CN115057901A - Nucleoside purification system and purification process - Google Patents
Nucleoside purification system and purification process Download PDFInfo
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- CN115057901A CN115057901A CN202210822467.9A CN202210822467A CN115057901A CN 115057901 A CN115057901 A CN 115057901A CN 202210822467 A CN202210822467 A CN 202210822467A CN 115057901 A CN115057901 A CN 115057901A
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- 239000002777 nucleoside Substances 0.000 title claims abstract description 52
- 150000003833 nucleoside derivatives Chemical class 0.000 title claims abstract description 52
- 238000000746 purification Methods 0.000 title claims abstract description 31
- 239000011347 resin Substances 0.000 claims abstract description 311
- 229920005989 resin Polymers 0.000 claims abstract description 311
- 230000008929 regeneration Effects 0.000 claims abstract description 99
- 238000011069 regeneration method Methods 0.000 claims abstract description 99
- 238000005406 washing Methods 0.000 claims abstract description 89
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 80
- 238000005342 ion exchange Methods 0.000 claims abstract description 46
- 238000004140 cleaning Methods 0.000 claims abstract description 40
- 239000000463 material Substances 0.000 claims abstract description 38
- 238000010612 desalination reaction Methods 0.000 claims abstract description 37
- 238000001914 filtration Methods 0.000 claims abstract description 21
- 238000002425 crystallisation Methods 0.000 claims abstract description 15
- 230000008025 crystallization Effects 0.000 claims abstract description 15
- 238000005349 anion exchange Methods 0.000 claims abstract description 10
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000011033 desalting Methods 0.000 claims abstract description 9
- 238000005341 cation exchange Methods 0.000 claims abstract description 8
- 238000000605 extraction Methods 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims description 99
- 150000001768 cations Chemical class 0.000 claims description 45
- 239000002253 acid Substances 0.000 claims description 43
- 239000003513 alkali Substances 0.000 claims description 43
- 150000001450 anions Chemical class 0.000 claims description 38
- 239000012528 membrane Substances 0.000 claims description 29
- 239000002994 raw material Substances 0.000 claims description 15
- 239000000919 ceramic Substances 0.000 claims description 14
- 238000000108 ultra-filtration Methods 0.000 claims description 13
- 239000002699 waste material Substances 0.000 claims description 12
- 238000006386 neutralization reaction Methods 0.000 claims description 11
- 238000004064 recycling Methods 0.000 claims description 11
- 238000001223 reverse osmosis Methods 0.000 claims description 11
- 239000012535 impurity Substances 0.000 claims description 10
- 238000000034 method Methods 0.000 claims description 7
- 238000000855 fermentation Methods 0.000 claims description 4
- 230000004151 fermentation Effects 0.000 claims description 4
- 238000000502 dialysis Methods 0.000 claims description 3
- 238000001704 evaporation Methods 0.000 claims description 3
- 230000008020 evaporation Effects 0.000 claims description 3
- 239000002351 wastewater Substances 0.000 abstract description 11
- 238000004519 manufacturing process Methods 0.000 abstract description 8
- 239000000126 substance Substances 0.000 abstract description 6
- 238000004090 dissolution Methods 0.000 abstract description 3
- 239000012492 regenerant Substances 0.000 description 18
- 102000004169 proteins and genes Human genes 0.000 description 4
- 108090000623 proteins and genes Proteins 0.000 description 4
- 150000003839 salts Chemical class 0.000 description 3
- 229920006395 saturated elastomer Polymers 0.000 description 3
- 241001052560 Thallis Species 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000001963 growth medium Substances 0.000 description 1
- 239000003456 ion exchange resin Substances 0.000 description 1
- 229920003303 ion-exchange polymer Polymers 0.000 description 1
- 230000003472 neutralizing effect Effects 0.000 description 1
- 238000011027 product recovery Methods 0.000 description 1
- 230000001172 regenerating effect Effects 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000001360 synchronised effect Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H19/00—Compounds containing a hetero ring sharing one ring hetero atom with a saccharide radical; Nucleosides; Mononucleotides; Anhydro-derivatives thereof
- C07H19/02—Compounds containing a hetero ring sharing one ring hetero atom with a saccharide radical; Nucleosides; Mononucleotides; Anhydro-derivatives thereof sharing nitrogen
- C07H19/04—Heterocyclic radicals containing only nitrogen atoms as ring hetero atom
- C07H19/06—Pyrimidine radicals
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H1/00—Processes for the preparation of sugar derivatives
- C07H1/06—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07H—SUGARS; DERIVATIVES THEREOF; NUCLEOSIDES; NUCLEOTIDES; NUCLEIC ACIDS
- C07H19/00—Compounds containing a hetero ring sharing one ring hetero atom with a saccharide radical; Nucleosides; Mononucleotides; Anhydro-derivatives thereof
- C07H19/02—Compounds containing a hetero ring sharing one ring hetero atom with a saccharide radical; Nucleosides; Mononucleotides; Anhydro-derivatives thereof sharing nitrogen
- C07H19/04—Heterocyclic radicals containing only nitrogen atoms as ring hetero atom
- C07H19/16—Purine radicals
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Biochemistry (AREA)
- Biotechnology (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Molecular Biology (AREA)
- Treatment Of Water By Ion Exchange (AREA)
Abstract
The invention relates to the field of ion exchange, and discloses a nucleoside purification system which comprises a filtration system, a continuous ion exchange desalination system, a concentration system and a crystallization drying device which are sequentially connected. The continuous ion exchange desalting system comprises a material washing area, a material feeding area, a water topping area, a cleaning area and a regeneration area which are connected in sequence. The feeding zone, the washing zone, the top water zone, the washing zone and the regeneration zone comprise a rotary switching valve, a cation exchange system and an anion exchange system. The continuous ion-exchange desalting system optimizes and integrates the anion-cation ion-exchange system, reduces the occupied area and simultaneously makes the system more concise and convenient. The resin units in each zone are improved through connection, and the flow is shortened. The invention also discloses a nucleoside purification process, which adopts the nucleoside purification system and comprises the following steps: s1, extraction, S2, purification, S3, concentration, S4 and crystallization. The invention not only can improve the production efficiency and the nucleoside dissolution purity, but also can effectively save the use of chemicals and reduce the discharge of waste water.
