure 0.2MPa, top hole pressure 0.15MPa, flux 55.8LMH,
Step (2): microfiltration of ceramic membrane liquid, solid content 20%, lysine content 15.1g/100mL.Micro-filtrate uses burgy decolouring, and burgy addition is the 0.0014g/mL of micro-filtrate, and bleaching temperature is 67 DEG C, and bleaching time is 40min.It is 83% that 430nm measures dialyzate mixing transmittance.
Step (3): destainer is concentrated in vacuo to solid content 74%, concentrated solution uses concentrated hydrochloric acid adjust ph to 4.6 after pumping into crystallizer, be cooled to 55 DEG C and add 450g crystal seed, growing the grain 2h, growing the grain terminates rear beginning decrease temperature crystalline, and controlling cooling rate between wherein 55 DEG C ~ 45 DEG C is 1 DEG C/h, controlling cooling rate between 45 DEG C ~ 15 DEG C is 3 DEG C/h, decrease temperature crystalline to 15 DEG C, centrifugation, crystal absolute ethanol washing.Mother liquor solid content 56% (m/m), lysine content 34.2% (m/v).
The wet crystal efficient ebullated bed 50-60 DEG C of oven dry of gained, crystal is white needles, crystalline content 98.8% (in hydrochloride), ammonia-nitrogen content 0.025% (m/m), ash content 0.14% (m/m).
Step (4): by step (1) gained ceramic membrane concentrated phase and step (3) gained crystalline mother solution mixture vacuum concentration, vacuum tightness is at-0.085MPa, thickening temperature is 67 DEG C, vacuum concentration, to solid content 32% (m/m) spraying dry afterwards, is prepared into the lysine hydrochloride that content is 65%.
The present embodiment lysine hydrochloride crystal purity is 99%, and yield is 72.6%; In lysine hydrochloride mixture, lysine hydrochloride purity is 66%, and yield is 94.6%.The present embodiment lysine hydrochloride total recovery is 98.5%.
Embodiment 5
The invention provides a kind of method extracting lysine hydrochloride from lysine hydrochloride fermented liquid, specifically comprise following steps:
Step (1): get 400L and heat secondary fermentation liquid, solid content 23%, lysine content 18.2g/100mL, pH value 6.75.
Fermented liquid uses 0.05 μm of ceramic membrane filter except thalline, film intake pressure 0.2MPa, top hole pressure 0.15MPa, flux 56.1LMH, concentrated 6.6 times, water-dialyzing dosage 130L.Concentrated phase volume 80L, concentrated phase lysine content 4.2g/100mL, solid content 12.6%.
Step (2): microfiltration of ceramic membrane liquid, solid content 18%, lysine content 14.7g/100mL.Micro-filtrate uses burgy decolouring, and burgy addition is the 0.0012g/mL of micro-filtrate, and bleaching temperature is 65 DEG C, and bleaching time is 38min.It is 81% that 430nm measures dialyzate mixing transmittance.
Step (3): destainer is concentrated to solid content 75%, concentrated solution uses concentrated hydrochloric acid adjust ph to 4.8 after pumping into crystallizer, be cooled to 55 DEG C and add 300g crystal seed, growing the grain 2.5h, growing the grain terminates rear beginning decrease temperature crystalline, and controlling cooling rate between wherein 55 DEG C ~ 45 DEG C is 1 DEG C/h, controlling cooling rate between 45 DEG C ~ 15 DEG C is 3 DEG C/h, decrease temperature crystalline to 15 DEG C, centrifugation, crystal absolute ethanol washing.Mother liquor solid content 57.5% (m/m), lysine content 32% (m/v).
The wet crystal efficient ebullated bed 50-60 DEG C of oven dry of gained, crystal is white needles, crystalline content 98.7% (in hydrochloride), ammonia-nitrogen content 0.02% (m/m), ash content 0.15% (m/m).
Step (4): gained ceramic membrane concentrated phase and crystalline mother solution mixture vacuum concentration, vacuum tightness is at-0.085MPa, and thickening temperature is 65 DEG C, and vacuum concentration, to solid content 37% (m/m) spraying dry afterwards, is prepared into 65% lysine hydrochloride.
The present embodiment lysine hydrochloride crystal purity is 99.1%, and yield is 71.8%; In lysine hydrochloride mixture, lysine hydrochloride purity is 65.8%, and yield is 94.1%.The present embodiment lysine hydrochloride total recovery is 98.3%.
Embodiment 6
The invention provides a kind of method extracting lysine hydrochloride from lysine hydrochloride fermented liquid, specifically comprise following steps:
Step (1): get 300L and heat secondary fermentation liquid, solid content 22%, lysine content 16.9g/100mL, pH value 6.9.
Fermented liquid uses 0.05 μm of ceramic membrane filter except thalline, film intake pressure 0.2MPa, top hole pressure 0.15MPa, flux 56.7LMH, concentrated 6.2 times, water-dialyzing dosage 90L.Concentrated phase volume 63L, concentrated phase lysine content 4.2g/100mL, solid content 14.4%.
Step (2): microfiltration of ceramic membrane liquid, solid content 19.5%, lysine content 15.7g/100mL.Micro-filtrate uses burgy decolouring, and burgy addition is the 0.0016g/mL of micro-filtrate, and bleaching temperature is 65 DEG C, and bleaching time is 40min.It is 84% that 430nm measures dialyzate mixing transmittance.
