CN108191868B - A kind of processing method of the molten refinement mother liquor of riboflavin acid - Google Patents
A kind of processing method of the molten refinement mother liquor of riboflavin acid Download PDFInfo
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- CN108191868B CN108191868B CN201810004007.9A CN201810004007A CN108191868B CN 108191868 B CN108191868 B CN 108191868B CN 201810004007 A CN201810004007 A CN 201810004007A CN 108191868 B CN108191868 B CN 108191868B
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D475/00—Heterocyclic compounds containing pteridine ring systems
- C07D475/12—Heterocyclic compounds containing pteridine ring systems containing pteridine ring systems condensed with carbocyclic rings or ring systems
- C07D475/14—Benz [g] pteridines, e.g. riboflavin
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Abstract
The invention discloses a kind of processing methods of the molten refinement mother liquor of riboflavin acid, belong to riboflavin extractive technique field.This method comprises: the molten refinement mother liquor of acid to be passed through to the process of batch fractionating concentrate hydrochloric acid, obtain the azeotropic hydrochloric acid of acid content 20% or so, due to during concentrate hydrochloric acid, reduce content of hydrochloric acid in the molten mother liquor of acid, 0.5% or so is reduced to by 6-8% and steams partial moisture, so that riboflavin is precipitated in mother liquor, then pass through membrane separation concentration crystal recycling riboflavin therein.Wherein membrane separation concentration crystal step includes periosteum pretreatment (micro-filtration) and diffusion dialysis film process two-stage film process, and the concentrate of diffusion dialysis film is returned to again in pretreatment periosteum, further recycles the dissolubility riboflavin in the pretreated penetrating fluid of periosteum.After the above method is handled, the extract yield of riboflavin improves about 3% during preparing high-content riboflavin, and greatly reduces the discharge amount of high-salt wastewater.
Description
Technical field
The present invention relates to riboflavin extractive technique fields, and in particular to a kind of processing side of the molten refinement mother liquor of riboflavin acid
Method.
Background technique
Riboflavin (Riboflavin) also known as vitamin B2 (abbreviation VB2) are a kind of water soluble vitamins needed by human.
Riboflavin has extensive physiological function as a kind of basal nutrient substance.Evaluation is thus classified as by the World Health Organization (WHO)
One of the six big indexs of growth in humans development and nutrition condition, in clinical treatment, feed processing, food industry and cosmetics system
Field is made with important value.
It is a kind of very cost-effective method that microbe fermentation method, which prepares riboflavin, prepares riboflavin method phase with other
Prepare that riboflavin is at low cost, and pollution is few than, microbe fermentation method, the big production commercial city of the riboflavin of world's production at present is using micro-
Biological fermentation process produces riboflavin.
During microbe fermentation method prepares high-content riboflavin, the riboflavin for generalling use high level passes through acid
It is molten, be precipitated and etc. can just obtain the riboflavin of high-content, to meet food, drug standards requirement.Since riboflavin is in acidity
There is certain solubility, in order to recycle riboflavin therein, traditional processing method is the method by adding alkali in aqueous solution
Acid therein is neutralized, allows riboflavin to be precipitated, sedimentation filtration.Since a large amount of salt can be generated in N-process, to obtain one
Kind high-salt wastewater.
In the patent of 101205230 A of Publication No. CN, a kind of multistage continuous membrane filter separating riboflavin is provided
With the method for riboflavin thallus, Lactochrome fermentation liquor is passed through alkali tune by this method, and multistage continuous membrane filter washing impurity-removing stabilizes
Processing, crystallization, membrane separation concentration crystal step directly obtain riboflavin product, since this method requires first by Lactochrome fermentation liquor
Alkali tune processing, and riboflavin be under alkaline condition it is unstable, riboflavin is easy to produce degradation, reduces product quality, together
When its crystallization process be exactly acid adding neutralize process, salt can be also generated in N-process, to generate a kind of high-salt wastewater.
The patent disclosures such as Publication No. CN1774438A, CN1275375A, CN1765898A, CN 1056845A are all
A kind of high-content, the riboflavin of high-quality are obtained with corresponding step by the way that acid is molten using a kind of riboflavin of high level.?
The processing method of the subsequent molten refinement mother liquor of acid is not all provided in these patents.