Description
Technical Field
The invention relates to the field of ion exchange, in particular to a nucleoside purification system and a nucleoside purification process.
Background
A large amount of salt-containing wastewater is generated in the existing purification process of nucleoside, the treatment difficulty is high, and the environmental protection pressure is large. In the ion exchange desalination process, the application of various ion exchange resins to one set of system cannot be realized, and the production efficiency is low.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, and provides a nucleoside purification system which can improve the production efficiency and the nucleoside dissolution purity, effectively save the use of chemicals and reduce the discharge of waste water.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention discloses a nucleoside purification system, which comprises a filtration system, a continuous ion exchange desalination system, a concentration system and a crystallization drying device which are connected in sequence.
The continuous ion-exchange desalination system comprises a material washing area, a feeding area, a water topping area, a cleaning area and a regeneration area which are connected in sequence. The feeding zone, the washing zone, the top water zone, the washing zone and the regeneration zone respectively comprise a rotary switching valve, a cation exchange system consisting of a plurality of cation resin units and an anion exchange system consisting of a plurality of anion resin units.
The male resin unit and the female resin unit are distributed in an up-down symmetrical mode and are connected with the rotary switching valve. The flow direction of the liquid in the male resin unit and the female resin unit is opposite to the rotation direction thereof.
The regeneration zone comprises a thorough regeneration zone and a pre-regeneration zone which are connected in sequence.
And the positive resin unit and the negative resin unit in the complete regeneration zone are connected in series in an opposite direction. The positive resin units and the negative resin units in the pre-regeneration zone are connected in series in a reverse manner after being connected in parallel pairwise.
Further, the filtering system comprises a ceramic membrane filtering system and an ultrafiltration membrane impurity removal system; the ceramic membrane filtering system comprises a ceramic mold core, and the aperture of the ceramic mold core is 40nm-50 nm; the ultrafiltration membrane impurity removal system comprises a hollow ultrafiltration membrane and a roll-type ultrafiltration membrane.
Furthermore, the concentration system adopts a reverse osmosis membrane concentration system, and dialysate of the reverse osmosis membrane concentration system is connected with a cleaning area of the continuous ion-exchange desalination system through a dialysis tube.
Further, the regeneration zone also comprises a waste acid and alkali neutralization tank; the thorough regeneration zone comprises a first male resin unit regeneration zone and a first female resin unit regeneration zone; the pre-regeneration zone comprises a second male resin unit regeneration zone and a second female resin unit regeneration zone.
The dilute acid liquid flows into the first cation resin unit regeneration area for complete regeneration, the discharge liquid of the dilute acid liquid is mixed with the discharge liquid of the cation resin unit cleaning area of the cleaning area and then flows into the second cation resin unit regeneration area for pre-regeneration, and the discharge liquid of the dilute acid liquid flows into a waste acid alkali neutralization tank.
The dilute alkali liquor flows into the first negative resin unit regeneration area for complete regeneration, the discharge liquid of the dilute alkali liquor is mixed with the discharge liquid of the negative resin unit cleaning area of the cleaning area and then flows into the second negative resin unit regeneration area for pre-regeneration, and the discharge liquid of the dilute alkali liquor flows into a waste acid alkali neutralization tank.
Further, the material washing area comprises a male resin unit material washing area, a female resin unit material washing area and a material washing tank.
Pure water flows into a positive resin unit material washing area and a negative resin unit material washing area respectively, liquid outlets of the two areas are mixed and connected into a material washing tank, and resin units in the positive resin unit material washing area and the negative resin unit material washing area are connected in series in a forward direction.
Further, the feed zones include a first male resin unit feed zone, a first female resin unit feed zone, a second male resin unit feed zone, a second female resin unit feed zone, a third male resin unit feed zone, a third female resin unit feed zone, and a product tank.
