CN117599860B - Cephalosporium decoloring system and process - Google Patents
Cephalosporium decoloring system and process Download PDFInfo
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- CN117599860B CN117599860B CN202410094218.1A CN202410094218A CN117599860B CN 117599860 B CN117599860 B CN 117599860B CN 202410094218 A CN202410094218 A CN 202410094218A CN 117599860 B CN117599860 B CN 117599860B
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- 238000000034 method Methods 0.000 title claims abstract description 116
- 241001619326 Cephalosporium Species 0.000 title description 4
- 239000011347 resin Substances 0.000 claims abstract description 194
- 229920005989 resin Polymers 0.000 claims abstract description 194
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims abstract description 122
- 238000002386 leaching Methods 0.000 claims abstract description 71
- 235000017557 sodium bicarbonate Nutrition 0.000 claims abstract description 61
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims abstract description 61
- 150000001450 anions Chemical class 0.000 claims abstract description 55
- 238000004042 decolorization Methods 0.000 claims abstract description 55
- 239000007788 liquid Substances 0.000 claims abstract description 50
- 238000011069 regeneration method Methods 0.000 claims abstract description 48
- 230000008929 regeneration Effects 0.000 claims abstract description 42
- 230000009466 transformation Effects 0.000 claims abstract description 38
- 238000011001 backwashing Methods 0.000 claims abstract description 34
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- WDLWHQDACQUCJR-ZAMMOSSLSA-N (6r,7r)-7-[[(2r)-2-azaniumyl-2-(4-hydroxyphenyl)acetyl]amino]-8-oxo-3-[(e)-prop-1-enyl]-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylate Chemical compound C1([C@@H](N)C(=O)N[C@H]2[C@@H]3N(C2=O)C(=C(CS3)/C=C/C)C(O)=O)=CC=C(O)C=C1 WDLWHQDACQUCJR-ZAMMOSSLSA-N 0.000 claims abstract description 15
- 229960002580 cefprozil Drugs 0.000 claims abstract description 15
- 239000000463 material Substances 0.000 claims description 44
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 26
- 239000002994 raw material Substances 0.000 claims description 22
- 229960000583 acetic acid Drugs 0.000 claims description 13
- 239000012362 glacial acetic acid Substances 0.000 claims description 13
- 125000004122 cyclic group Chemical group 0.000 claims description 12
- 239000012527 feed solution Substances 0.000 claims description 12
- 238000005520 cutting process Methods 0.000 claims description 4
- 230000001131 transforming effect Effects 0.000 claims description 4
- 230000001172 regenerating effect Effects 0.000 claims description 3
- 125000000129 anionic group Chemical group 0.000 claims description 2
- 239000003513 alkali Substances 0.000 abstract description 16
- 239000002253 acid Substances 0.000 abstract description 12
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 230000007613 environmental effect Effects 0.000 abstract description 3
- 239000000126 substance Substances 0.000 abstract description 3
- 238000006243 chemical reaction Methods 0.000 abstract description 2
- 229930186147 Cephalosporin Natural products 0.000 description 19
- 229940124587 cephalosporin Drugs 0.000 description 19
- 150000001780 cephalosporins Chemical class 0.000 description 19
- 238000000855 fermentation Methods 0.000 description 16
- 230000004151 fermentation Effects 0.000 description 16
- 238000002834 transmittance Methods 0.000 description 9
- 229920006395 saturated elastomer Polymers 0.000 description 8
- 238000011084 recovery Methods 0.000 description 6
- 239000011550 stock solution Substances 0.000 description 6
- HOKIDJSKDBPKTQ-GLXFQSAKSA-N Cephalosporin C Natural products S1CC(COC(=O)C)=C(C(O)=O)N2C(=O)[C@@H](NC(=O)CCC[C@@H](N)C(O)=O)[C@@H]12 HOKIDJSKDBPKTQ-GLXFQSAKSA-N 0.000 description 5
- HOKIDJSKDBPKTQ-GLXFQSAKSA-M cephalosporin C(1-) Chemical compound S1CC(COC(=O)C)=C(C([O-])=O)N2C(=O)[C@@H](NC(=O)CCC[C@@H]([NH3+])C([O-])=O)[C@@H]12 HOKIDJSKDBPKTQ-GLXFQSAKSA-M 0.000 description 5
- 238000010586 diagram Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 4
- 238000005342 ion exchange Methods 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 3
- KEJCWVGMRLCZQQ-YJBYXUATSA-N Cefuroxime axetil Chemical compound N([C@@H]1C(N2C(=C(COC(N)=O)CS[C@@H]21)C(=O)OC(C)OC(C)=O)=O)C(=O)\C(=N/OC)C1=CC=CO1 KEJCWVGMRLCZQQ-YJBYXUATSA-N 0.000 description 3
- 229960002620 cefuroxime axetil Drugs 0.000 description 3
- 238000003860 storage Methods 0.000 description 3
- XWCFYHBHOFBVIV-UHFFFAOYSA-N Deacetylcephalosporin C Natural products S1CC(CO)=C(C(O)=O)N2C(=O)C(NC(=O)CCCC(N)C(O)=O)C21 XWCFYHBHOFBVIV-UHFFFAOYSA-N 0.000 description 2
- XWCFYHBHOFBVIV-JWKOBGCHSA-N deacetylcephalosporin C Chemical compound S1CC(CO)=C(C(O)=O)N2C(=O)[C@@H](NC(=O)CCC[C@@H](N)C(O)=O)[C@H]21 XWCFYHBHOFBVIV-JWKOBGCHSA-N 0.000 description 2
- 238000007599 discharging Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 238000007781 pre-processing Methods 0.000 description 2
- NVIAYEIXYQCDAN-MHTLYPKNSA-N (6r,7s)-7-azaniumyl-3-methyl-8-oxo-5-thia-1-azabicyclo[4.2.0]oct-2-ene-2-carboxylate Chemical compound S1CC(C)=C(C([O-])=O)N2C(=O)[C@H]([NH3+])[C@@H]12 NVIAYEIXYQCDAN-MHTLYPKNSA-N 0.000 description 1
- HSHGZXNAXBPPDL-HZGVNTEJSA-N 7beta-aminocephalosporanic acid Chemical compound S1CC(COC(=O)C)=C(C([O-])=O)N2C(=O)[C@@H]([NH3+])[C@@H]12 HSHGZXNAXBPPDL-HZGVNTEJSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical class OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- URDOHUPGIOGTKV-JTBFTWTJSA-M Cefuroxime sodium Chemical compound [Na+].N([C@@H]1C(N2C(=C(COC(N)=O)CS[C@@H]21)C([O-])=O)=O)C(=O)\C(=N/OC)C1=CC=CO1 URDOHUPGIOGTKV-JTBFTWTJSA-M 0.000 description 1