The solubility of riboflavin in an acidic solution is related to concentration, that is, acid content of acid, the core yellow in the molten refinement mother liquor of acid
Element is substantially at the state of dissolution.In order to recycle riboflavin therein.Traditional technique is neutralized wherein by way of adding alkali
Acid, alkali addition process is there are three disadvantage: first is that needing to consume a large amount of alkali；Second is that plus a large amount of salt is generated after alkali neutralization, obtain
A kind of high-salt wastewater of salt content 8-10% increases cost, clean manufacturing added cost to subsequent sewage treatment；Third is that riboflavin
Solubility is larger in salting liquid, causes recycling yield lower.
Therefore, it during preparing high-content riboflavin, needs to study the subsequent molten refinement mother liquor of acid, finds one kind
More efficient, clean method handles the molten refinement mother liquor of acid, to obtain higher yield and more clean production method.?
In the case where scale, cleanly production, the processing of dilute hydrochloric acid and the processing of the mother liquor containing dilute hydrochloric acid cannot be taken traditional again
A kind of method of alkali neutralization, it should develop more scientific, more economical, clean method.
Summary of the invention
In order to solve the processing method defect of traditional dilute hydrochloric acid and the mother liquor containing dilute hydrochloric acid, further increase from fermentation liquid
The extract yield for preparing high-content riboflavin, the present invention provides a kind of processing methods of the molten refinement mother liquor of riboflavin acid, with this
Extract yield improves 2%-4% after method handles the molten mother liquor of riboflavin acid, extraction cost of material has been saved, by per kilogram riboflavin
Meter, it is every to extract one kilogram of riboflavin 1 kilogram of sodium hydroxide of saving.I.e. this method solve prepare high-content riboflavin to pass in the process
The method for subsequent processing of system leads to the problem of high-salt wastewater, and improves extract yield.The scheme is as follows:
The present invention implements to provide a kind of processing method of the molten refinement mother liquor of riboflavin acid, method includes the following steps:
(1) the molten refinement mother liquor of acid is subjected to intermittent fractionation under the conditions of 70-75 DEG C, it is (dense to distillate azeotropic hydrochloric acid from tower top
19-20% is spent, due to measurement error, data are had differences), it is the rectifying mother liquor less than 0.5% from tower bottom extraction acid content.The step
Suddenly not only the acid distillation in the molten refinement mother liquor of acid is come out, reduces the concentration of acid；Also steaming partial moisture makes the dense of riboflavin
Degree is increased so that precipitation and subsequent film process.
(2) insoluble riboflavin is separated by micro-filtration after the rectifying mother liquor that step (1) obtains staticly settles, concentrate is used
In recycling riboflavin；Wherein, riboflavin is almost insoluble in water, by the rectifying mother liquor after batch distillation by standing the side to cool down
Formula allows riboflavin therein that sedimentation is precipitated.Under the driving of pressure and speed, by acidproof microfiltration membranes make suspended solid material with
Liquid separation can filter out the solid particle that diameter is greater than 0.1 micron from water, and the riboflavin of solubilised state send step (3).It will
Riboflavin in micro-filtration treated concentrate by plate-frame filtering can (between also changeable riboflavin crystal form so that its more
Filters pressing separates well) the riboflavin filter cake containing a small amount of impurity, by the riboflavin for being further refining to obtain high-content.
(3) penetrating fluid that step (2) obtains is concentrated by diffusion dialysis film, and cycles of concentration is 3-7 times (preferably 5
Times or so), concentrate return step (2) is handled.Core yellow containing 800-1000ppm in micro-filtration treated penetrating fluid
Element, 0.5% or so hydrochloric acid and a small amount of organic matter, retained by riboflavin of the diffusion dialysis film to wherein solubilised state, and salt
Acid and small molecular weight impurity then penetrate diffusion dialysis film, be constantly concentrated by diffusion dialysis film, in concentrate riboflavin concentration by
Step improves, and so that the soluble riboflavin overwhelming majority is converted to insoluble core yellow when riboflavin concentration is improved to 4000-5000ppm
Element, concentrate is back to microfiltration membranes and handles when by after diffusion dialysis film process.Penetrating fluid warp after diffusion dialysis UF membrane
Simple biochemical treatment can direct emission or reuse.