The raw material flows into a first cation resin unit feeding area and a first anion resin unit feeding area in sequence for primary ion exchange desalination, the discharge liquid of the raw material is mixed with the discharge liquid of a washing area and flows into a second cation resin unit feeding area and a second anion resin unit feeding area in sequence for secondary ion exchange desalination, the discharge liquid of the raw material flows into a third cation resin unit feeding area and a third anion resin unit feeding area in sequence for third ion exchange desalination, and the final discharge liquid flows into a product tank.
The resin units among the feeding areas of the first male resin units, the resin units among the feeding areas of the first female resin units, the resin units among the feeding areas of the second male resin units, the resin units among the feeding areas of the second female resin units, the resin units among the feeding areas of the third male resin units and the resin units among the feeding areas of the third female resin units are connected in parallel in the forward direction.
Further, the top water area comprises a top water positive resin unit, a top water negative resin unit and a reuse water tank; the liquid outlet of the feeding area is communicated with the recycling water tank after being connected with the water-ejecting positive resin unit and the water-ejecting negative resin unit in a reverse series mode.
The cleaning area comprises a male resin unit cleaning area and a female resin unit cleaning area; a first liquid outlet of the reuse water tank is connected with the cation resin unit cleaning area, and the discharged cleaning liquid flows back to be mixed with the discharged liquid of the first cation resin unit regeneration area; and a second liquid outlet of the reuse water tank is connected with the anion resin unit cleaning area, and the discharged cleaning liquid flows back to be mixed with the discharged liquid of the first anion resin unit regeneration area.
Wherein the resin units in the male resin unit washing zone and the resin units in the female resin unit washing zone are connected in series in an inverted manner.
The invention also discloses a nucleoside purification process, which adopts the nucleoside purification system and comprises the following steps:
s1, extraction: coarsely filtering the fermentation liquor to remove macromolecular impurities to obtain a primary clarified liquor; fine filtering the first-stage clarified liquid to remove organic matters to obtain a second-stage clarified liquid;
s2, purification: carrying out continuous ion exchange on the secondary clarified liquid, and carrying out desalination treatment to obtain a purified liquid;
s3, concentration: carrying out reverse osmosis concentration on the purified solution to remove redundant water, so as to obtain concentrated solution and dialyzate;
s4, crystallization: and (4) carrying out evaporation concentration, crystallization and drying on the concentrated solution to obtain the product.
Further, the conductivity of the first-stage clarified liquid is 5000 us/cm-15000 us/cm, the pH is 3.0-4.0, and the content of nucleoside is 1.0-2.0%; the conductivity of the secondary clarified liquid is 3000-15000us/cm, the pH value is 3.0-4.0, and the nucleoside content is 0.5-2.0%.
Further, the purified solution has a conductivity of less than 20us/cm, a pH of 6.8-8.0, and a nucleoside content of about 0.5-1.5%; the purity of the nucleoside in the nucleoside solution is more than 99 percent; the nucleoside content of the concentrated solution is 6.0-8.0%, and the dialyzate is returned to the continuous ion exchange system for recycling.
The invention has the advantages that:
1. the invention can replace the traditional nucleoside production process, changes the traditional manual operation into automatic production, shortens the flow through reasonable procedures and design, not only improves the product precision, but also greatly improves the production efficiency.
2. The continuous ion exchange desalination system optimizes and integrates two sets of different ion exchange processes, reduces equipment investment, reduces occupied area and simultaneously makes the system more concise and convenient.
3. The continuous ion-exchange desalination system fully and effectively recycles residual raw materials, reuse water and regenerant, effectively saves the use of the regenerant, reduces the discharge of waste water, reduces the content of residual chemicals in the waste water, and saves the water consumption.
Drawings
FIG. 1 is a process flow diagram of the present invention.
FIG. 2 is a schematic diagram of the continuous ion-exchange desalination system of the present invention.
Description of the main component symbols:
1. a material washing area 11, a pure water tank 12, a positive resin unit material washing area 13, a negative resin unit material washing area 14 and a material washing tank;
2. a feed zone, 21, a raw material tank, 22, a first male resin unit feed zone, 23, a first female resin unit feed zone, 24, a second male resin unit feed zone, 25, a second female resin unit feed zone, 26, an intermediate feed tank, 27, a third male resin unit feed zone, 28, a third female resin unit feed zone, 29, a product tank;
3. a top water area 31, a top water positive resin unit 32, a top water negative resin unit 33 and a reuse water tank;
4. a washing zone, 41, a male resin unit washing zone, 42, a female resin unit washing zone;
5. a regeneration zone, 51, a dilute acid tank, 52, a first cation resin unit regeneration zone, 53, an acid applying tank, 54, a second cation resin unit regeneration zone, 55, a dilute alkali tank, 56, a first anion resin unit regeneration zone, 57, an alkali applying tank, 58, a second anion resin unit regeneration zone, 59, and a waste acid alkali neutralization tank;
6. a cationic cross-linking system;
7. anion exchange system.
