CN108503570A - The technique that electroosmose process substitutes centrifugation exchange process extraction L- hydroxyl prolines - Google Patents
The technique that electroosmose process substitutes centrifugation exchange process extraction L- hydroxyl prolines Download PDFInfo
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- CN108503570A CN108503570A CN201810227124.1A CN201810227124A CN108503570A CN 108503570 A CN108503570 A CN 108503570A CN 201810227124 A CN201810227124 A CN 201810227124A CN 108503570 A CN108503570 A CN 108503570A
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- electrodialysis
- ultrafiltration
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D207/00—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom
- C07D207/02—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom
- C07D207/04—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members
- C07D207/10—Heterocyclic compounds containing five-membered rings not condensed with other rings, with one nitrogen atom as the only ring hetero atom with only hydrogen or carbon atoms directly attached to the ring nitrogen atom having no double bonds between ring members or between ring members and non-ring members with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D207/16—Carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals
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Abstract
The present invention relates to a kind of electroosmose process to substitute the technique that centrifugation exchange process extracts L hydroxyl prolines, includes the following steps：1) ultrafiltration；2) electrodialysis：Ultrafiltrate is pumped into electrodialysis fresh water room, open electrodialysis feed pump, adjust flow, flow is controlled between 4000L~6000L/h, make three cell pressures substantially close to, by voltage, electric current is transferred to minimum, power module selects constant voltage mode, voltage is adjusted to 160V, electric current can slowly rise in the gradual transition process of salt amount, after electric current reaches 10A, power supply is closed, power module selects constant current mode, then it turns on the power switch and allows voltage gradually toward decline, when equal desalinations are close to terminal, voltage can gradually go up, it cuts off the power when being raised to 160V, switch to constant voltage mode, it continues to run with, material conductance to be run is down to≤3000us/cm from 35000~50000us/cm of starting；3) it concentrates；4) it decolourizes；5) condensing crystallizing；6) it centrifuges；7) dry.
Description
Technical field
The invention belongs to biochemical industry production fields, are related to industrialization extraction L- hydroxyl proline zymotic fluids, and in particular to one
The technique that kind electroosmose process substitutes centrifugation exchange process extraction L- hydroxyl prolines.
Background technology
Referring to Fig.1, existing industrialization extraction L- hydroxyl proline zymotic fluids use the technique of ion exchange column technical solution,
The ion exchange of this technique is that target product is adsorbed when material passes through resin, then goes a target by weak aqua ammonia again
Product parses, and this technique one is that the operating time is long, second is that ammonium hydroxide (being recycled later to ammonium hydroxide) is used, ammonium hydroxide
The consumption energy is compared in recycling, third, the cleaning and activation of resin need to consume a large amount of water, relatively low so as to cause yield, wastewater flow rate is big
The shortcomings that.
Invention content
It is an object of the present invention to provide a kind of electroosmose process to substitute the technique that centrifugation exchange process extracts L- hydroxyl prolines, saves
Energy consumption reduces cost, substantially reduces the extracting cycle of zymotic fluid, improves extract yield.
