CN106587408A - Separation and concentration method of VB2 crystalline mother solution - Google Patents
Separation and concentration method of VB2 crystalline mother solution Download PDFInfo
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- CN106587408A CN106587408A CN201611127616.0A CN201611127616A CN106587408A CN 106587408 A CN106587408 A CN 106587408A CN 201611127616 A CN201611127616 A CN 201611127616A CN 106587408 A CN106587408 A CN 106587408A
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- membrane
- milipore filter
- permeate
- dope
- separation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/444—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D61/00—Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
- B01D61/58—Multistep processes
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D3/00—Halides of sodium, potassium or alkali metals in general
- C01D3/04—Chlorides
- C01D3/06—Preparation by working up brines; seawater or spent lyes
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/44—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
- C02F1/442—Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by nanofiltration
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/36—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the manufacture of organic compounds
Abstract
The invention discloses a separation and concentration method of a VB2 crystalline mother solution. According to the separation and concentration method, a ceramic membrane, an ultrafiltration membrane and a nanofiltration membrane are sequentially used for treating the VB2 crystalline mother solution. By the separation and concentration method, more than 95% of riboflavin in the crystalline mother solution can be recycled, the total yield is increased by about 14.25-19%, the purpose of recycling NaCl can be achieved, the sewage discharge in a workshop is reduced by approximately 20 times, the sewage treatment burden is reduced, and the production cost is reduced.
Description
Technical field
The invention belongs to VB2 crystalline mother solution processing technology fields, and in particular to a kind of separation concentration side of VB2 crystalline mother solutions
Method.
Background technology
VB2, is yellow or orange-yellow crystalline powder also known as riboflavin, mildly bitter flavor, about 280 degree of fusing point, and molecular weight is 369,
Amphoteric compound, it is more stable with acid solution in neutrality.In prior art, enterprise mostly using the mode of natural subsidence, reaches
To the separation of crystal and mother liquor, the mother liquor on upper strata is directly discharged, and causes the VB2 losses that there are about 15～20%, direct economic loss
Up to about 600,000/day, sewage disposal difficulty is increased.Again because the NaCl that there are about 8%～10% is present, sewage is set to be difficult to biochemical drop
Solution, to follow-up environmental protection huge pressure is caused.
The content of the invention
It is an object of the invention to overcome prior art defect, there is provided a kind of separation and concentration method of VB2 crystalline mother solutions.
Technical scheme is as follows：
A kind of separation and concentration method of VB2 crystalline mother solutions, 20～35 DEG C of the temperature of the VB2 crystalline mother solutions, pH is 4～5, is glued
Close water is spent, and the VB2 crystalline mother solutions mix to obtain solid-liquid system, in its clear liquid, VB2's for saturation VB2 solution with crystal
Content is 500～2000mg/L, and in its system, the content of VB2 is 1700～1900mg/L, and the content of NaCl is 8%～10%,
Comprise the steps：
(1) VB2 crystalline mother solutions are carried out into filtration treatment by 80～120nm ceramic membranes, obtains ceramic membrane permeate and ceramics
Film dope, 70～110min of carrying out practically time, it is 2.8～3.2Bar to enter pressure, and it is 1.8～2.2Bar to go out pressure, and mean temperature is
23～27 DEG C, average flux is 330～540LMH, and cycles of concentration is 10～32 times；
(2) the crystallized process of ceramic membrane dope is obtained into VB2；
(3) ceramic membrane permeate is adjusted after pH to 9～10 with NaOH, the rolling by 1800～2200 molecular weight is organic
Milipore filter carries out filtering and impurity removing process, obtains milipore filter permeate and milipore filter dope, and the carrying out practically time is 60～240min, is entered
Press as 17～19Bar, it is 17～18Bar to go out pressure, and mean temperature is 23～28 DEG C, average flux is 20～55LMH, cycles of concentration
For 20～37 times；
(4) milipore filter dope is carried out into emission treatment；
(5) milipore filter permeate is carried out into filtration treatment by the rolling organic nanofiltration membrane of molecular weight 180～220, must be received
Filter membrane permeate and NF membrane dope, the carrying out practically time is 50～160min, and it is 19～21Bar to enter pressure, go out pressure for 19～
21Bar, mean temperature is 23～27 DEG C, and average flux is 30～41LMH, and cycles of concentration is 12～25 times；
(6) by the crystallized process of NF membrane permeate, NaCl is obtained；
(7) NF membrane dope is adjusted after pH to 4～5, return to step (1) carries out filtration treatment, then sequentially passes through step
Suddenly (2) to (6), further to obtain VB2 and NaCl；
In a preferred embodiment of the invention, the step (1) is：VB2 crystalline mother solutions is ceramic by 100nm
Film carries out filtration treatment, obtains ceramic membrane permeate and ceramic membrane dope.