- 229920002261 Corn starch Polymers 0.000 description 1
- 241000233866 Fungi Species 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 229910052783 alkali metal Inorganic materials 0.000 description 1
- 150000001340 alkali metals Chemical class 0.000 description 1
- 238000007098 aminolysis reaction Methods 0.000 description 1
- 239000003957 anion exchange resin Substances 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 229940088710 antibiotic agent Drugs 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003782 beta lactam antibiotic agent Substances 0.000 description 1
- 229960001668 cefuroxime Drugs 0.000 description 1
- JFPVXVDWJQMJEE-IZRZKJBUSA-N cefuroxime Chemical compound N([C@@H]1C(N2C(=C(COC(N)=O)CS[C@@H]21)C(O)=O)=O)C(=O)\C(=N/OC)C1=CC=CO1 JFPVXVDWJQMJEE-IZRZKJBUSA-N 0.000 description 1
- 229960000534 cefuroxime sodium Drugs 0.000 description 1
- 239000008120 corn starch Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- -1 hydrogen ions Chemical class 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000002503 metabolic effect Effects 0.000 description 1
- 239000002207 metabolite Substances 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 239000002132 β-lactam antibiotic Substances 0.000 description 1
- 229940124586 β-lactam antibiotics Drugs 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J47/00—Ion-exchange processes in general; Apparatus therefor
- B01J47/02—Column or bed processes
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J47/00—Ion-exchange processes in general; Apparatus therefor
- B01J47/14—Controlling or regulating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J49/00—Regeneration or reactivation of ion-exchangers; Apparatus therefor
- B01J49/05—Regeneration or reactivation of ion-exchangers; Apparatus therefor of fixed beds
- B01J49/07—Regeneration or reactivation of ion-exchangers; Apparatus therefor of fixed beds containing anionic exchangers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J49/00—Regeneration or reactivation of ion-exchangers; Apparatus therefor
- B01J49/50—Regeneration or reactivation of ion-exchangers; Apparatus therefor characterised by the regeneration reagents
- B01J49/57—Regeneration or reactivation of ion-exchangers; Apparatus therefor characterised by the regeneration reagents for anionic exchangers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J49/00—Regeneration or reactivation of ion-exchangers; Apparatus therefor
- B01J49/60—Cleaning or rinsing ion-exchange beds
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D501/00—Heterocyclic compounds containing 5-thia-1-azabicyclo [4.2.0] octane ring systems, i.e. compounds containing a ring system of the formula:, e.g. cephalosporins; Such ring systems being further condensed, e.g. 2,3-condensed with an oxygen-, nitrogen- or sulfur-containing hetero ring
- C07D501/02—Preparation
- C07D501/12—Separation; Purification
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D501/00—Heterocyclic compounds containing 5-thia-1-azabicyclo [4.2.0] octane ring systems, i.e. compounds containing a ring system of the formula:, e.g. cephalosporins; Such ring systems being further condensed, e.g. 2,3-condensed with an oxygen-, nitrogen- or sulfur-containing hetero ring
- C07D501/14—Compounds having a nitrogen atom directly attached in position 7
- C07D501/16—Compounds having a nitrogen atom directly attached in position 7 with a double bond between positions 2 and 3
- C07D501/20—7-Acylaminocephalosporanic or substituted 7-acylaminocephalosporanic acids in which the acyl radicals are derived from carboxylic acids
- C07D501/24—7-Acylaminocephalosporanic or substituted 7-acylaminocephalosporanic acids in which the acyl radicals are derived from carboxylic acids with hydrocarbon radicals, substituted by hetero atoms or hetero rings, attached in position 3
- C07D501/26—Methylene radicals, substituted by oxygen atoms; Lactones thereof with the 2-carboxyl group
- C07D501/28—Methylene radicals, substituted by oxygen atoms; Lactones thereof with the 2-carboxyl group with the 7-amino radical acylated by an aliphatic carboxylic acid, which is substituted by hetero atoms
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Treatment Of Water By Ion Exchange (AREA)
Abstract
The invention discloses a cefprozil decoloring system and a process, wherein the system formed by a plurality of anion resin columns comprises the following process positions: the device comprises a sodium bicarbonate ejection area, a circulating feeding area, a color removal area, a secondary leaching area, a transformation area, a primary leaching area, a regeneration area and a backwashing area, wherein a plurality of self-control valves are arranged on each resin column, and the switching of anion resin columns is realized through the opening and closing of different self-control valves, so that the continuous operation of the system is realized through the switching of the control process positions; in each period, the anion resin column of the color removal zone is cut out and enters a circulating feeding zone for pretreatment of feed liquid, and the anion resin column is recovered and converted in exchange capacity through a sodium bicarbonate ejection zone, a backwashing zone, a regeneration zone, a primary leaching zone, a conversion zone and a secondary leaching zone. The invention can reduce the consumption of chemicals, namely acid and alkali, and simultaneously reduce the consumption of water, the production cost and the environmental protection cost by connecting in series-parallel connection.