In order to achieve the goal above, the technical solution adopted by the present invention is：A kind of electroosmose process substitutes centrifugation exchange process and carries
The technique for taking L- hydroxyl prolines, includes the following steps：
1) ultrafiltration：Film device is opened to L- hydroxyl proline zymotic fluid ultrafiltration, after ultrafiltration Membrane cleaning qualification to carry out zymotic fluid
Filtering, 35~40 DEG C of ultrafiltrate temperature enter film pressure≤0.3Mpa, and front and back pressure difference control is in 0.1Mpa, 60~80L/m of flow velocity2/ small
When, early period is filtered using infinite reflux formula, switches discharging after filtrate clarification, the later stage is washed in trapped fluid with water top to target product content
Terminate ultrafiltration below 0.02%；
2) electrodialysis：Ultrafiltrate is pumped into electrodialysis fresh water room, opens electrodialysis feed pump, adjusts flow, and control flow exists
Between 4000L~6000L/h, make three cell pressures substantially close to voltage, electric current being transferred to minimum, power module selection is permanent
Die pressing type adjusts voltage to 160V, and electric current can slowly rise in the gradual transition process of salt amount, after electric current reaches 10A, by power supply
It closes, power module selects constant current mode, then turns on the power switch and allows voltage gradually toward decline, when waiting desalinations close to terminal,
Voltage can gradually go up, and cut off the power when being raised to 160V, switch to constant voltage mode, continue to run with, and material conductance to be run is from
35000~the 50000us/cm to begin is down to≤3000us/cm；
3) it concentrates：Electrodialysis filtered fluid is squeezed into concentrator and is concentrated, concentration process uses negative-pressure operation, vacuum
Degree is maintained within 10Kpa, and temperature of charge≤80 DEG C terminate to concentrate when concentration volume reaches 4~5 times；
4) it decolourizes：769 activated carbons are added by the 0.5% of concentration volume, decolourize 30min at a temperature of 60 DEG C, except carbon filters；
5) condensing crystallizing：Destainer continues after being concentrated into 1~2 times of cycles of concentration volume, and chuck leads to chilled water and cools down rapidly
To 0 DEG C~10 DEG C, 60 revs/min of growing the grain 4h ± 1h of stirring or so are opened；
6) it centrifuges：Growing the grain liquid is transferred to centrifuge drying, a small amount of ice water elution；
7) dry：Wet crystal is entered 80 degrees Celsius of double cone dryer to be dried in vacuo 4~6 hours.
Further, in step 1) to L- hydroxyl proline zymotic fluid ultrafiltration, film device pair is opened after ultrafiltration Membrane cleaning qualification
Zymotic fluid is filtered, 40 DEG C of ultrafiltrate temperature, enters film pressure 0.3Mpa, front and back pressure difference control is in 0.1Mpa, 60~80L/ of flow velocity
m2/ hour, early period are filtered using infinite reflux formula, switch discharging after filtrate clarification, and the later stage is washed in trapped fluid with water top and produced to target
Object content terminates ultrafiltration below 0.02%.
The technical effects of the invention are that：The present invention provides a kind of work of extraction bioanalysis fermentation L- hydroxyl proline zymotic fluids
Skill industrializes extraction L- hydroxyl proline zymotic fluids using the process, substantially increases the extract yield of L- hydroxyl prolines, carry
Product quality has been risen, has reduced production cost, while drastically reducing sewage pollution.
Present invention process method utilizes electrodialytic technique scheme instead of the ion exchange column technical solution in former technique, originally
Invented technology technical solution is by amberplex material to reach desalination purpose using electrodialysis, need not be disappeared halfway
Any chemicals is consumed, the equipment needed is simple, easy to operate, while considerably reducing its wastewater flow rate, the waste water generated
Amount only has 1/6th of former technique ion exchange column；The extracting cycle for substantially reducing zymotic fluid, improves extract yield.
Description of the drawings
Fig. 1 is the technological process that L- hydroxyl proline zymotic fluids are extracted in existing industrialization；
Fig. 2 is the technological process of the present invention.
