CN105349608A - Method for recycling phenylglycine in cefalexin crystallization mother liquid - Google Patents
Method for recycling phenylglycine in cefalexin crystallization mother liquid Download PDFInfo
- Publication number
- CN105349608A CN105349608A CN201510940748.4A CN201510940748A CN105349608A CN 105349608 A CN105349608 A CN 105349608A CN 201510940748 A CN201510940748 A CN 201510940748A CN 105349608 A CN105349608 A CN 105349608A
- Authority
- CN
- China
- Prior art keywords
- phenylglycine
- nanofiltration
- cephalexin monohydrate
- recoverying
- monohydrate micro
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P35/00—Preparation of compounds having a 5-thia-1-azabicyclo [4.2.0] octane ring system, e.g. cephalosporin
- C12P35/02—Preparation of compounds having a 5-thia-1-azabicyclo [4.2.0] octane ring system, e.g. cephalosporin by desacylation of the substituent in the 7 position
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C227/00—Preparation of compounds containing amino and carboxyl groups bound to the same carbon skeleton
- C07C227/38—Separation; Purification; Stabilisation; Use of additives
- C07C227/40—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
- C07D501/02—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
- C07D501/22—7-Acylaminocephalosporanic or substituted 7-acylaminocephalosporanic acids in which the acyl radicals are derived from carboxylic acids with radicals containing only hydrogen and carbon atoms, attached in position 3
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P13/00—Preparation of nitrogen-containing organic compounds
- C12P13/04—Alpha- or beta- amino acids
Abstract
The invention relates to a method for recycling phenylglycine in cefalexin crystallization mother liquid. The method comprises the steps of pyrolysis, centrifugation, pretreatment, desalination and nano-filtration concentration. The method provided by the invention solves the difficulty that wastewater containing cefalexin cannot be directly treated biochemically, and phenylglycine recovered by the method can be directly applied to subsequent production. According to the method disclosed by the invention, an organic solvent is not used, and the production cost is reduced, so that the method is beneficial for environmental protection and is a green and efficient recovery method.
Description
Technical field
The present invention relates to organism disposing mother liquor and utilize technique, especially relate to the recoverying and utilizing method of phenylglycine in a kind of Cephalexin Monohydrate Micro/Compacted crystalline mother solution.
Background technology
Cephalexin Monohydrate Micro/Compacted is a kind of Broad spectrum antibiotics, the Cephalexin Monohydrate Micro/Compacted mother liquor waste water produced in its production process contains a large amount of organism, inorganic salt and a small amount of Cephalexin Monohydrate Micro/Compacted product, the very difficult standard biochemical methods of organic wastewater of this supersalinity or simply nanofiltration process and recovery.The existing scheme of Cephalexin Monohydrate Micro/Compacted mother liquid disposal adopts organic solvent to carry out extracting and chelating, extract Cephalexin Monohydrate Micro/Compacted, this method not only wastes phenylglycine, and organic solvent consumption is large, environmental protection cannot be disposed to and carry out biochemical treatment, can only form solid waste by evaporation, reprocessing solid waste, this method cost is too high and waste resource.
Patent application CN103788115A discloses a kind of method that integrated membrane process and concentrated enzyme process concentrate Cephalexin Monohydrate Micro/Compacted, by essence filter, ultra-filtration membrane, nanofiltration and reverse osmosis, make concentrated more than 10 times of original Cephalexin Monohydrate Micro/Compacted solution, but it only just reaches concentrated object, how concentrated solution is processed to the concrete grammar of not announcement; Patent CN104058537B discloses a kind of method processing Cephalexin Monohydrate Micro/Compacted enzymatic clarification mother liquor waste water, and it can only recycle the water and minerals crystal in this mother liquor, and other value components still had in mother liquor cannot reclaim.Patent CN102816803B discloses the recoverying and utilizing method of effective constituent in the mother liquor of a kind of enzymatic clarification amoxycilline Trihydrate bp, comprises that hydrolysis, resin isolation, ultrafiltration removal of impurities, nanofiltration are concentrated, isoelectric point crystallizing, reclaims to obtain D-pHPG; Patent CN102392060B discloses a kind of method utilizing nanofiltration to reclaim effective ingredient in the mother liquor of enzymatic clarification amoxycilline Trihydrate bp, comprise hydrolysis, nanofiltration, isoelectric point crystallization, reclaim D-hydroxyphenylglycine and 6-amino-penicillanic acid, wherein also need in nanofiltration process to regulate pH.Due to amoxycilline Trihydrate bp and Ampicillin Trihydrate mother liquor salts contg lower, just can be able to concentrate with simple nanofiltration, and concentrated after concentrated solution need isoelectric point crystallizing to obtain product.