Description
Technical Field
The invention relates to the technical field of cephalosporin preparation, in particular to a cephalosporin decoloring system and process.
Background
Cephalosporin C (CPC), one of the important raw materials of cephalosporin antibiotics, is a metabolic product of cephalosporin fungi by fermentation culture. The water-soluble compound is an amphoteric compound, the water solubility is extremely good, the polarity is stronger than that of the deacetylcephalosporin C (DCPC), CPC exists in a free form in neutral and slightly acidic environments, free hydrogen ions exist in aqueous solution, corresponding salts can be formed with alkali metals, the compound can be rapidly deactivated in a strong alkali environment, and the compound is subjected to aminolysis and hydrolysis under a weak alkali condition.
The cephalosporin C is a metabolite formed by taking corn starch as a raw material and fermenting by using cephalosporin mould, and can be used as a raw material for producing two beta-lactam antibiotics of 7-ACA and 7-ADCA after adsorption, purification, decolorization and drying.
The anion resin adopted in the current decolorization process of cephalosporin C is gel type acrylic acid series weak alkaline anion exchange resin, and the mode is fixed bed decolorization, but because the color value of the raw material is high and the color value of the discharged material is high, when the decolorization resin column cannot meet the requirement on the decolorization discharge color value of the material, the exchange capacity of the resin column is required to be switched and recovered, but the resin column does not reach the saturated state at the moment, and the exchange capacity of the resin column is recovered under the condition, and the utilization rate of the decolorization resin column is not maximized at the moment, so that the utilization rate of the resin column is lower, and the production cost is increased.
Disclosure of Invention
In view of the above-mentioned drawbacks or shortcomings in the prior art, an object of the present invention is to provide a cefprozil decolorizing system, which introduces a circulation feeding area, on one hand, fully utilizes a resin column, on the other hand, pretreats raw materials, reduces the color value of the raw materials, and increases the throughput of decolorizing the resin column;
the invention also aims to provide a cefprozil decoloring process which comprises a sodium bicarbonate ejection process, a cyclic feeding process, a decoloring process, a secondary leaching process, a transformation process, a primary leaching process, a regeneration process and a backwashing process. Wherein the decoloring process, the sodium bicarbonate material ejection process, the regeneration process, the transformation process and the leaching process at least comprise two anion resin columns, and the cyclic feeding process and the backwashing process at least comprise one anion resin column. The sodium bicarbonate material ejection process, the secondary leaching process, the transformation process, the primary leaching process and the regeneration process are all connected in series, so that the consumption of chemicals and the consumption of water can be reduced. The decoloring process adopts a mode of combining serial connection and parallel connection to improve the decoloring effect.
According to the technical scheme provided by the embodiment of the application, a cefprozil decoloring system, a plurality of anion resin columns are sequentially arranged from left to right, and the system comprises the following process positions: the device comprises a sodium bicarbonate ejection area, a circulating feeding area, a color removal area, a secondary leaching area, a transformation area, a primary leaching area, a regeneration area and a backwashing area, wherein a plurality of self-control valves are arranged on each resin column, and the switching of anion resin columns is realized through the opening and closing of different self-control valves, so that the continuous operation of the system is realized through the switching of the control process positions; in each period, the anion resin column of the color removal zone is cut out and enters a circulating feeding zone for pretreatment of feed liquid, and the anion resin column is recovered and converted in exchange capacity through a sodium bicarbonate ejection zone, a backwashing zone, a regeneration zone, a primary leaching zone, a conversion zone and a secondary leaching zone.
Preferably, the anion resin column is packed with the converted acetate type anion resin.
Preferably, at least two anion resin columns in the color removal zone, the sodium bicarbonate ejection zone, the regeneration zone, the transformation zone and the leaching zone are connected in series; at least one anionic resin column is arranged in the circulating feeding area and the backwashing area, so that the decoloring effect is improved.
Preferably, the color-removed zone is two-stage decolorization.
Preferably, the first-stage decolorization is performed by two anion resin columns connected in parallel, the second-stage decolorization is performed by two anion resin columns connected in parallel, and a discharge port of the first-stage decolorization is connected with a feed port of the second-stage decolorization, so that the decolorization treatment capacity is increased.
A process for decolorizing cephalosporin, comprising the steps of:
(1) And (3) a cyclic feeding procedure: the material liquid to be decolorized enters a circulating feeding zone to pretreat the raw materials, and the discharged material is returned to a feed front tank;
(2) Decoloring procedure: feeding the feed liquid of the feed front tank into a decoloring area for two-stage decoloring;
(3) Sodium bicarbonate ejection procedure: carrying out material ejection treatment on the anion resin column switched in the cyclic feeding procedure by adopting sodium bicarbonate solution;
(4) Backwashing: the anion resin column switched by the sodium bicarbonate liftout area is backwashed by adopting the regeneration area liquid, thereby improving the utilization rate of the process circulating water and reducing the water consumption;
(5) And (3) a regeneration procedure: regenerating the anion resin column switched from the backwashing zone by adopting NaOH solution;
(6) Primary leaching: eluting the anion resin column switched from the regeneration zone for one time by adopting pure water;
(7) Transformation procedure: transforming the anion resin column switched out from the primary leaching area by adopting glacial acetic acid solution;
(8) And (3) a secondary leaching process: carrying out secondary leaching on the anion resin column switched in the transformation zone by adopting pure water;
the continuous operation of the system is realized by sequentially switching the process positions of the anion resin column in different periods.