100. A filtering system, 101, a ceramic membrane filtering system; 102. an ultrafiltration membrane impurity removal system;
200. a continuous ion-exchange desalination system;
300. a concentration system;
400. crystallization drying device.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
As shown in FIGS. 1 to 2, the present invention discloses a nucleoside purification system, which comprises a filtration system 100, a continuous ion-exchange desalination system 200, a concentration system 300, and a crystallization drying device 400, which are connected in sequence.
Wherein the filtering system 100 comprises a ceramic membrane filtering system and an ultrafiltration membrane impurity removal system. The ceramic membrane filtering system comprises a ceramic mold core, the aperture of the ceramic mold core is 40nm-50nm, and the ceramic mold core can filter the fermentation liquor to remove suspended matters such as culture medium and the like, thalli, macromolecular protein and the like in the nucleoside solution. The ultrafiltration membrane impurity removal system comprises a hollow ultrafiltration membrane and a roll-type ultrafiltration membrane. Can remove organic matters such as protein, pigment, etc.
The continuous ion-exchange desalination system 200 comprises a washing zone 1, a feeding zone 2, a top water zone 3, a washing zone 4 and a regeneration zone 5 which are connected in sequence. The feeding zone 1, the washing zone 2, the top water zone 3, the washing zone 4 and the regeneration zone 5 respectively comprise a rotary switching valve, a cation exchange system 6 consisting of a plurality of cation resin units and an anion exchange system 7 consisting of a plurality of anion resin units.
The male resin unit and the female resin unit are distributed up and down symmetrically and are connected by a rotary switching valve. The rotary switching valve comprises an upper valve core and a lower valve core which are connected with two ends of a resin unit, the resin unit can rotate relative to the rotary switching valve, and the flowing direction of liquid in the male resin unit and the female resin unit is opposite to the rotating direction of the male resin unit and the female resin unit. The system steps one resin unit position each time, the cation exchange system 6 and the anion exchange system 7 step at the same time, and the two systems can run synchronously. Not only improves the product precision, but also greatly improves the production efficiency.
The concentration system 300 adopts a reverse osmosis membrane concentration system, nucleoside is intercepted by a reverse osmosis membrane, water passes through a membrane layer, and dialysate is formed and discharged, so that the aim of circular concentration is fulfilled. The dialysate of the reverse osmosis membrane concentration system 300 is connected with the cleaning zone of the continuous ion-exchange desalination system 200 through a dialysis tube, and is used for cleaning the resin unit for recycling.
Wherein, the crystallization drying device 400 may be a conventional device in the market, and is not described herein again. The solution concentrated by the reverse osmosis membrane can be evaporated to remove water through the crystallization drying device 400, and is further concentrated, so that crystals are separated out, and the crystals are dried to obtain the product.
In order to effectively save the use of the regenerant, reduce the wastewater discharge, reduce the content of the residual chemicals in the wastewater, and save the water consumption, the continuous ion-exchange desalination system 200 of this embodiment sufficiently and effectively recycles the residual raw materials, reuse water, and regenerant. The continuous ion exchange desalting system has the following specific structure:
a feeding area:
the feed section 2 includes a stock tank 21, a first male resin unit feed section 22, a first female resin unit feed section 23, a second male resin unit feed section 24, a second female resin unit feed section 25, an intermediate feed tank 26, a third male resin unit feed section 27, a third female resin unit feed section 28, and a product tank 29, which are connected in this order.
The raw material flows into a first cation resin unit feeding area 22 and a first anion resin unit feeding area 23 in sequence through a raw material tank 21 for primary ion-exchange desalination, the discharge liquid of the raw material and the discharge liquid of a washing area 1 respectively flow into a washing tank 14 to be mixed, the mixed liquid flows into a second cation resin unit feeding area 24 and a second anion resin unit feeding area 25 in sequence for secondary ion-exchange desalination, the discharge liquid flows into a third cation resin unit feeding area 27 and a third anion resin unit feeding area 28 in sequence for third ion-exchange desalination, and the final discharge liquid flows into a product tank 29. And the precision of the product is improved by three times of ion exchange and desalination.
Wherein, the resin units between the first male resin unit feeding areas 22, the resin units between the first female resin unit feeding areas 23, the resin units between the second male resin unit feeding areas 24, the resin units between the second female resin unit feeding areas 25, the resin units between the third male resin unit feeding areas 27 and the resin units between the third female resin unit feeding areas 28 are connected in parallel in the forward direction. The mode of first parallel connection and then series connection can improve the feeding efficiency and can carry out cation-anion exchange desalination in order.
Wherein, the raw material tank 21, the intermediate feeding tank 26 and the product tank 29 are all provided with a power pump, a blow-down valve, a feeding hole and a discharging hole.
A material washing area:
the material washing area 1 comprises a pure water tank 11, a positive resin unit material washing area 12, a negative resin unit material washing area 13 and a material washing tank 14 which are connected in sequence.
Pure water flows into a positive resin unit washing area 12 and a negative resin unit washing area 13 through a pure water tank 11 respectively, and liquid outlets of the two areas are mixed and connected into a washing tank 14 and used for washing products remained on the positive and negative resins, so that the product recovery rate is improved.