Wherein, the source of the molten refinement mother liquor of acid in present invention implementation are as follows: riboflavin, prior art are extracted from fermentation liquid
Acid extracting is generally used, the acid solution containing riboflavin is obtained after the riboflavin of low content is dissolved by concentrated hydrochloric acid, then should
Riboflavin is precipitated by way of adding water in acid solution, the riboflavin after filtering precipitation, respectively obtains our height of needs and contains
Measure riboflavin and the molten refinement mother liquor of acid containing riboflavin.Specifically, the acid content of the molten refinement mother liquor of acid is 6-8%, and riboflavin contains
Amount is 2000-3000ppm, contains a small amount of organic matter.
Wherein, in step (1), the reflux ratio of intermittent fractionation is 0.5-0.8.
Wherein, in step (1), the core yellow cellulose content of rectifying mother liquor is 4000-5000ppm, and acid content contains less than 0.5%
There is a small amount of organic matter.Preferably, the acid content of the riboflavin of rectifying mother liquor is controlled in 0.3-0.5% to reduce distillation energy consumption.
Specifically, in step (2), the aperture of microfiltration membranes is 100-200nm, operating pressure 0.1-0.2MPa, operation
Temperature is 30-40 DEG C.
Preferably, in step (2), micro-filtration is carried out using periosteum, membrane tube length and membrane tube diameter ratio are 60-70:1；?
The clarifying effect for making us satisfied can be reached between this ratio, and guarantee that film has longer service life and preferable film
Flux.
Wherein, in step (2), cross-current flow is used to carry out micro-filtration to reduce attachment of the crystal on periosteum.
Wherein, in step (2), the core yellow cellulose content of penetrating fluid is 800-1000ppm, and acid content contains less than 0.5%
A small amount of organic matter.
Wherein, in step (3), the molecular cut off of diffusion dialysis film is 200-400, operating pressure 0.1-
0.2MPa, operation temperature are 30-40 DEG C.
Wherein, the core yellow cellulose content for the concentrate that step (3) obtains is the concentration difference of 4000-5000ppm and rectifying mother liquor
Seldom, acid and organic matter are substantially free of.
Wherein, the core yellow cellulose content for the penetrating fluid that step (3) obtains is less than 80ppm, and acid content is highly susceptible to less than 0.7%
Processing.Wherein, a series of structural units that the diffusion dialysis device that step (3) uses is made of a certain number of films, wherein
Each unit separates into dialysing compartment and diffuser casing by an anion homogeneous membrane, using counter-current operation, isolates therein low
Content acid solution and a small amount of organic matter.
Preferably, method provided by the invention the following steps are included:
(1) the molten refinement mother liquor of acid is subjected to intermittent fractionation, reflux ratio 0.5-0.8, from tower top under the conditions of 70-75 DEG C
Azeotropic hydrochloric acid is distillated, is the rectifying mother liquor less than 0.5% from tower bottom extraction acid content.Wherein, the core yellow cellulose content of rectifying mother liquor is
4000-5000ppm, acid content 0.3-0.5%.
(2) micro-filtration is carried out by periosteum after the rectifying mother liquor that step (1) obtains staticly settles, the aperture of microfiltration membranes is 100-
200nm, operating pressure 0.1-0.2MPa, operation temperature are 30-40 DEG C, concentrate filters pressing are obtained riboflavin, by penetrating fluid
Step (3) is sent to be handled.Wherein, the core yellow cellulose content of penetrating fluid is 800-1000ppm, acid content 0.3-0.5%.
(3) penetrating fluid that step (2) obtains is concentrated by the diffusion dialysis film that molecular cut off is 200-400, dense
Demagnification number is 3-7 times, operating pressure 0.1-0.2MPa, and operation temperature is 30-40 DEG C, at concentrate return step (2)
Reason.Wherein, the core yellow cellulose content of concentrate is 4000-5000ppm.