Preferably, the feed solution to the sodium bicarbonate topping zone is sodium bicarbonate solution at a concentration of 0.2%.
Preferably, the feed solution to the regeneration zone is a 4% NaOH solution.
Preferably, the liquid inlets of the primary leaching area and the secondary leaching area are pure water.
Preferably, the feed liquid to the transformation zone is a 6% strength glacial acetic acid solution.
To sum up, the beneficial effects of this application: the invention has the following advantages:
1. the invention is provided with a plurality of anion resin columns transformed by glacial acetic acid, which are divided into different functional areas, and the switching of the different functional areas and the continuous operation of the system are realized through automatic valves on the anion resin columns;
2. in the decoloring area, two-stage decoloring is arranged, so that the raw material handling capacity of each period is improved;
3. a plurality of units of continuous ion exchange are used, a resin column is cut from the decoloring area to the circulating feeding area in each period, and raw materials needing decoloring treatment are pretreated, so that the resin column can be fully utilized, and the resin utilization rate is improved; on the other hand, the raw material is pretreated, the color value of the raw material is reduced, the pressure of a subsequent color-removing zone is reduced, and the processing capacity of the color-removing zone in each period is increased;
4. the decoloring process adopts a serial-parallel connection mode to connect, so that the decoloring effect is improved;
5. the sodium bicarbonate material ejection process, the secondary leaching process, the transformation process, the primary leaching process and the regeneration process are all connected in series, so that the consumption of chemicals, namely acid and alkali, can be reduced, the consumption of water is reduced, and the production cost and the environmental protection cost are reduced.
Drawings
Other features, objects and advantages of the present application will become more apparent upon reading of the detailed description of non-limiting embodiments, made with reference to the following drawings, in which:
FIG. 1 is a diagram of a process for producing cefuroxime sodium by decolorizing when the sodium bicarbonate jacking area is a single column;
FIG. 2 is a diagram of a process for producing cefprozil decoloration when a sodium bicarbonate ejection area is a double column;
FIG. 3 is a diagram of a process for producing cefuroxime axetil by decoloring after a decoloring system is added in a circulating feeding area;
FIG. 4 is a diagram of a process for decoloring cephalosporin in the prior art;
FIG. 5 is a process diagram of a second cycle of cefuroxime axetil decolorization after adding a decolorizing system to the cyclic feed zone of the present invention.
Reference numerals in the drawings: reference numerals 1-19 are process positions, and reference numerals 1-19 are resin column numbers.
Detailed Description
The present application is described in further detail below with reference to the drawings and examples. It is to be understood that the specific embodiments described herein are merely illustrative of the invention and are not limiting of the invention. It should be noted that, for convenience of description, only the portions related to the invention are shown in the drawings.
It should be noted that, in the case of no conflict, the embodiments and features in the embodiments may be combined with each other. The present application will be described in detail below with reference to the accompanying drawings in conjunction with embodiments.
Example 1
As shown in fig. 1, 17 anion resin columns are sequentially arranged from left to right, a rectangular frame which is vertically arranged is a resin column, and the labels above the rectangular frame are the labels of the resin column, such as 1, 2, 3, 4 …, 17; the labels in the boxes below the rectangle are process position labels, such as 1, 2, 3, 4, … …, 16, 17; the process comprises the following steps: the device comprises a sodium bicarbonate ejection area, a color removal area, a secondary leaching area, a transformation area, a primary leaching area, a regeneration area and a backwashing area, wherein the sodium bicarbonate ejection area is a resin column with the mark of 1; the color-removed areas are resin columns with the marks of 2, 3, 4 and 5; the marks of the resin columns in the secondary leaching area are 6, 7 and 8; the resin columns of the transformation area are numbered 9, 10 and 11; the resin columns in the primary leaching area are numbered 12, 13 and 14; the resin columns in the regeneration zone are marked by 15 and 16; the backwashing area is a No. 17 resin column;
the decoloring method of the whole decoloring system for the cephalosporin fermentation broth is as follows:
(1) Decoloring procedure: the method comprises the steps of (1) enabling cefuroxime fermentation liquor with light transmittance of 60-70% and pH of 3.5-4.5 to enter parallel resin columns with the numbers of 2 and 3 for primary decolorization, enabling liquid discharged from the primary decolorization to enter parallel resin columns with the numbers of 4 and 5 for secondary decolorization, enabling liquid discharged from the secondary decolorization to pass through 95-99% and enabling pH to be 4-6;
when the light transmittance of discharged material is lower than 95%, the decolorizing treatment capacity of the resin column of the decolorizing zone is reduced, and the exchange capacity of the resin in the resin column of the decolorizing zone is required to be recovered, and the recovery process is as follows:
(2) Resin exchange capacity recovery process in resin column:
A. sodium bicarbonate ejection procedure: the resin column with the mark number of 1, the feed liquor is sodium bicarbonate solution with the concentration of 0.2%, the anion resin column with the mark number of 1 (the anion resin column with the adsorption saturation is the resin column just switched from the decoloring process to the sodium bicarbonate ejection process) is ejected, and the liquid is returned to the feed tank;
B. backwashing: a resin column with the reference numeral 17, wherein the liquid inlet is a liquid outlet of the regeneration zone;
C. and (3) a regeneration procedure: resin columns 15 and 16, the feed solution of which is 4% sodium hydroxide solution, to recover the resin exchange capacity;
D. primary leaching: resin columns with the reference numerals of 12, 13 and 14, and the feed liquor is pure water;
E. transformation procedure: resin columns with the numbers of 9, 10 and 11, wherein the feed liquid is 6% glacial acetic acid solution, and the regenerated hydroxyl anion resin column is converted into an acetate anion resin column;
F. and (3) a secondary leaching process: resin columns with the reference numerals 6, 7 and 8, and the feed liquid is pure water.