Wherein the resin units in the positive resin unit washing area 12 and the negative resin unit washing area 13 are connected in series in the positive direction. The serial connection mode is more beneficial to cleaning.
Wherein, the pure water tank 11 is provided with a blowoff valve, a first material washing pump connected with the positive resin unit material washing area 12, a second material washing pump connected with the negative resin unit material washing area 13, and a pure water pump connected with an external pure water pipe.
A regeneration zone:
the regeneration zone 5 comprises a dilute acid tank 51, a first cation resin unit regeneration zone 52, an acid applying tank 53, a second cation resin unit regeneration zone 54, a dilute alkali tank 55, a first anion resin unit regeneration zone 56, an alkali applying tank 57, a second anion resin unit regeneration zone 58 and a waste acid alkali neutralization tank 59 which are connected in sequence.
Wherein, dilute acid liquid flows into a first cation resin unit regeneration area 52 for complete regeneration through a dilute acid tank 51, the discharge liquid of the dilute acid liquid and the discharge liquid of a cation resin unit cleaning area 41 of a cleaning area 4 are mixed in an acid tank 53 for pre-regeneration, and then the discharge liquid flows into a second cation resin unit regeneration area 54 for pre-regeneration, and the discharge liquid of the dilute acid liquid flows into a waste acid alkali neutralization tank 59; and removing the metal salt adsorbed by the positive resin unit, and regenerating the saturated positive resin unit.
Dilute alkali liquor flows into a first anion resin unit regeneration area 56 for complete regeneration through a dilute alkali tank 55, the discharge liquid of the dilute alkali liquor is mixed with the discharge liquid of an anion resin unit cleaning area 42 of a cleaning area 4 in an alkali tank 57 for application, and then flows into a second anion resin unit regeneration area 58 for pre-regeneration, and the discharge liquid of the dilute alkali liquor flows into a waste acid alkali neutralization tank 59; the metal salt adsorbed by the negative resin unit is taken out, and the saturated negative resin unit is regenerated.
The resin units in the first male resin unit regeneration zone 52 and the resin units in the first female resin unit regeneration zone 56 are connected in series and in reverse.
The resin units in the second male resin unit regeneration zone 54 and the resin units in the second female resin unit regeneration zone 58 are connected in series and in reverse after being connected in parallel.
The liquid in the acid applying tank 53 and the alkali applying tank 57 is the regenerant regenerated in the dilute acid tank 51 and the dilute alkali tank 55 after secondary utilization, and the liquid cleaned in the cleaning area 4 is mixed to pre-regenerate the anion and cation resin units, so that the regenerant is fully used. After pre-regeneration, the clean regenerants in the dilute acid tank 51 and the dilute alkali tank 55 are used for serial reverse regeneration, so that the cation and anion resin units are regenerated thoroughly.
Meanwhile, diluted acid and diluted alkali waste liquid after regeneration of the anion and cation resin units is mixed and discharged into a waste acid and alkali neutralizing tank 59 for neutralization and then is treated in a unified way, so that the difficulty of sewage treatment is reduced.
Wherein, the dilute acid tank 51, the dilute alkali tank 55, the acid applying tank 53 and the alkali applying tank 57 are all provided with a power pump, a blow-down valve, a liquid inlet and a liquid outlet.
A cleaning area:
the cleaning zone 4 includes a male resin unit cleaning zone 41 and a female resin unit cleaning zone 42.
A first outlet of the reuse water tank 33 is connected to the cation resin unit washing section 41, and the discharged washing liquid is returned to the reuse acid tank 53 to be mixed with the regeneration discharge liquid of the first cation resin unit regeneration section 52 as a pre-regeneration solvent. A second outlet of the reuse water tank 33 is connected to the anion resin unit washing section 42, and the discharged cleaning solution is returned to the reuse alkali tank 57 and mixed with the discharge solution of the first anion resin unit regeneration section 56 to be used as a pre-regeneration solvent.
Wherein the resin units in the male resin unit washing section 41 and the resin units in the female resin unit washing section 42 are connected in series in opposite directions. The serial connection mode is more beneficial to cleaning.
After the anion and cation resin units are regenerated, the regenerant is remained in the anion and cation resin units, and the regenerant can be prevented from entering a product after the anion and cation resin units are reversely connected in series and washed by recycled water. The liquid after washing flows into an alkali applying tank 57 and an acid applying tank 53 for reuse as a regenerant for pre-regeneration. Fully uses the regenerant, saves the regenerant and reduces the wastewater discharge.
A water-pushing area:
the top water area 3 comprises a top water cation resin unit 31, a top water anion resin unit 32 and a reuse water tank 33; the liquid outlet of the product tank 29 is connected with the top water cation resin unit 31 and the top water anion resin unit 32 in series in the reverse direction and then communicated with the reuse water tank 33. The water in the washed anion and cation resin unit is pushed to the reuse water tank 33 through the product in the product tank 29 for reuse, so that the water consumption is saved, and the excessive water is prevented from flowing into the product tank 29.