Summary of the invention
Problem to be solved by this invention is the deficiency overcoming prior art existence, provides the recoverying and utilizing method of phenylglycine in a kind of Cephalexin Monohydrate Micro/Compacted crystalline mother solution.
Concrete scheme is as follows:
A recoverying and utilizing method for phenylglycine in Cephalexin Monohydrate Micro/Compacted crystalline mother solution, comprises the following steps:
Cracking: add penicillin G acylase in Cephalexin Monohydrate Micro/Compacted crystalline mother solution, makes the lysate that its cracking obtains containing 7-aminodesacetoxycephalosporanic acid, phenylglycine;
Centrifugal: lysate centrifugation is obtained 7-aminodesacetoxycephalosporanic acid crystal and centrifugal rear liquid, its medium speed is 4000-8000r/min, and centrifugal rear liquid carries out lower step;
Pre-treatment: by centrifugal rear liquid by membrane filtration, obtains cracking concentrated solution and filters dialyzate, filters dialyzate and carries out lower step;
Desalination: filtration dialyzate is passed into electrodialyzer or by ion exchange resin, sloughs the small molecules salt in dialyzate, obtain liquid after desalination, small molecules salt is reclaimed by evaporative crystallization;
Nanofiltration concentrates: liquid after desalination is carried out nanofiltration and concentrates, obtain nanofiltration dialyzate, phenylglycine crystal and nanofiltration concentrated solution, wherein, nanofiltration dialyzate turns back to desalting steps and applies mechanically, phenylglycine crystal is discharged together with exporting with nanofiltration concentrated solution, after reclaiming phenylglycine crystal, residue mother liquor is turned back to reuse in upper step pre-treatment step.
Its further technical scheme is, described crack reacting condition is, pH=5-9, and temperature is react 1-5h under the condition of 25-50 DEG C.
Its further technical scheme is, described lysate regulates its pH to be 3-5, and temperature is 25-30 DEG C of storage, with anti-metamorphic.
Its further technical scheme is, in described preprocessing process, the film core of membrane filtration is that rolling ultrafiltration membrane or rolling nanofiltration membrane or rolling ultrafiltration membrane and rolling nanofiltration membrane combinationally use, and operating pressure is 1bar-20bar.
Its further technical scheme is, in described demineralising process, electrodialysis determines supplied DC voltage according to film logarithm; Optional, X lies prostrate voltage to film supply 0.5X-X.
Its further technical scheme is, described demineralising process ion exchange resin flow velocity is 1-3BV/H.
Its further technical scheme is, described nanofiltration concentrated use film core for nanofiltration membrane core, operating pressure is 15-25bar;
Its further technical scheme is, described phenylglycine crystal can mix with commercially available phenylglycine, for methyl alcohol Reactive Synthesis Phenylglycine methyl ester, or synthesize Phenylglycine methyl ester with methanol of reaction again after recrystallization.
Its further technical scheme is, in described pre-treatment, desalination and nanofiltration concentration process, the temperature range of operation of film is 5-30 DEG C, and single membrane element pressure reduction is no more than 1bar.
Cephalexin Monohydrate Micro/Compacted crystalline mother solution used in the present invention is that in Production by Enzymes Cephalexin Monohydrate Micro/Compacted process, rear residual waste solution is extracted in crystallization; it is after penicillin G acylase effect; Cephalexin Monohydrate Micro/Compacted is cracked into 7-aminodesacetoxycephalosporanic acid crystal (7ADCA) and phenylglycine; go bad for avoiding lysate; need to regulate its pH=3-5, store under the condition of temperature 25-30 DEG C.