Specific implementation mode
With reference to attached drawing, the detailed process of technique of the invention：
(1) it extracts, extraction includes the following steps successively：Zymotic fluid flocculates first, and zymotic fluid storage tank clamping sleeve is heated to 80 DEG C
± 1 DEG C and temperature 30min is maintained, then is cooled to 35~40 DEG C；With pump squeeze into membrane molecule amount be 1000 ceramic membrane to flocculation
Material is filtered, and ceramic film pressure≤0.3Mpa, front and back pressure difference is maintained at 0.1Mpa or so, and ceramic membrane filtration liquid is pumped into electric osmose
Analysis carries out desalination, opens electrodialysis feed pump, adjusts flow, and control flow makes three compartments between 4000L~6000L/h
Pressure by voltage, electric current substantially close to being transferred to minimum, power module selects constant voltage mode, adjusts voltage to 160V, salt amount is gradual
Electric current can slowly rise in transition process, and after electric current reaches 10A, power supply is closed, and power module selects constant current mode, then
It turns on the power switch and allows voltage gradually toward declining, when waiting desalinations close to terminal, voltage can gradually go up, cut-out electricity when being raised to 160V
Source switches to constant voltage mode, continues to run with, material conductance to be run to≤3000us/cm, end operation；
(2) electrodialysis filtered fluid is squeezed into concentrator and is concentrated, concentration process uses negative-pressure operation, vacuum degree to protect
It holds within 10Kpa, temperature of charge≤80 DEG C, terminates to concentrate when concentration volume reaches 4~5 times；
(3) 769 activated carbons are added in press concentration volume 0.5%, and decolourize 30min at a temperature of 60 DEG C, except carbon filters；
(4) destainer is continued after being concentrated into 1~2 times of cycles of concentration volume, chuck lead to chilled water be cooled to rapidly 0 DEG C~
10 DEG C, 60 revs/min of growing the grain 4h ± 1h of stirring or so are opened, growing the grain liquid is transferred to centrifuge drying, a small amount of ice water elution；
(5) wet crystal is entered into 80 degrees Celsius of vacuum drying of double cone dryer and obtains L- hydroxy-proline fine work in 4~6 hours.
Above-mentioned new process simplifies operating procedure than prior art, to save energy consumption, reduces cost, improves receipts
Rate.
Above-mentioned new process reduces a large amount of waste water (only 1/6th of prior art wastewater flow rate) than prior art, from
And reduce processing cost, avoid environmental pollution.
Embodiment：
1., first to L- hydroxyl proline zymotic fluid ultrafiltration, film device is opened after ultrafiltration Membrane cleaning qualification, zymotic fluid is carried out
Filtering, 40 DEG C of ultrafiltrate temperature enter film pressure 0.3Mpa, and front and back pressure difference control is in 0.1Mpa, 60~80L/m of flow velocity2It is/hour, preceding
Phase is filtered using infinite reflux formula, switches discharging after filtrate clarification, the later stage is washed with water top in trapped fluid to exist to target product content
0.02% or less terminates ultrafiltration；
2., ultrafiltrate be pumped into electrodialysis fresh water room, open electrodialysis feed pump, adjust flow, control flow 4000L~
Between 6000L/h, make three cell pressures substantially close to, voltage, electric current are transferred to minimum, power module selects constant voltage mode,
Voltage is adjusted to 160V, electric current can slowly rise in the gradual transition process of salt amount, and after electric current reaches 10A, power supply is closed, electricity
Source module selects constant current mode, then turns on the power switch and allows voltage gradually toward declining, when waiting desalinations close to terminal, voltage can be by
Step is gone up, and is cut off the power when being raised to 160V, is switched to constant voltage mode, continues to run with, and material conductance to be run is from the 35000 of starting
~50000us/cm is down to≤3000us/cm；
3., electrodialysis filtered fluid squeezed into concentrator concentrate, concentration process uses negative-pressure operation, vacuum degree to protect
It holds within 10Kpa, temperature of charge≤80 DEG C, terminates to concentrate when concentration volume reaches 4~5 times；
4., by concentration volume 0.5% be added 769 activated carbons, decolourize 30min at a temperature of 60 DEG C, except carbon filter.
5. destainer is continued after being concentrated into 1~2 times of cycles of concentration volume, chuck lead to chilled water be cooled to rapidly 0 DEG C~
10 DEG C, 60 revs/min of growing the grain 4h ± 1h of stirring or so are opened, growing the grain liquid is transferred to centrifuge drying, a small amount of ice water elution；
6. wet crystal, which is entered 80 degrees Celsius of vacuum drying of double cone dryer, obtains L- hydroxy-proline fine work in 4~6 hours.