The invention also discloses a nucleoside purification process, which adopts the nucleoside purification system and comprises the following steps:
s1, extraction: and (3) roughly filtering the fermentation liquor, and removing impurities such as suspended matters, thalli, macromolecular proteins and the like in the nucleoside solution to obtain a first-stage clarified liquid, wherein the first-stage clarified liquid is obtained. The first-stage clarified liquid has an electric conductivity of 5000 us/cm-15000 us/cm, a pH of 3.0-4.0, and a nucleoside content of 1.0-2.0%.
And then finely filtering the primary clarified liquid to remove organic matters such as protein, pigment and the like to obtain a secondary clarified liquid. Wherein, the conductivity of the secondary clarified liquid is 3000-15000us/cm, the pH is 3.0-4.0, and the nucleoside content is 0.5-2.0%.
S2, purification: and carrying out continuous ion exchange on the secondary clarified liquid, and carrying out desalination treatment to obtain a purified liquid. Wherein, the electric conductivity of the purified liquid is less than 20us/cm, the pH is 6.8-8.0, and the nucleoside content is about 0.5-1.5%; the purity of the nucleoside in the nucleoside solution is more than 99%.
S3, concentration: carrying out reverse osmosis concentration on the purified solution to remove redundant water, and obtaining concentrated solution and dialysate; the nucleoside content of the concentrated solution is 6.0-8.0%. Wherein the dialysate is returned to the continuous ion exchange system for recycling.
S4, crystallization: and (4) carrying out evaporation concentration, crystallization and drying on the concentrated solution to obtain the product.
In order to effectively save the use of the regenerant, reduce the wastewater discharge, reduce the content of the residual chemicals in the wastewater, and save the water consumption, the continuous ion-exchange desalination system 200 of this embodiment sufficiently and effectively recycles the residual raw materials, reuse water, and regenerant. And meanwhile, ion exchange desalination in the feeding area is performed for multiple times, so that the purity of the nucleoside dissolving solution is greatly improved, and after technological purification, the purity can be over 99 percent through one-time crystallization, and qualified products can be obtained.
The continuous ion-exchange desalination system 200 process is specifically as follows:
in this embodiment, the continuous ion-exchange desalination system is provided with 42 resin units, each numbered 1# -42 #.
Odd numbers (1#, 3#, 5#, as well as the 9#, 11 #) are the positive resin units, specifically, 1#, 3#, 5#, and 7# are located in the positive resin unit washing area 12, 9#, and 11# are located in the first positive resin unit feeding area 22, 13#, and 15# are located in the second positive resin unit feeding area 24, 17#, and 19# are located in the third positive resin unit feeding area 27, 21# is the top water positive resin units 31, 23#, 25#, 27#, and 29# are located in the positive resin unit washing area 41, 31#, and 33# are located in the first positive resin unit regeneration area 52, and 35#, 37#, 39#, and 41# are located in the second positive resin unit regeneration area 54.
Wherein the even numbers (2#, 4#, 6#, 42#) are female resin units. Specifically, 2#, 4#, 6#, 8# are located in the female resin unit washing zone 13, 10#, 12# are located in the first female resin unit feeding zone 23, 14#, 16 are located in the second female resin unit feeding zone 25, 18#, 20# are located in the third female resin unit feeding zone 28, 22# is the top water female resin unit 32, 24#, 26#, 28#, 30# is located in the female resin unit washing zone 42, 32#, 34# are located in the first female resin unit regeneration zone 56, 36#, 38#, 40#, 42# are located in the second female resin unit regeneration zone 58.
The resin units of the entire continuous ion-exchange desalination system 200 are moved in a cyclic rotation in a synchronized right-to-left fixed direction, with the flow direction of the various liquids being opposite to the direction of rotation.
Ion exchange desalting:
1. the raw material liquid is conveyed to the 9# and 11# resin units by a feed pump, is parallelly connected to enter a cation exchange system 6, is adsorbed and then parallelly connected to enter the 10# and 12# resin units for anion exchange desalination. The feed liquid from the No. 10 and No. 12 resin units enters a washing tank 14.
2. The washing water from the No. 7 resin unit and the No. 8 resin unit and the feed liquid from the No. 10 and No. 12 resin units enter the washing tank 14 to be mixed, and then the washing water is conveyed by a primary feed pump to enter the No. 13 and No. 15 resin units and the No. 14 and No. 16 resin units for secondary cation exchange and anion exchange desalination, so that the feed liquid is secondarily desalinated. The feed liquid from the 14# and 16# resin units enters the intermediate feed tank 26.
3. The feed liquid in the middle feeding tank 26 is conveyed to the No. 17 and No. 19 resin units through a middle feeding pump, and then enters the No. 18 and No. 20 resin units for third desalting, and the feed liquid after desalting enters a product tank 29 to finish ion exchange desalting purification.
4. After the resin units fed are adsorbed and saturated, the resin units rotate from left to right by one position, and the No. 9 and No. 10 resin units in the feeding area 2 enter the material washing area 1 for water washing.