For the 7ADCA in lysate, after micron order filter bag (filter bag aperture 5um-10um) can be used after centrifugation to filter, the method for evaporative crystallization is utilized to reclaim; The content filtering phenylglycine in dialyzate is 3-7mg/mL, by isoelectric pH=2-7 crystallizable recovery small part phenylglycine, remains most of phenylglycine still in filtration dialyzate, needs to process further.
The cracking concentrated solution produced in preprocessing process can be disposed to environmental protection unit and do biochemical treatment, filters dialyzate and carries out desalting treatment, slough small molecules salt, be mainly ammonium sulfate.Phenylglycine solution after desalination is by nanofiltration concentration and recovery phenylglycine, and the reuse of nanofiltration dialyzate part is to desalination system, and part can be disposed to environmental protection and do biochemical treatment.
In membrane filtration processes, hypertonia can shorten the work-ing life of film, even damages film device, and hypotony filter effect is not good, and the long period may be needed just to reach set effect, time-consuming bothersome.
Electrodialysis determines supplied DC voltage according to film logarithm, and voltage provides power for ion migration, too highly affects product property, and too low migration effect is not good.
Beneficial effect: (1) the present invention mainly uses embrane method process Cephalexin Monohydrate Micro/Compacted crystalline mother solution, final discharge COD is low, directly can give environmental protection unit and carry out biochemical treatment; (2) method provided by the present invention avoids evaporation to form solid waste on the one hand, reduce processing cost on the other hand, reclaim valuable material simultaneously, reclaim the phenylglycine obtained and also directly can apply to subsequent production, increase benefit, be conducive to the maximum using of resource; (3) present invention reduces production cost, be conducive to environment protection, is a kind of recovery method of green high-efficient.
The present invention mainly uses embrane method process Cephalexin Monohydrate Micro/Compacted crystalline mother solution, and final discharge COD is about 20000mg/L, and ammonia nitrogen is about 10000mg/L, and environmental protection unit discharges after can carrying out biochemical treatment.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Below in conjunction with drawings and Examples, technical solution of the present invention is further elaborated.Unreceipted concrete technology or condition person in embodiment, according to the technology described by the document in this area or condition or carry out according to product description.Agents useful for same or the unreceipted production firm person of instrument, being can by the conventional products of commercial acquisition.
Fig. 1 is process flow sheet of the present invention, the recoverying and utilizing method of phenylglycine in a kind of Cephalexin Monohydrate Micro/Compacted crystalline mother solution, comprise cracking, centrifugal, pre-treatment, desalination, nanofiltration concentrates, the effect that Cephalexin Monohydrate Micro/Compacted mother liquor is cracked into 7ADCA (crystal) and phenylglycine is mainly born in cracking, 7ADCA is after whizzer reclaims, Cephalexin Monohydrate Micro/Compacted lysate carries out pre-treatment, after pre-treatment, concentrated solution contains high molecular weight protein and other impurity is disposed to environmental protection processed in units, filtration dialyzate contains phenylglycine and small molecules salt carries out desalting treatment, phenylglycine is separated with small molecules salt, small molecules saline solution reclaims small molecule salt crystal by evaporation, phenylglycine solution after desalination carries out nanofiltration concentration and recovery phenylglycine, nanofiltration dialyzate can reuse to desalination system, redundance also can be disposed to environmental protection unit and do deep biochemical process.
Embodiment 1
Get enzyme process Cephalexin Monohydrate Micro/Compacted crystalline mother solution 100L; wherein Cephalexin Monohydrate Micro/Compacted content is 15-18g/L; add penicillin G acylase 10kg wherein; regulate pH=7; temperature is react 2h under the condition of 40 DEG C; make the lysate that its cracking obtains containing 7-aminodesacetoxycephalosporanic acid and phenylglycine; wherein phenylglycine 15-18g/L; Cephalexin Monohydrate Micro/Compacted content is less than 1g/L, and ammonium sulfate is about 100g/L, specific conductivity is about 10ms/cm, biochemical oxygen demand (COD) is about 200000mg/L, ammonia nitrogen (NH
3-N) be about 30000mg/L, pH=6-7.Use dilute sulphuric acid to regulate lysate pH to pH=4, holding temperature be 30 DEG C for subsequent use.