Under the condition of the process position setting as shown in FIG. 1, one (1 m 3 ) The proportions of the acid, the alkali and the water which are required to be consumed in the feed liquid are as follows:
TABLE 1 consumption ratio of acid, alkali and Water in the production of decolorized Cephalosporium when the sodium bicarbonate top material zone is a single column
Acid-material ratio (volume ratio) | Alkali-material ratio (volume ratio) | Water-to-material ratio (volume ratio) | Sodium bicarbonate material ratio (volume ratio) |
6% glacial acetic acid/feed stock solution | 4% NaOH/feed solution | Pure water/raw material liquid | 0.2% sodium bicarbonate/feed solution |
0.02 | 0.02 | 0.08 | 0.0762 |
Example 2
As shown in fig. 2, 18 anion resin columns are sequentially arranged from left to right, a rectangular frame which is vertically arranged is a resin column, and the labels above the rectangular frame are the labels of the resin column, such as 1, 2, 3, 4 …, 16, 17 and 18; the labels in the boxes below the rectangle are process position labels, such as 1, 2, 3, 4, … …, 16, 17, 18; the process comprises the following steps: the device comprises a sodium bicarbonate ejection area, a color removal area, a secondary leaching area, a transformation area, a primary leaching area, a regeneration area and a backwashing area, wherein the sodium bicarbonate ejection area is a resin column with serial numbers of 1 and 2; the color-removed areas are resin columns with the reference numbers of 3, 4, 5 and 6; the marks of the resin columns in the secondary leaching area are 7, 8 and 9; the resin columns of the transformation area are marked as 10, 11 and 12; the resin columns in the primary leaching area are marked as 13, 14 and 15; the resin columns in the regeneration zone are numbered 16 and 17; the resin column of the backwashing zone is 18;
the decoloring procedure of the whole system on the cephalosporin fermentation broth is as follows:
(1) Decoloring procedure: the cefuroxime axetil fermentation liquid with the light transmittance of 60-70% and the pH of 3.5-4.5 enters into resin columns 3 and 4 which are connected in parallel for primary decolorization; the discharged material enters into parallel resin columns 5 and 6 for secondary decolorization, and finally the discharged material transmits light by 95-99% and has pH value of 4-6;
when the light transmittance of discharged material is lower than 95%, the decolorizing treatment capacity of the resin column of the decolorizing zone is reduced, and the exchange capacity of the resin in the resin column of the decolorizing zone is required to be recovered, and the recovery process is as follows:
(2) Resin exchange capacity recovery process in resin column:
A. sodium bicarbonate ejection procedure: resin columns with the serial numbers of 1 and 2 are used for jacking an adsorption saturated anion resin column (the adsorption saturated anion resin column is a resin column which is just switched from a decoloring process to a sodium bicarbonate jacking process) with a sodium bicarbonate solution with the concentration of 0.2 percent, and a liquid outlet is returned to a feeding tank;
B. backwashing: a resin column with the reference numeral 18, wherein the liquid inlet is a regeneration zone liquid outlet;
C. and (3) a regeneration procedure: resin columns numbered 16 and 17, with 4% sodium hydroxide solution as feed to restore resin exchange capacity;
D. primary leaching: resin columns with the reference numerals of 13, 14 and 15, and pure water is used as feed liquid;
E. transformation procedure: resin columns with the reference numbers of 10, 11 and 12, wherein the feed liquor is 6% glacial acetic acid solution, and the regenerated hydroxyl anion resin column is converted into an acetate anion resin column;
F. and (3) a secondary leaching process: resin columns with the reference numerals 7, 8 and 9, and the feed liquid is pure water.
Under the condition of the process position setting as shown in FIG. 2, one side (1 m 3 ) The proportions of the acid, the alkali and the water which are required to be consumed in the feed liquid are as follows:
TABLE 2 consumption ratio of acid, alkali and Water in the production of decolorized Cephalosporium when the sodium bicarbonate top material zone is double column series connection
Acid-material ratio (volume ratio) | Alkali-material ratio (volume ratio) | Water-to-material ratio (volume ratio) | Sodium bicarbonate material ratio (volume ratio) |
6% glacial acetic acid/feed stock solution | 4% NaOH/feed solution | Pure water/raw material liquid | 0.2% sodium bicarbonate/feed solution |
0.02 | 0.02 | 0.08 | 0.04 |
As shown in fig. 2, the cefprozil fermentation liquor decoloring system comprises a sodium bicarbonate ejection area, a color removal area, a secondary leaching area, a transformation area, a primary leaching area, a regeneration area and a backwashing area, and compared with the embodiment 1, the sodium bicarbonate ejection area of the embodiment 2 adopts a two-column series connection mode to eject the decoloring area, and the process can greatly reduce the consumption of sodium bicarbonate.