The molten refinement mother liquor of riboflavin acid of the invention is a kind of acid content 6- generated during preparing high-content riboflavin
8%, a kind of mixed aqueous solution of 000-3000ppm containing Riboflavin Tetrabutyrate and a small amount of organic matter.It is removed in the mixture and contains riboflavin
Outside, also contain cell fragment, protein and other organic stickums, and most riboflavin are in a kind of dissolution
State.In order to recycle riboflavin therein, it is necessary to reduce content sour in the mixed aqueous solution.It reduces sour in mixed aqueous solution
The method of content are as follows: the batch fractionating mixed solution, in control charging rate (0.5-2.0L/min), reflux ratio, heating temperature
When concentrate concentration of hydrochloric acid, so that realizing reduces sour content in the mixed solution.In batch distillation process, first carry out
The fixation split ratio of certain time (0.5-2.0h) operates, and rectifying column is made to be in a kind of stable state, after the operation, control
Reflux ratio carries out rectifying at certain value (0.5-0.8).The dilute hydrochloric acid that acid content is 20% or so is obtained in tower top, tower bottom is contained
The mixed solution that acid amount is 0.5% or so.
Part water distillates in reduction due to acid content and distillation process in mixed aqueous solution after reducing acid content, makes
Core yellow cellulose content is obtained to be concentrated into 4000-5000ppm by original 2000-3000ppm and crystallized out.Due to the ingredient of the feed liquid
Complexity, there are also some organic stickums in addition to riboflavin, common separate mode is difficult to separate in riboflavin, in order to divide
From riboflavin therein, the present invention recycles riboflavin therein by the way of the filtering of two-stage film.The first order use aperture for
The periosteum of 100-200nm recycles wherein particle riboflavin, and film stabilized flux is maximum when to guarantee separation, and fouling membrane degree is minimum,
Binding experiment data, preferentially select the operating parameter for making us satisfied, operating pressure 0.1-0.2MPa, and operation temperature is
30-40℃.It can guarantee the continuous and steady operation of film in the operating parameter control range, and alleviate fouling membrane, the infiltration of periosteum
Transparent liquid enters diffusion dialysis film, wherein soluble riboflavin is further recycled, using diffusion dialysis film to the core of wherein solubilised state
Flavine is retained, and salinity and small molecular weight impurity then penetrate diffusion dialysis film, since pipe membrane separation concentration crystal is in material
Riboflavin particle have good rejection effect, ensure that the stable operation of diffusion dialysis film.It is opposite due to riboflavin molecule
Molecular weight is 376.4, and diffusion dialysis retaining molecular weight is generally in 200-400, by selecting a kind of suitable diffusion dialysis film
The rejection to riboflavin can be guaranteed in 90-95%.The concentrate of diffusion dialysis film is back to periosteum and is further processed recycling core
Flavine.
Method provided by the invention has the advantages that
(1) azeotropic hydrochloric acid recycled can be recycled after processing in acid dissolution.
(2) extract yield improves 2-4% during preparing high-content riboflavin by broth extraction.
(3) it does not need to additionally incorporate the raw materials such as alkali, reduces production cost.
(4) greatly reduce high-salt wastewater, while BOD value can also drop to 50% or so, be subsequent sewage treatment save the cost,
Realize energy-saving, clean manufacturing.
(5) this method energy separate section colloid is easy to filters pressing separating riboflavin, can improve speed of filter pressing.
(6) a kind of good solution of molten refinement mother liquor treatment process of suitable acid has been determined, has been conducive to industrialized production.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, embodiment of the present invention is made below further
Ground detailed description.