Step (3): destainer is concentrated to solid content 72%, concentrated solution uses concentrated hydrochloric acid adjust ph to 4.7 after pumping into crystallizer, be cooled to 55 DEG C and add 200g crystal seed, growing the grain 3h, growing the grain terminates rear beginning decrease temperature crystalline, and controlling cooling rate between wherein 55 DEG C ~ 45 DEG C is 1 DEG C/h, controlling cooling rate between 45 DEG C ~ 15 DEG C is 3 DEG C/h, decrease temperature crystalline to 15 DEG C, centrifugation, crystal absolute ethanol washing.Mother liquor solid content 55% (m/m), lysine content 31.8% (m/v).
The wet crystal efficient ebullated bed 50-60 DEG C of oven dry of gained, crystal is white needles, crystalline content 98.7% (in hydrochloride), ammonia-nitrogen content 0.018% (m/m), ash content 0.1% (m/m).
Step (4): gained ceramic membrane concentrated phase and crystalline mother solution mixture vacuum concentration, vacuum tightness is at-0.085MPa, and thickening temperature is 67 DEG C, and vacuum concentration, to solid content 34% (m/m) spraying dry afterwards, is prepared into 65% lysine hydrochloride.
The present embodiment lysine hydrochloride crystal purity is 98.8%, and yield is 70%; In lysine hydrochloride mixture, lysine hydrochloride purity is 66%, and yield is 94%.The present embodiment lysine hydrochloride total recovery is 98.2%.
From above-described embodiment, method technique of the present invention is simple, and environmental protection, mother liquor and film concentrated phase prepare the object that 65% Methionin can reach waste reclaimation.Meanwhile, and traditional technology compares, and adopts method of purification of the present invention can obtain the Methionin by product of content 98.5% and above lysine hydrochloride salable product and 65%.And the Methionin of 65% is as the by product of this technique, abundanter economic benefit can be brought to production.
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (9)
1. a method of purification for lysine hydrochloride, is characterized in that, comprises following steps:
Step (1): adopt microporous membrane to filter lysine hydrochloride fermented liquid, obtain micro-filtrate and film concentrated phase;
Step (2): adopt gac to decolour described micro-filtrate, obtain destainer;
Step (3): by gained destainer through vacuum concentration, acid adjustment, decrease temperature crystalline, obtains wet crystal and crystalline mother solution; The further centrifugal oven dry of wherein said wet crystal, obtains lysine hydrochloride crystal;
Step (4): step (1) gained film concentrated phase and step (3) gained crystalline mother solution are merged, gained mixed solution, through vacuum concentration, spraying dry, obtains the lysine hydrochloride of content more than 65%.
2. method according to claim 1, is characterized in that, in step (1), the intake pressure of described microporous membrane is 0.2 ~ 0.3MPa, and inlet and outlet pressure difference is 0.05MPa.
3. method according to claim 1, is characterized in that, in step (1), the membrane flux of described microporous membrane is 50 ~ 70LMH; The aperture of described microporous membrane is 0.05 μm ~ 0.1 μm.
4. method according to claim 1, is characterized in that, in step (2), described gac addition is 0.001 ~ 0.002g/mL micro-filtrate; Bleaching temperature is 60 ~ 70 DEG C, and the time is 30 ~ 60min.
5. the method according to any one of Claims 1 to 4, is characterized in that, in step (3), described vacuum concentration condition is: vacuum tightness is-0.08 ~-0.09MPa, and temperature is 60 ~ 70 DEG C.
6. the method according to any one of Claims 1 to 4, is characterized in that, in step (3), is that acid adjustment to pH value are 4.0 ~ 5.0 after 70 ~ 75% by destainer vacuum concentration to solid content.
7. the method according to any one of Claims 1 to 4, it is characterized in that, in step (3), described decrease temperature crystalline concrete operation step is: be first cooled to 55 DEG C, 1 ~ 10% throw in lysine hydrochloride crystal seed by mass percentage, after growing the grain 2 ~ 4h, be down to 45 DEG C with the speed of 1 DEG C/h; Then 15 DEG C are down to the speed of 3 DEG C/h, centrifugal, with absolute ethanol washing, utilize efficient ebullated bed in 50-60 DEG C of oven dry, obtain lysine hydrochloride crystal.
8. the method according to any one of Claims 1 to 4, is characterized in that, in step (4), described vacuum concentration condition is: vacuum tightness is at-0.08Mpa ~-0.09Mpa, and thickening temperature is 65 ~ 70 DEG C; Being concentrated into solid content is 30% ~ 40%, then carries out spraying dry, obtains lysine hydrochloride.
9. method according to claim 1, is characterized in that, in described lysine hydrochloride fermented liquid, solid content is 22 ~ 25%, and pH value is 6.7 ~ 6.9, lysine hydrochloride content 15 ~ 20g/100mm.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN114181388A (en) * | 2021-11-30 | 2022-03-15 | 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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| CN104892437A (en) * | 2015-05-15 | 2015-09-09 | 南通荣泰生物科技有限公司 | Production technology for L-lysine hydrochloride |
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| CN103553951A (en) * | 2013-10-31 | 2014-02-05 | 安徽丰原发酵技术工程研究有限公司 | Method of extracting and preparing lysine sulphate from fermenting liquid containing lysin |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN114181388A (en) * | 2021-11-30 | 2022-03-15 | 河北圣雪大成制药有限责任公司 | Method for extracting polylysine from 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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