Example 3
As shown in fig. 3, 19 anion resin columns are sequentially arranged from left to right, a rectangular frame which is vertically arranged is an anion resin column, and the labels above the rectangular frame are the labels of the resin columns, such as 1, 2, 3, 4 …,17, 18 and 19; the labels in the boxes below the rectangle are process position labels, such as 1, 2, 3, 4, … …, 16, 17, 18, 19; the process comprises the following steps: the device comprises a sodium bicarbonate jacking area, a circulating feeding area, a color removal area, a secondary leaching area, a transformation area, a primary leaching area, a regeneration area and a backwashing area, wherein the sodium bicarbonate jacking area is a resin column with serial numbers of 1 and 2; the resin column in the circulating feeding zone is denoted by the reference numeral 3; the resin columns of the color removal areas are marked as 4, 5, 6 and 7; the marks of the resin columns in the secondary leaching area are 8, 9 and 10; the resin columns of the transformation area are numbered 11, 12 and 13; the resin columns in the primary leaching area are marked as 14, 15 and 16; the resin columns of the regeneration zone are numbered 17 and 18; the resin column of the backwashing zone is marked as 19;
the decoloring procedure of the whole system on the cephalosporin fermentation broth is as follows:
(1) And (3) a cyclic feeding procedure: the cefprozil fermentation liquor with the light transmittance of 60-70% and the pH of 3.5-4.5 is sent to a resin column with the number 3 for pretreatment, and the treated feed liquor is sent to a front tank;
(2) Decoloring procedure: feeding raw material liquid of a feed front tank into resin columns with the serial numbers of 4 and 5 which are connected in parallel for primary decolorization, pumping a liquid outlet of the primary decolorization into resin columns with the serial numbers of 6 and 7 which are connected in parallel for secondary decolorization, wherein the transmittance of the liquid outlet in the resin columns with the secondary decolorization is 95-99%, and the pH value is 4-6;
in the decoloring process, after the resin column is subjected to a cyclic feeding process, the resin column almost reaches a saturated state, and the resin is required to be treated to recover the exchange capacity, wherein the recovery process is as follows:
A. and (3) material ejection working procedure: the sodium bicarbonate jacking area is a resin column with serial numbers of 1 and 2, the feed liquor is sodium bicarbonate solution with concentration of 0.2%, the resin column cut in the cyclic feeding procedure is jacked, the liquid outlet titer is greater than 500, the resin column is sent to a storage tank, and the resin column is recovered and concentrated and then enters a decoloring process again, and when the titer is less than 500, the feed liquor is not recovered;
B. backwashing: the backwashing zone is a resin column with the number of 19, and the liquid inlet is the liquid outlet of the regeneration zone;
C. and (3) a regeneration procedure: the regeneration zone is a resin column with serial numbers of 17 and 18, and the regeneration feed liquid is NaOH solution with concentration of 4%;
D. primary leaching: the primary leaching area is a series of resin columns with the reference numbers of 14, 15 and 16, and the feed liquor is pure water;
E. transformation procedure: the transformation area is a series of resin columns with the reference numbers 11, 12 and 13, and the feed liquor is glacial acetic acid solution with the concentration of 6 percent;
F. and (3) a secondary leaching process: the secondary leaching area is a series of resin columns with the reference numbers of 8, 9 and 10, and the feed liquor is pure water.
Under the condition of the process position setting as shown in FIG. 3, one (1 m 3 ) The proportions of the acid, the alkali and the water which are required to be consumed in the feed liquid are as follows:
TABLE 3 consumption ratio of acid, alkali and Water in Cefprozier production after adding the decoloring System to the circulation feeding zone
Acid-material ratio (volume ratio) | Alkali-material ratio (volume ratio) | Water-to-material ratio (volume ratio) | Sodium bicarbonate material ratio (volume ratio) |
6% glacial acetic acid/feed stock solution | 4% NaOH/feed solution | Pure water/raw material liquid | 0.2% sodium bicarbonate/feed solution |
0.016 | 0.016 | 0.064 | 0.032 |
As shown in fig. 3, the cefprozil decolorizing process comprises a sodium bicarbonate ejection area, a circulating feeding area, a decolorizing area, a secondary leaching area, a transformation area, a primary leaching area, a regeneration area and a backwashing area, and compared with the embodiment 2, the embodiment 3 adds the circulating feeding area, namely a resin column with the reference number of 3, in front of the ejection area, because the requirements of the cefprozil discharge decolorizing index are high, and the decolorizing effect of the column switched from the decolorizing area still has a certain decolorizing capacity although the decolorizing effect can not reach the discharge index. As shown in fig. 3, the circulation feeding area is to pre-treat the cephalosporin fermentation liquor to be decolorized in the circulation feeding area, fully utilize the unsaturated resin column No. 3, increase the process, maximally utilize the resin and reduce the decolorization pressure of the subsequent decolorization area on the cephalosporin fermentation liquor.
Example 4
As shown in fig. 4, in the conventional process of domestic cephalosporin production, resin columns numbered 1 and 2 are used as a decoloring function region, a resin column No. 3 is used as a standby waiting region, a resin column No. 4 is used as a recovery exchange capacity region,
the cefprozil fermentation liquor with the light transmittance of 60-70% and the pH of 3.5-4.5 which need to be decolorized is decolorized by a resin column with the reference numbers of 1 and 2, and when the discharged light transmittance reaches 95-99% and the pH reaches 4-6, the production requirement is met. Treatment ofOne (1 m) 3 ) The proportions of the acid, the alkali and the water which are required to be consumed in the feed liquid are as follows:
TABLE 4 consumption ratio of acid, alkali and water in the production of cefprozil by using domestic cefprozil decolorizing traditional process system
Acid-material ratio (volume ratio) | Alkali-material ratio (volume ratio) | Water-to-material ratio (volume ratio) | Sodium bicarbonate material ratio (volume ratio) |
6% glacial acetic acid/feed stock solution | 4% NaOH/feed solution | Pure water/raw material liquid | 0.2% sodium bicarbonate/feed solution |
0.03 | 0.07 | 0.11 | 0.08 |
As can be seen from a comparison of Table 4 and Table 1, the regeneration zone was treated for 1m by using a multi-column series connection 3 The alkali ratio of the feed liquid is reduced from 0.07 to 0.02, a transformation area adopts multi-column series connection to treat 1m 3 The acid-material ratio of the feed liquid is reduced from 0.03 to 0.02, which indicates that the regeneration zone adopts column-series regeneration, thereby saving the regeneration consumption; the transformation areas are connected in a column-string mode, so that transformation consumption is saved;
as can be seen from a comparison of Table 3 and Table 4, the stripping of example 3 was usedColor treatment process, each treatment side (1 m 3 ) The acid-material ratio needed to be consumed of the feed liquid is reduced by 46.7%; the alkali material ratio is reduced by 77.14 percent; the water-material ratio is reduced by 41.82%; the sodium bicarbonate material ratio is reduced by 60%, the consumption of acid, alkali and water can be greatly reduced, the resource cost in the process of decoloring the cephalosporin is reduced, and the production income is greatly improved.