Embodiment 1:
The molten refinement mother liquor of 500L acid, acid content 6.9%, wherein 276ppm containing Riboflavin Tetrabutyrate.The molten mother liquor of the batch fractionating acid,
Charging rate is controlled in the case where 1L/min, is first run 1 hour in the case where reflux ratio is 0.5, so that entire rectifying column
It is stable, rectifying is then carried out under this reflux ratio.Tower top obtains the dilute hydrochloric acid that concentration is 19.3%, and volume is about 200L, tower
Bottom obtains the mixed solution that volume is about 300L, 4006ppm containing riboflavin in the solution, acid content 0.45%.By the solution
It stands, riboflavin is allowed to be precipitated.The feed liquid is first crossed into periosteum filtering, about 3 squares of total membrane area, the aperture of film is in 100-200nm, behaviour
Making pressure is 0.15MPa, and control feed liquid temperature is lower than 35 DEG C.Undissolved riboflavin is recycled, in the penetrating fluid after crossing periosteum also
Containing riboflavin about 900ppm, which is crossed into diffusion dialysis film, riboflavin is further concentrated, water penetration is allowed to come out, diffusion is seeped
Analysis retaining molecular weight is 200-400, and most riboflavin is allowed to retain.In the case where cycles of concentration is 5 times, by concentrate
It is back to periosteum, is repeated above operation, riboflavin therein is constantly recycled.The clear liquid of diffusion dialysis film is due to containing minute quantity
Acid discharges after being neutralized by way of adding alkali through simple biochemical treatment, and riboflavin can be recycled about after handling above
1kg。
Embodiment 2:
The molten refinement mother liquor of 800L acid, acid content 7.4%, wherein 900ppm containing Riboflavin Tetrabutyrate.The molten mother liquor of the batch fractionating acid,
Charging rate is controlled in the case where 1.5L/min, is first run 1 hour in the case where reflux ratio is 0.7, so that entire rectifying
Tower is stable, and rectifying is then carried out under this reflux ratio.Tower top obtains the dilute hydrochloric acid that concentration is 19.0%, and volume is about 300L.
Tower bottom obtains the mixed solution that volume is about 500L, 4600ppm containing riboflavin in the solution, acid content 0.4%.By the solution
It stands, riboflavin is allowed to be precipitated.The feed liquid is first crossed into periosteum filtering, about 3 squares of total membrane area, the aperture of film is in 100-200nm, behaviour
Making pressure is 0.15MPa, and control feed liquid temperature is lower than 35 DEG C.Undissolved riboflavin is recycled, in the penetrating fluid after crossing periosteum also
Containing riboflavin about 800ppm, which is crossed into diffusion dialysis film, riboflavin is further concentrated, water penetration is allowed to come out, diffusion is seeped
Analysis retaining molecular weight is 200-400, and most riboflavin is allowed to retain.In the case where cycles of concentration is 5 times, by concentrate
It is back to periosteum, is repeated above operation, riboflavin therein is constantly recycled.The clear liquid of diffusion dialysis film is due to containing minute quantity
Acid discharges after being neutralized by way of adding alkali through simple biochemical treatment, and riboflavin can be recycled about after handling above
2kg。
Embodiment 3:
The embodiment is that the molten refinement mother liquor of method processing acid neutralized using tradition recycles riboflavin therein, is embodiment
2 comparison example.
The molten refinement mother liquor of 800L acid, acid content 7.4%, wherein 900ppm containing Riboflavin Tetrabutyrate.For recycle riboflavin therein and
Sewage qualified discharge, first with, with acid therein, pH to 6.5, alkali charge about 65kg is adjusted in lye, obtaining salt content is 10%, is contained
The mixed solution of Riboflavin Tetrabutyrate 900ppm stands the mixed solution, riboflavin is allowed to be precipitated, since riboflavin is in saline solns center
Flavine solubility greatly increases, and filters the solution and obtains riboflavin about 1kg, obtaining salt content in clear liquid after filtering is about 10%
High-salt wastewater, due to salt content height, wastewater biochemical processing is difficult, and the period is long and is difficult to qualified discharge.
From embodiment 2 and embodiment 3 it is found that the yield for the method that the present invention uses is 2 times of conventional method, alkali can be reduced
Hydrochloric acid 400L or so/1000L mother liquor, remarkable in economical benefits can be recycled in dosage 81.25kg/1000L mother liquor.Meanwhile it and will not produce
Raw high-salt wastewater, to reduce the cost of wastewater treatment.
The foregoing is merely presently preferred embodiments of the present invention, is not intended to limit the invention, it is all in spirit of the invention and
Within principle, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of processing method of the molten refinement mother liquor of riboflavin acid, which is characterized in that the described method comprises the following steps:
(1) the molten refinement mother liquor of acid is subjected under the conditions of 70-75 DEG C intermittent fractionation, azeotropic hydrochloric acid is distillated from tower top, from tower bottom
Producing acid content is the rectifying mother liquor less than 0.5%；
(2) insoluble riboflavin is separated by micro-filtration after the rectifying mother liquor that step (1) obtains staticly settles, concentrate is used for back
Receive riboflavin；
(3) penetrating fluid that step (2) obtains is concentrated by diffusion dialysis film, and cycles of concentration is 3-7 times, and concentrate returns to step
Suddenly (2) are handled.