Claims (2)
1. the technique that electroosmose process substitutes centrifugation exchange process extraction L- hydroxyl prolines, which is characterized in that include the following steps：
1) ultrafiltration：Film device is opened to L- hydroxyl proline zymotic fluid ultrafiltration, after ultrafiltration Membrane cleaning qualification to be filtered zymotic fluid,
35~40 DEG C of ultrafiltrate temperature enters film pressure≤0.3Mpa, and front and back pressure difference control is in 0.1Mpa, 60~80L/m of flow velocity2It is/hour, preceding
Phase is filtered using infinite reflux formula, switches discharging after filtrate clarification, the later stage is washed with water top in trapped fluid to exist to target product content
0.02% or less terminates ultrafiltration；
2) electrodialysis：Ultrafiltrate is pumped into electrodialysis fresh water room, opens electrodialysis feed pump, adjusts flow, control flow is in 4000L
Between~6000L/h, make three cell pressures substantially close to voltage, electric current being transferred to minimum, power module selects constant pressure mould
Formula adjusts voltage to 160V, and electric current can slowly rise in the gradual transition process of salt amount, and after electric current reaches 10A, power supply is closed
It closing, power module selects constant current mode, then turns on the power switch and allows voltage gradually toward decline, when waiting desalinations close to terminal, electricity
Pressure can gradually go up, and cut off the power when being raised to 160V, switch to constant voltage mode, continue to run with, and material conductance to be run is from starting
35000~50000us/cm be down to≤3000us/cm；
3) it concentrates：Electrodialysis filtered fluid is squeezed into concentrator and is concentrated, concentration process uses negative-pressure operation, vacuum degree to protect
It holds within 10Kpa, temperature of charge≤80 DEG C, terminates to concentrate when concentration volume reaches 4~5 times；
4) it decolourizes：769 activated carbons are added by the 0.5% of concentration volume, decolourize 30min at a temperature of 60 DEG C, except carbon filters；
5) condensing crystallizing：Destainer continues after being concentrated into 1~2 times of cycles of concentration volume, and chuck leads to chilled water and is cooled to 0 DEG C rapidly
~10 DEG C, open 60 revs/min of growing the grain 4h ± 1h of stirring or so；
6) it centrifuges：Growing the grain liquid is transferred to centrifuge drying, a small amount of ice water elution；
7) dry：Wet crystal is entered 80 degrees Celsius of double cone dryer to be dried in vacuo 4~6 hours.
2. electroosmose process according to claim 1 substitutes the technique of centrifugation exchange process extraction L- hydroxyl prolines, feature exists
In, it opens film device to L- hydroxyl proline zymotic fluid ultrafiltration in step 1), after ultrafiltration Membrane cleaning qualification and zymotic fluid is filtered,
40 DEG C of ultrafiltrate temperature enters film pressure 0.3Mpa, and front and back pressure difference control is in 0.1Mpa, 60~80L/m of flow velocity2/ hour, early period use
Infinite reflux formula filter, filtrate clarification after switch discharging, the later stage with water top wash in trapped fluid to target product content 0.02% with
Lower end ultrafiltration.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810227124.1A CN108503570A (en) | 2018-03-20 | 2018-03-20 | The technique that electroosmose process substitutes centrifugation exchange process extraction L- hydroxyl prolines |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810227124.1A CN108503570A (en) | 2018-03-20 | 2018-03-20 | The technique that electroosmose process substitutes centrifugation exchange process extraction L- hydroxyl prolines |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105837488A (en) * | 2016-03-31 | 2016-08-10 | 天津市敬业精细化工有限公司 | Hydroxyproline fermentation production technology |
| CN107513030A (en) * | 2017-10-19 | 2017-12-26 | 福建师范大学 | A kind of method that L hydroxyprolines are isolated and purified in the hydroxyproline zymotic fluid from L |
-
2018
- 2018-03-20 CN CN201810227124.1A patent/CN108503570A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105837488A (en) * | 2016-03-31 | 2016-08-10 | 天津市敬业精细化工有限公司 | Hydroxyproline fermentation production technology |
| CN107513030A (en) * | 2017-10-19 | 2017-12-26 | 福建师范大学 | A kind of method that L hydroxyprolines are isolated and purified in the hydroxyproline zymotic fluid from L |
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