Example 5
The periodic switching steps of the system are as follows:
the first cycle is shown in figure 3, and the sodium bicarbonate liftout zone is a series of anion resin columns with the reference numbers of 1 and 2; the resin column in the circulating feeding zone is denoted by the reference numeral 3; the resin columns of the color removal areas are marked as 4, 5, 6 and 7; the marks of the resin columns in the secondary leaching area are 8, 9 and 10; the resin columns of the transformation area are numbered 11, 12 and 13; the resin columns in the primary leaching area are marked as 14, 15 and 16; the resin columns of the regeneration zone are numbered 17 and 18; the resin column of the backwashing zone is marked by the numeral 19;
the second cycle, as shown in figure 5,
the sodium bicarbonate jacking area is a resin column with serial numbers of 2 and 3; the resin column in the circulating feeding zone is denoted by the reference numeral 4; the resin columns of the color removal areas are marked as 5, 6, 7 and 8; the marks of the secondary leaching areas are 9, 10 and 11; the resin columns of the transformation area are numbered 12, 13 and 14; the resin columns in the primary leaching area are marked as 15, 16 and 17; the resin columns of the regeneration zone are marked as 18 and 19; the resin column of the backwashing zone is marked as 1;
according to multi-unit continuous ion exchange, in the first period, the No. 3 resin column carries out pretreatment on the cephalosporin fermentation liquor until the resin in the No. 3 resin column is saturated; the pretreated stock solution enters a front tank for storage, and then enters resin columns of decolorizing areas 4, 5, 6 and 7 for decolorization. When the raw material treatment in the decoloring area cannot reach the discharge standard (the light transmittance is 95% -99% and the pH is 4-6), reaching a second period, as shown in fig. 5, cutting out a No. 4 resin column, wherein the No. 4 resin column is a circulating feeding area, and preprocessing the cephalosporin fermentation liquid until the resin in the No. 4 resin column is saturated; the pretreated stock solution enters a front tank for storage, then enters resin columns 5, 6, 7 and 8 for decolorization, and at the moment, the sodium bicarbonate jacking area is a resin column with serial numbers of 2 and 3; the marks of the resin columns in the secondary leaching area are 9, 10 and 11; the resin columns of the transformation area are numbered 12, 13 and 14; the resin columns in the leaching area are marked as 15, 16 and 17; the resin columns of the regeneration zone are marked as 18 and 19; the resin column of the backwash zone is numbered 1. And (3) entering the next period after the material liquid in the color-removing zone does not meet the material discharging standard.
And in the third period, cutting out the No. 5 resin column of the color removal zone in the second period to form a circulating feeding zone, preprocessing the cephalosporin fermentation liquor, cutting in the No. 9 resin column into the decoloring zone to decolor until the discharged liquor does not reach the standard, and continuously switching one position to the left of each ion exchange column, wherein the No. 6 column is the circulating feeding zone, the No. 7, 8, 9 and 10 columns are color removal zones, the No. 11, 12 and 13 columns are secondary leaching zones, the No. 14, 15 and 16 columns are transformation zones, the No. 17, 18 and 19 columns are primary leaching zones, the No. 1 and 2 columns are regeneration zones, the No. 3 column is a backwashing zone, and the No. 4 and 5 columns are sodium bicarbonate jacking zones.
… and so on, according to the principle of multi-unit continuous ion exchange, in each period, a resin column which is cut from a decoloring area and is not completely invalid but cannot meet the discharging requirement of the decoloring area is cut into a circulating feeding procedure to pretreat the cephalosporin fermentation raw material, and after the resin is saturated, the exchange capacity of the saturated resin column is recovered by utilizing a multi-unit treatment functional area, such as a sodium bicarbonate ejection area, a secondary leaching area, a transformation area, a primary leaching area, a regeneration area and a backwashing area, so that the consumption of acid, alkali and water is greatly reduced, and the industrial production cost and the environmental protection pressure are saved;
after the resin column of the color removal zone is cut out in each period, the resin column enters a circulating feeding zone, and the cephalosporin fermentation liquor is pretreated, so that on one hand, the utilization efficiency of the resin column of the color removal zone is improved, and on the other hand, after the raw materials are pretreated, the color value of the raw materials can be reduced, and the treatment capacity of the resin column of the color removal zone is increased.
The above description is only illustrative of the preferred embodiments of the present application and of the principles of the technology employed. Meanwhile, the scope of the invention referred to in this application is not limited to the technical solutions of the specific combination of the above technical features, but also covers other technical solutions formed by any combination of the above technical features or their equivalents without departing from the inventive concept. Such as the above-described features and technical features having similar functions (but not limited to) disclosed in the present application are replaced with each other.