In a preferred embodiment of the invention, the step (3) is：Ceramic membrane permeate is adjusted into pH with NaOH
To after 9～10, filtering and impurity removing process is carried out by the organic milipore filter of the rolling of 2000 molecular weight, obtain milipore filter permeate and ultrafiltration
Film dope.
In a preferred embodiment of the invention, the step (5) is：By milipore filter permeate by 200nm's
Rolling organic nanofiltration membrane carries out filtration treatment, obtains NF membrane permeate and NF membrane dope.
In a preferred embodiment of the invention, also including step (8)：Ceramic membrane is carried out with 1%NaOH solution
Cleaning, 40～60min of scavenging period, cleaning temperature is 50～60 DEG C, and the flux for making ceramic membrane recovers completely.
In a preferred embodiment of the invention, also including step (9)：It is organic to rolling super with LC90# cleaning agents
Filter membrane is cleaned, and scavenging period is 40～60min, and cleaning temperature is room temperature, makes the flux of the organic milipore filter of rolling completely extensive
It is multiple.
In a preferred embodiment of the invention, also including step (10)：Received with LC90# cleaning agents are organic to rolling
Filter membrane is cleaned, and scavenging period is 40～60min, and cleaning temperature is room temperature, makes the flux of rolling organic nanofiltration membrane completely extensive
It is multiple.
Beneficial effects of the present invention：The present invention adopts membrane separation process, and production process On-line Control, the rate of filtration is fast, alkali
The property time is short, riboflavin less degradation；Sewage discharge is few, and equipment is corrosion-free；Disposing mother liquor process, reduces treatment pressure of sewage, returns
Product is received, in crystalline mother solution more than 95% riboflavin can be reclaimed, improve total recovery about 14.25～19%.
Description of the drawings
Ceramic membrane core rod variations of flux figure in the step of Fig. 1 is the embodiment of the present invention 1 (1).
The organic milipore filter core rod variations of flux figure of rolling in the step of Fig. 2 is the embodiment of the present invention 1 (3).
The organic nanofiltration core rod variations of flux figure of rolling in the step of Fig. 3 is the embodiment of the present invention 1 (5).
Specific embodiment
Technical scheme is further detailed below by way of specific embodiment and is described.