5. The first pure water pump conveys pure water in the pure water tank 11 to the No. 1 resin unit, and the No. 1, No. 3, No. 5 and No. 7 resin units in the positive resin unit washing area 12 are washed in series in the forward direction; the second pure water pump delivers pure water to the No. 2 resin unit, and carries out forward serial water washing on the No. 2, No. 4, No. 6 and No. 8 resin units in the washing area 13 of the female resin unit. And the washing water from the resin units 7# and 8# and the washing water from the resin units 10# and 12# enter the washing tank 14 to be mixed and then are desalted for the second time.
(II) resin unit regeneration:
1. after the washing of the resin unit in the washing area 1 is completed, the regeneration of the regenerant is needed, and then the desalting treatment can be continued after the washing.
2. After the system moves one resin unit position from right to left, the resin unit # 1 of the cation exchange system 6 and the resin unit # 2 of the anion exchange system 7 are completely cleaned, and then the system is transferred to the regeneration zone 5.
3. After the resin unit with the 1# position is transferred to the resin unit with the 35#, 37#, 39#, 41# positions (2 strings are adopted), the diluted acid in the acid applying tank 53 is reversely conveyed to the resin units with the 35#, 37#, 39#, 41# positions by using an acid applying pump for acid applying regeneration; after the resin unit in the 2# position is transferred to the resin unit positions of 36#, 38#, 40# and 42# (2 strings are adopted), the diluted alkali in the alkali applying tank 57 is reversely conveyed to the resin units of 36#, 38#, 40# and 42# by using an alkali applying pump for alkali applying regeneration. The indiscriminate regeneration is to carry out the pre-regeneration on the resin by secondarily utilizing the regenerant after the primary regeneration, so that the regenerant is fully utilized.
4. After the recycling is finished, the cation resin unit carries out clean dilute acid series reverse recycling on the 31# resin unit and the 33# resin unit, the cation resin is recycled completely, and the recycling agent discharged from the 33# resin unit enters a recycling acid tank 53; the anion resin unit carries out clean dilute alkali series regeneration at the 32# and 34# resin units, the anion resin is regenerated completely, and the regenerant discharged from the 34# resin unit enters the alkali applying tank 57.
5. After the regeneration of acid and alkali is finished, the resin unit can continue to be adsorbed after being cleaned by the regenerant. The cation resin unit enters the No. 23, No. 25, No. 27 and No. 29 resin units for reverse series water washing, and the residual dilute acid comes out of the No. 29 resin unit and enters the acid applying tank 53 for secondary utilization. The negative resin unit enters 24#, 26#, 28# and 30# resin units for serial water washing, and the residual diluted alkali comes out from the 30# resin unit and enters an alkali applying tank 57 for secondary utilization.
6. The 21# and 22# resin units are connected in series to form a top water. After the resin units are cleaned, the resin units 21# and 22# are replaced by the product before feeding, and then the resin units enter the feeding area 2 for feeding. The water displaced by the 21# and 22# resin units is returned to the reuse water tank 33 for recycling. Then enters the feeding zone 2 for adsorption desalination.
The whole system forms a one-way continuous circulation process.
In conclusion, the invention not only can improve the production efficiency and the nucleoside dissolution purity, but also can effectively save the use of chemicals and reduce the discharge of waste water.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention are also included in the scope of the present invention.
Claims (10)
1. A nucleoside purification system, characterized by: comprises a filtering system, a continuous ion exchange desalting system, a concentration system and a crystallization drying device which are connected in sequence;
the continuous ion exchange desalination system comprises a material washing zone, a material feeding zone, a water topping zone, a washing zone and a regeneration zone which are connected in sequence; the feeding zone, the washing zone, the top water zone, the washing zone and the regeneration zone respectively comprise a rotary switching valve, a cation exchange system consisting of a plurality of cation resin units and an anion exchange system consisting of a plurality of anion resin units;
the male resin units and the female resin units are distributed in an up-down symmetrical mode and are connected with the rotary switching valve; the liquid flowing direction in the male resin unit and the female resin unit is opposite to the rotating direction;
the regeneration zone comprises a thorough regeneration zone and a pre-regeneration zone which are connected in sequence;
the positive resin unit and the negative resin unit in the thorough regeneration zone are connected in series in an opposite direction; the positive resin units and the negative resin units in the pre-regeneration zone are connected in series in reverse after being connected in parallel pairwise.
2. The nucleoside purification system according to claim 1, wherein: the filtering system comprises a ceramic membrane filtering system and an ultrafiltration membrane impurity removal system; the ceramic membrane filtering system comprises a ceramic mold core, and the aperture of the ceramic mold core is 40nm-50 nm; the ultrafiltration membrane impurity removal system comprises a hollow ultrafiltration membrane and a roll-type ultrafiltration membrane.
3. The nucleoside purification system according to claim 1, wherein: the concentration system adopts a reverse osmosis membrane concentration system, and dialysate of the reverse osmosis membrane concentration system is connected with a cleaning area of the continuous ion-exchange desalination system through a dialysis tube.