Claims (8)
1. A cefprozil decolorizing system, characterized in that:
the anion resin columns are sequentially arranged from left to right, and the system comprises the following process positions: the device comprises a sodium bicarbonate ejection area, a circulating feeding area, a color removal area, a secondary leaching area, a transformation area, a primary leaching area, a regeneration area and a backwashing area, wherein a plurality of self-control valves are arranged on each resin column, and the switching of anion resin columns is realized through the opening and closing of different self-control valves, so that the continuous operation of the system is realized through the switching of the control process positions;
in each period, cutting out the anion resin column of the color removal zone, entering a circulating feeding zone for pretreatment of feed liquid, and recovering and transforming the exchange capacity of the anion resin column through a sodium bicarbonate ejection zone, a backwashing zone, a regeneration zone, a primary leaching zone, a transformation zone and a secondary leaching zone;
the decoloring process completed by the decoloring system comprises the following steps:
(1) And (3) a cyclic feeding procedure: the material liquid to be decolorized enters a circulating feeding zone to pretreat the raw materials, and the discharged material is returned to a feed front tank;
(2) Decoloring procedure: feeding the feed liquid of the feed front tank into a decoloring area for two-stage decoloring;
(3) Sodium bicarbonate ejection procedure: carrying out material ejection treatment on the anion resin column switched in the cyclic feeding procedure by adopting sodium bicarbonate solution;
(4) Backwashing: backwashing the anion resin column switched by the sodium bicarbonate liftout area by adopting the regeneration area liquid;
(5) And (3) a regeneration procedure: regenerating the anion resin column switched from the backwashing zone by adopting NaOH solution;
(6) Primary leaching: eluting the anion resin column switched from the regeneration zone for one time by adopting pure water;
(7) Transformation procedure: transforming the anion resin column switched out from the primary leaching area by adopting glacial acetic acid solution;
(8) And (3) a secondary leaching process: carrying out secondary leaching on the anion resin column switched in the transformation zone by adopting pure water;
the continuous operation of the system is realized by sequentially switching the process positions of the anion resin column in different periods.
2. A cefprozil decolorizing system according to claim 1, wherein: at least two anion resin columns in the color removal zone, the sodium bicarbonate ejection zone, the regeneration zone, the transformation zone and the leaching zone are connected in series; at least one anionic resin column is arranged in the circulating feeding area and the backwashing area.
3. A cefprozil decolorizing system according to claim 2, wherein: the first-stage decolorization is carried out by two anion resin columns connected in parallel, the second-stage decolorization is carried out by two anion resin columns connected in parallel, and a discharge port of the first-stage decolorization is connected with a feed inlet of the second-stage decolorization.
4. A decolorizing process utilizing the system of any one of claims 1-3, comprising the steps of:
(1) And (3) a cyclic feeding procedure: the material liquid to be decolorized enters a circulating feeding zone to pretreat the raw materials, and the discharged material is returned to a feed front tank;
(2) Decoloring procedure: feeding the feed liquid of the feed front tank into a decoloring area for two-stage decoloring;
(3) Sodium bicarbonate ejection procedure: carrying out material ejection treatment on the anion resin column switched in the cyclic feeding procedure by adopting sodium bicarbonate solution;
(4) Backwashing: backwashing the anion resin column switched by the sodium bicarbonate liftout area by adopting the regeneration area liquid;
(5) And (3) a regeneration procedure: regenerating the anion resin column switched from the backwashing zone by adopting NaOH solution;
(6) Primary leaching: eluting the anion resin column switched from the regeneration zone for one time by adopting pure water;
(7) Transformation procedure: transforming the anion resin column switched out from the primary leaching area by adopting glacial acetic acid solution;
(8) And (3) a secondary leaching process: carrying out secondary leaching on the anion resin column switched in the transformation zone by adopting pure water;
the continuous operation of the system is realized by sequentially switching the process positions of the anion resin column in different periods.
5. The decolorization process according to claim 4, wherein: the sodium bicarbonate solution is taken as the feed liquid in the sodium bicarbonate ejection zone, and the concentration is 0.2%.
6. The decolorization process according to claim 5, wherein: the feed solution to the regeneration zone was a 4% NaOH solution.
7. The decolorization process according to claim 6, wherein: and the liquid inlets of the primary leaching area and the secondary leaching area are pure water.
8. The decolorization process according to claim 7, wherein: the feed liquid to the transformation zone was a 6% glacial acetic acid solution.
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US5096500A (en) * | 1989-10-23 | 1992-03-17 | Rar-Refinarias De Acucar Reunidas, S.A. | Process for decolorization and decalcification of sugar solutions |
CN102993214A (en) * | 2012-12-07 | 2013-03-27 | 西北大学 | Method for decoloring cephalosporin |
CN104673872A (en) * | 2014-12-31 | 2015-06-03 | 西安蓝晓科技新材料股份有限公司 | Method for recycling DCPC (deacetyl cephalosporin C) from cephalosporin C resin adsorption waste liquor |
CN116474419A (en) * | 2023-06-09 | 2023-07-25 | 焦作市华康糖醇科技有限公司 | Continuous decolorizing system for xylose production and using method thereof |
WO2023169166A1 (en) * | 2022-03-10 | 2023-09-14 | 欧尚元智能装备有限公司 | Sucrose decoloring method and system |
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US5096500A (en) * | 1989-10-23 | 1992-03-17 | Rar-Refinarias De Acucar Reunidas, S.A. | Process for decolorization and decalcification of sugar solutions |
CN102993214A (en) * | 2012-12-07 | 2013-03-27 | 西北大学 | Method for decoloring cephalosporin |
CN104673872A (en) * | 2014-12-31 | 2015-06-03 | 西安蓝晓科技新材料股份有限公司 | Method for recycling DCPC (deacetyl cephalosporin C) from cephalosporin C resin adsorption waste liquor |
WO2023169166A1 (en) * | 2022-03-10 | 2023-09-14 | 欧尚元智能装备有限公司 | Sucrose decoloring method and system |
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