Embodiment 1
A kind of separation and concentration method of VB2 crystalline mother solutions, 20～35 DEG C of the temperature of the VB2 crystalline mother solutions, pH is 4～5, is glued
Close water is spent, and the VB2 crystalline mother solutions mix to obtain solid-liquid system, in its clear liquid, VB2's for saturation VB2 solution with crystal
Content is 500～2000mg/L, and in its system, the content of VB2 is 1700～1900mg/L, and the content of NaCl is 8%～10%,
Comprise the steps：
(1) VB2 crystalline mother solutions are passed through into 100nm ceramic membranes (T7/60/255, purchased from the limited public affairs of SanDa film Science (Xiamen)
Department) filtration treatment is carried out, obtain ceramic membrane permeate and ceramic membrane dope, 70～110min of carrying out practically time, enter pressure for 2.8～
3.2Bar, it is 1.8～2.2Bar to go out pressure, and mean temperature is 23～27 DEG C, and average flux is 330～540LMH, and cycles of concentration is
10～32 times, the concrete test parameters of the step is as shown in table 1：
The ceramic membrane experimental result of table 1 collects
| Batch | Run time | Enter to press Bar | Go out to press Bar | Mean temperature | Circular flow m3/h | Average flux | Cycles of concentration |
| 1 | 105 | 3 | 2 | 27 | 10 | 496.10 | 12.20 |
| 2 | 100 | 3 | 2 | 25 | 10 | 414.30 | 19.73 |
| 3 | 70 | 3 | 2 | 23 | 10 | 348.30 | 27.11 |
| 4 | 95 | 3 | 2 | 25 | 10 | 330.00 | 19.07 |
| 5 | 60 | 3 | 2 | 23 | 10 | 540.00 | 30.12 |
| 6 | 80 | 3 | 2 | 26 | 10 | 440.00 | 28.00 |
It is can be found that by table 1：A, from 100nm ceramic membrane filter VB2 crystalline mother solutions, enter film pressure 3Bar, rate of circulating flow
10m3/ H, 25 DEG C of mean temperature, membrane flux is between 330～540LMH, and the rate of filtration is fast.B, each batch film core flux are relatively steady
It is fixed, illustrate that the film core is adapted to long-term operation；
The testing result of ceramic membrane permeate and ceramic membrane dope is as shown in table 2：
The ceramic membrane experimental test data of table 2
It is can be found that by table 2：From 100nm ceramic membrane filter VB2 crystalline mother solutions, the mesh for improving VB2 contents can be reached
, and in fact not ceramic membrane interception VB2, but the ceramic membrane interception crystal of VB2, the separation of solid and liquid of realization.
The core rod variations of flux of ceramic membrane is as shown in Figure 1.By Fig. 1 it can be found that：Batch 1～6 meets pottery membrane flux
Variation tendency.With the carrying out of filtration experiment, film core is constantly contaminated, and flux declines；In addition, clear liquid constantly passes through film, it is dense
Liquid is stayed in membranous system and constantly circulated, and concentration is constantly raised, and forms film gel surface, and membrane flux can slowly decline.Six batches
The last flux of ceramic membrane is stable in 300LMH or so, illustrates having good stability for ceramic membrane membrane flux, is adapted to industry park plan；
(2) the crystallized process of ceramic membrane dope is obtained into VB2；
(3) ceramic membrane permeate is adjusted after pH to 9～10, by the organic milipore filter of the rolling of 2000 molecular weight with NaOH
(Suntar-2B02, purchased from Sandamo Science and Technology (Xiamen) Co., Ltd.) carries out filtering and impurity removing process, obtains milipore filter permeate and surpasses
Filter membrane dope, the carrying out practically time is 60～240min, and it is 17～19Bar to enter pressure, and it is 17～18Bar to go out pressure, and mean temperature is
23～28 DEG C, average flux is 20～55LMH, and cycles of concentration is 20～37 times, and the concrete test parameters of the step is as shown in table 3：
The milipore filter experimental result of table 3 collects
As shown in Table 3：A, by ceramic membrane permeate directly use ultra-filtration filters, when dope reaches saturation content, just have VB2 brilliant
Body is separated out.Irreversible damage can be caused to organic film；B, the pH to 9～10 for adjusting ceramic membrane permeate with NaOH can increase
The solubility of VB2, can reach the purpose of removal of impurities and partial concentration using ultra-filtration filters, and dope is not crystallized, and cycles of concentration is all 20
More than times；C, from 2000 molecular weight milipore filter core ceramic for filtration film permeate, enter film pressure 18Bar, mean temperature is 25 DEG C,
Average flux has 21～55LMH, and cycles of concentration has 20～36 times.
The testing result of milipore filter permeate and milipore filter dope is as shown in table 4：
The milipore filter experimental test data of table 4
It is can be found that by upper table 4：It is right from the organic milipore filter film core ceramic for filtration film permeate of rolling of 2000 molecular weight
The rejection close 20% of VB2.