4. The nucleoside purification system according to claim 1, wherein: the regeneration zone also comprises a waste acid and alkali neutralization tank; the thorough regeneration zone comprises a first male resin unit regeneration zone and a first female resin unit regeneration zone; the pre-regeneration zone comprises a second male resin unit regeneration zone and a second female resin unit regeneration zone;
the dilute acid liquid flows into a first cation resin unit regeneration area for complete regeneration, the discharge liquid of the dilute acid liquid is mixed with the discharge liquid of a cation resin unit cleaning area of a cleaning area and then flows into a second cation resin unit regeneration area for pre-regeneration, and the discharge liquid of the dilute acid liquid flows into a waste acid alkali neutralization tank;
the dilute alkali liquor flows into the first negative resin unit regeneration area for complete regeneration, the discharge liquid of the dilute alkali liquor is mixed with the discharge liquid of the negative resin unit cleaning area of the cleaning area and then flows into the second negative resin unit regeneration area for pre-regeneration, and the discharge liquid of the dilute alkali liquor flows into a waste acid alkali neutralization tank.
5. The nucleoside purification system according to claim 1, wherein: the material washing area comprises a positive resin unit material washing area, a negative resin unit material washing area and a material washing tank;
pure water flows into a positive resin unit material washing area and a negative resin unit material washing area respectively, liquid outlets of the two areas are mixed and connected into a material washing tank, and resin units in the positive resin unit material washing area and the negative resin unit material washing area are connected in series in a forward direction.
6. The nucleoside purification system according to claim 1, wherein: the feed zones comprise a first male resin unit feed zone, a first female resin unit feed zone, a second male resin unit feed zone, a second female resin unit feed zone, a third male resin unit feed zone, a third female resin unit feed zone, and a product tank;
raw materials sequentially flow into a first cation resin unit feeding area and a first anion resin unit feeding area for primary ion-exchange desalination, the discharge liquid of the raw materials and the discharge liquid of a material washing area are mixed and sequentially flow into a second cation resin unit feeding area and a second anion resin unit feeding area for secondary ion-exchange desalination, the discharge liquid of the raw materials sequentially flow into a third cation resin unit feeding area and a third anion resin unit feeding area for third ion-exchange desalination, and the final discharge liquid flows into a product tank;
the resin units between the feeding areas of the first male resin units, the resin units between the feeding areas of the first female resin units, the resin units between the feeding areas of the second male resin units, the resin units between the feeding areas of the second female resin units, the resin units between the feeding areas of the third male resin units and the resin units between the feeding areas of the third female resin units are connected in parallel in the forward direction.
7. The nucleoside purification system according to claim 1, wherein: the top water area comprises a top water cation resin unit, a top water anion resin unit and a reuse water tank; a liquid outlet of the feeding area is communicated with the recycling water tank after being connected with the top water cation resin unit and the top water anion resin unit in series in a reverse direction;
the cleaning area comprises a male resin unit cleaning area and a female resin unit cleaning area; a first liquid outlet of the reuse water tank is connected with the cation resin unit cleaning area, and the discharged cleaning liquid flows back to be mixed with the discharged liquid of the first cation resin unit regeneration area; a second liquid outlet of the reuse water tank is connected with the anion resin unit cleaning area, and the discharged cleaning liquid flows back to be mixed with the discharged liquid of the first anion resin unit regeneration area;
wherein the resin units in the male resin unit washing zone and the resin units in the female resin unit washing zone are connected in series in an inverted manner.
8. A process for purifying a nucleoside, comprising: use of a nucleoside purification system as claimed in any one of claims 1 to 7, comprising the steps of:
s1, extraction: coarsely filtering the fermentation liquor to remove macromolecular impurities to obtain a first-stage clarified liquor; fine filtering the first-stage clarified liquid to remove organic matters to obtain a second-stage clarified liquid;
s2, purification: carrying out continuous ion exchange on the secondary clarified liquid, and carrying out desalination treatment to obtain a purified liquid;
s3, concentration: carrying out reverse osmosis concentration on the purified solution to remove redundant water, and obtaining concentrated solution and dialysate;
s4, crystallization: and (4) carrying out evaporation concentration, crystallization and drying on the concentrated solution to obtain the product.
9. A process for purifying a nucleoside according to claim 8, wherein: the conductivity of the first-stage clarified liquid is 5000 us/cm-15000 us/cm, the pH is 3.0-4.0, and the nucleoside content is 1.0-2.0%; the conductivity of the secondary clarified liquid is 3000-15000us/cm, the pH is 3.0-4.0, and the nucleoside content is 0.5-2.0%.
10. A process for purifying a nucleoside according to claim 8, wherein: the purified solution has a conductivity of less than 20us/cm, a pH of 6.8-8.0, and a nucleoside content of about 0.5-1.5%; the purity of the nucleoside in the nucleoside solution is more than 99 percent; the nucleoside content of the concentrated solution is 6.0-8.0%, and the dialyzate is returned to the continuous ion exchange system for recycling.
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