2. the processing method of the molten refinement mother liquor of riboflavin acid according to claim 1, which is characterized in that the molten purification of acid
The acid content of mother liquor is 6-8%, and the content of riboflavin is 2000-3000ppm.
3. the processing method of the molten refinement mother liquor of riboflavin acid according to claim 1, which is characterized in that in step (1),
The reflux ratio of intermittent fractionation is 0.5-0.8.
4. the processing method of the molten refinement mother liquor of riboflavin acid according to claim 1, which is characterized in that in step (1),
The core yellow cellulose content of rectifying mother liquor is 4000-5000ppm.
5. the processing method of the molten refinement mother liquor of riboflavin acid according to claim 1, which is characterized in that in step (2),
The aperture of microfiltration membranes is 100-200nm, and operating pressure 0.1-0.2MPa, operation temperature is 30-40 DEG C.
6. the processing method of the molten refinement mother liquor of riboflavin acid according to claim 1, which is characterized in that in step (2),
Micro-filtration is carried out using periosteum, membrane tube length and membrane tube diameter ratio are 60-70:1.
7. the processing method of the molten refinement mother liquor of riboflavin acid according to claim 1, which is characterized in that in step (2),
The core yellow cellulose content of penetrating fluid is 800-1000ppm.
8. the processing method of the molten refinement mother liquor of riboflavin acid according to claim 1, which is characterized in that in step (3),
The molecular cut off of diffusion dialysis film is 200-400, and operating pressure 0.1-0.2MPa, operation temperature is 30-40 DEG C.
9. the processing method of the molten refinement mother liquor of riboflavin acid according to claim 1, which is characterized in that step (3) obtains
Concentrate core yellow cellulose content be 4000-5000ppm.
10. the processing method of the molten refinement mother liquor of riboflavin acid according to claim 1, which is characterized in that the method packet
Include following steps:
(1) the molten refinement mother liquor of acid is subjected to intermittent fractionation under the conditions of 70-75 DEG C, reflux ratio 0.5-0.8 is distillated from tower top
Azeotropic hydrochloric acid produces rectifying mother liquor from tower bottom, and the core yellow cellulose content of the rectifying mother liquor is 4000-5000ppm, and acid content is greater than
0.3% and less than 0.5%；
(2) micro-filtration is carried out by periosteum after the rectifying mother liquor that step (1) obtains staticly settles, the aperture of microfiltration membranes is 100-
200nm, operating pressure 0.1-0.2MPa, operation temperature are 30-40 DEG C, concentrate filters pressing are obtained riboflavin, by penetrating fluid
Step (3) is sent to be handled, the core yellow cellulose content of the penetrating fluid is 800-1000ppm；
(3) penetrating fluid that step (2) obtains is concentrated by the diffusion dialysis film that molecular cut off is 200-400, concentration times
Number is 3-7 times, and concentrate return step (2) is handled, and the core yellow cellulose content of the concentrate is 4000-5000ppm.
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| CN109231556A (en) * | 2018-10-16 | 2019-01-18 | 合肥工业大学 | The diffusion dialysis processing unit and its processing method of acid/base waste liquid |
| CN113943291B (en) * | 2021-11-30 | 2023-09-08 | 湖北广济药业股份有限公司 | Method for removing residual DNA in riboflavin by nuclease |
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| US2367644A (en) * | 1943-05-28 | 1945-01-16 | Commercial Solvents Corp | Process for recovery of riboflavin |
| US2387023A (en) * | 1944-06-10 | 1945-10-16 | Commercial Solvents Corp | Process for the recovery of riboflavin |
| CN106396235B (en) * | 2016-11-30 | 2019-06-18 | 安徽普朗膜技术有限公司 | Mother liquor waste water processing unit and its technique in riboflavin subtractive process |
| CN106587408B (en) * | 2016-12-09 | 2019-11-05 | 三达膜科技（厦门）有限公司 | A kind of separation and concentration method of VB2 crystalline mother solution |
| CN107805251B (en) * | 2017-12-07 | 2021-01-08 | 内蒙古金达威药业有限公司 | Method for extracting riboflavin from riboflavin fermentation broth |
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