The core rod variations of flux of milipore filter is as shown in Figure 2.By Fig. 2 it can be found that：Batch 1～6 meets the change of film core operation
Change trend.With the carrying out of filtration experiment, film core is constantly contaminated, flux rapid decrease；In addition, clear liquid constantly passes through film,
Dope is stayed in membranous system and constantly circulated, and concentration is constantly raised, and the solution concentration the closer to film surface is higher, and concentration extreme differenceization is not
It is disconnected to increase, clear liquid is increased toward the migration difficulty on film surface, membrane flux can slowly decline, and most telolemma core flux is close to steady.Six
The last flux of batch milipore filter all in 30LMH or so, illustrate 2000 molecular weight the organic ultrafiltration membrane treatment flux of rolling it is steady
It is qualitative good, it is adapted to industry park plan；
(4) milipore filter dope is carried out into emission treatment；
(5) the rolling organic nanofiltration membrane (Suntar-3B02, purchased from SanDa film Science that milipore filter permeate is passed through into 200nm
(Xiamen) Co., Ltd) filtration treatment is carried out, obtain NF membrane permeate and NF membrane dope, the carrying out practically time is 50～
160min, enter pressure be 19～21Bar, go out pressure be 19～21Bar, mean temperature be 23～27 DEG C, average flux be 30～
41LMH, cycles of concentration is 12～25 times, and the concrete test parameters of the step is as shown in table 5：
The NF membrane experimental result of table 5 collects
Remarks：Batch 1 and batch 4 are less due to feed volume, and equipment entity product is larger, and cycles of concentration is relatively low.
It is can be found that by upper table 5：From the rolling organic nanofiltration membrane filtration Ultrafiltration film permeate of 200 molecular weight, enter mould
Power 20Bar, 24 DEG C of mean temperature, between 30～40LMH, the rate of filtration is fast, and cycles of concentration can reach 20 times for membrane flux.
The testing result of NF membrane permeate and NF membrane dope is as shown in table 6：
The NF membrane experimental test data of table 6
It is can be found that by upper table 6：NF membrane of the milipore filter permeate through 200 molecular weight is concentrated, permeate VB2 content
In below 80mg/L, rejection close 99%, it is possible to achieve the purpose of desalination.Finally the dope of nanofiltration is adjusted into PH to neutrality,
VB2 can be allowed to crystallize again.The dope of PH will be mixed up again through ceramic membrane, that is, reached the purpose for reclaiming VB2.Through three road films
Separating technology, not only can reach the purpose for reclaiming VB2, realize waste recovery, and the purpose for reclaiming NaCl can be reached again, mitigate factory
Area's environmental protection pressure, reduces 20 times of quantity of wastewater effluent in workshop, reduces production cost；
The core rod variations of flux of NF membrane is as shown in Figure 3.By Fig. 3 it can be found that：Batch 1～6 meets the change of film core operation
Change trend.With the carrying out of filtration experiment, film core is constantly contaminated, flux rapid decrease；In addition, clear liquid constantly passes through film,
Dope is stayed in membranous system and constantly circulated, and concentration is constantly raised, and the solution concentration the closer to film surface is higher, and concentration extreme differenceization is not
It is disconnected to increase, clear liquid is increased toward the migration difficulty on film surface, membrane flux can slowly decline.The last flux of six batch NF membranes is all
In 35LMH or so, the rolling organic nanofiltration membrane for illustrating 200nm processes having good stability for VB2 solution membrane fluxs, is adapted to industry fortune
OK；
(6) by the crystallized process of NF membrane permeate, NaCl is obtained；
(7) NF membrane dope is adjusted into pH to neutrality, return to step (1) carries out filtration treatment, then sequentially passes through step
Suddenly (2) to (6), further to obtain VB2 and NaCl；
(8) ceramic membrane is cleaned with 1%NaOH solution, 40～60min of scavenging period, cleaning temperature is 50～60
DEG C, the flux for making ceramic membrane recovers completely；
(9) the organic milipore filter of rolling is cleaned with LC90# cleaning agents, scavenging period be 40～60min, cleaning temperature
For room temperature, the flux for making the organic milipore filter of rolling recovers completely；
(10) rolling organic nanofiltration membrane is cleaned with LC90# cleaning agents, scavenging period is 40～60min, cleaning is warm
Spend for room temperature, the flux for making rolling organic nanofiltration membrane recovers completely
The above, only presently preferred embodiments of the present invention, therefore can not according to this limit the scope of present invention enforcement, i.e.,
The equivalence changes made according to the scope of the claims of the present invention and description and modification, all should still belong in the range of the present invention covers.
Claims (7)
1. a kind of separation and concentration method of VB2 crystalline mother solutions, it is characterised in that：20～35 DEG C of the temperature of the VB2 crystalline mother solutions, pH
For 4～5, the close water of viscosity, and the VB2 crystalline mother solutions mix to obtain solid-liquid system, its clear liquid for saturation VB2 solution with crystal
In, the content of VB2 is 500～2000mg/L, and in its system, the content of VB2 is 1700～1900mg/L, and the content of NaCl is
8%～10%, comprise the steps：
(1) VB2 crystalline mother solutions are carried out into filtration treatment by 80～120nm ceramic membranes, obtains ceramic membrane permeate and ceramic membrane is dense
Liquid, 70～110min of carrying out practically time, enter pressure be 2.8～3.2Bar, go out pressure be 1.8～2.2Bar, mean temperature be 23～
27 DEG C, average flux is 330～540LMH, and cycles of concentration is 10～32 times；
(2) the crystallized process of ceramic membrane dope is obtained into VB2；
(3) ceramic membrane permeate is adjusted after pH to 9～10, by the organic ultrafiltration of the rolling of 1800～2200 molecular weight with NaOH
Film carries out filtering and impurity removing process, obtains milipore filter permeate and milipore filter dope, and the carrying out practically time is 60～240min, and entering pressure is
17～19Bar, it is 17～18Bar to go out pressure, and mean temperature is 23～28 DEG C, and average flux is 20～55LMH, and cycles of concentration is 20
～37 times；
(4) milipore filter dope is carried out into emission treatment；
(5) milipore filter permeate is carried out into filtration treatment by the rolling organic nanofiltration membrane of molecular weight 180～220, obtains NF membrane
Permeate and NF membrane dope, the carrying out practically time is 50～160min, and it is 19～21Bar to enter pressure, and it is 19～21Bar to go out pressure,
Mean temperature is 23～27 DEG C, and average flux is 30～41LMH, and cycles of concentration is 12～25 times；
(6) by the crystallized process of NF membrane permeate, NaCl is obtained；
(7) NF membrane dope is adjusted after pH to 4～5, return to step (1) carries out filtration treatment, then sequentially passes through step (2)
To (6), further to obtain VB2 and NaCl.
2. separation and concentration method as claimed in claim 1, it is characterised in that：The step (1) is：VB2 crystalline mother solutions are led to
Crossing 100nm ceramic membranes carries out filtration treatment, obtains ceramic membrane permeate and ceramic membrane dope.
3. separation and concentration method as claimed in claim 1, it is characterised in that：The step (3) is：Ceramic membrane permeate is used
NaOH is adjusted after pH to 9～10, and by the organic milipore filter of the rolling of 2000 molecular weight filtering and impurity removing process is carried out, and obtains milipore filter saturating
Cross liquid and milipore filter dope.
4. separation and concentration method as claimed in claim 1, it is characterised in that：The step (5) is：Milipore filter permeate is led to
Crossing the rolling organic nanofiltration membrane of 200nm carries out filtration treatment, obtains NF membrane permeate and NF membrane dope.
5. separation and concentration method as claimed in claim 1, it is characterised in that：Also include step (8)：With 1%NaOH solution pair
Ceramic membrane is cleaned, 40～60min of scavenging period, and cleaning temperature is 50～60 DEG C, and the flux for making ceramic membrane recovers completely.
6. separation and concentration method as claimed in claim 1, it is characterised in that：Also include step (9)：With LC90# cleaning agents pair
The organic milipore filter of rolling is cleaned, and scavenging period is 40～60min, and cleaning temperature is room temperature, makes the organic milipore filter of rolling
Flux recovers completely.
7. separation and concentration method as claimed in claim 1, it is characterised in that：Also include step (10)：With LC90# cleaning agents pair
Rolling organic nanofiltration membrane is cleaned, and scavenging period is 40～60min, and cleaning temperature is room temperature, makes rolling organic nanofiltration membrane
Flux recovers completely.
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| CN106587408B (en) | 2019-11-05 |
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