Get lysate 100L and carry out centrifugation, rotating speed is 4000r/min, obtain 7-aminodesacetoxycephalosporanic acid crystal 1.02kg and centrifugal rear liquid is about 100L, centrifugal rear liquid is through the spiral wound membrane filtration of 2KDa-20KDa, operating pressure 3bar, temperature is less than 30 DEG C, run and add purified water 30L after 2 hours, obtain 10L concentrated solution and 120L permeate (filtration dialyzate), wherein concentrated solution COD is about 20000mg/L, ammonia nitrogen is about 10000mg/L, carries out biochemical treatment through discharge of pipes to environmental protection; Wherein permeate phenylglycine about 5g/L, ammonium sulfate about 83g/L.
Get permeate 120L and pass into electrodialyzer, electrodialyzer adopts 120 pairs of films, passes into voltage 120V, continuous operation 4h sloughs small molecules salt in dialyzate, and obtain liquid after desalination, small molecules salt is reclaimed by vaporizer crystallization, obtain the white crystal of about 9kg, purity is about 90%.
After getting desalination liquid 120L carry out nanofiltration concentrate, use film core for 150Da-500Da nanofiltration membrane core, operating pressure 15bar, operating temperature is 25 DEG C, working time is 4h, obtain nanofiltration dialyzate 100L, phenylglycine crystal and nanofiltration concentrated solution, wherein, nanofiltration dialyzate phenylglycine content is lower than 1g/L, pH=6-7, desalting steps can be turned back to apply mechanically, phenylglycine crystal is discharged together with exporting with nanofiltration concentrated solution, amount to 20L, wherein phenylglycine crystal is about 400g, purity 93%, employing rotating speed is that the whizzer of 4000r/min reclaims crystal, in residue mother liquor, the concentration of phenylglycine is 10mg/mL, reuse in step pre-treatment step can be turned back to, can be used for after phenylglycine crystal recrystallization and methyl alcohol Reactive Synthesis Phenylglycine methyl ester.
Embodiment 2
Get enzyme process Cephalexin Monohydrate Micro/Compacted crystalline mother solution 100L; wherein Cephalexin Monohydrate Micro/Compacted content is 15-18g/L; add penicillin G acylase 10kg wherein; pH=5 is regulated with dilute sulphuric acid; temperature is react 5h under the condition of 25 DEG C; make the lysate that its cracking obtains containing 7-aminodesacetoxycephalosporanic acid and phenylglycine; wherein phenylglycine 15-18g/L; Cephalexin Monohydrate Micro/Compacted content is less than 1g/L, and ammonium sulfate is about 100g/L, specific conductivity is about 10ms/cm, biochemical oxygen demand (COD) is about 200000mg/L, ammonia nitrogen (NH
3-N) be about 30000mg/L, pH=6-7.Use dilute sulphuric acid to regulate lysate pH to pH=3, holding temperature be 25 DEG C for subsequent use.
Get lysate 100L and carry out centrifugation, rotating speed is 8000r/min, obtain 7-aminodesacetoxycephalosporanic acid crystal 1.35kg and centrifugal rear liquid is about 100L, centrifugal rear liquid through rolling nanofiltration membrane, operating pressure 3bar, temperature is less than 30 DEG C, run and add purified water 30L after 2 hours, obtain 10L concentrated solution and 120L permeate (filtration dialyzate), wherein concentrated solution COD is about 20000mg/L, ammonia nitrogen is about 10000mg/L, carries out biochemical treatment through discharge of pipes to environmental protection; Wherein permeate phenylglycine about 5g/L, ammonium sulfate about 83g/L.
Get permeate 120L and pass into electrodialyzer, electrodialyzer adopts 120 pairs of films, passes into voltage 60V, continuous operation 8h sloughs small molecules salt in dialyzate, and obtain liquid after desalination, small molecules salt is reclaimed by vaporizer crystallization, obtain the white crystal of about 9kg, purity is about 90%.
After getting desalination liquid 120L carry out nanofiltration concentrate, use film core for 150Da-500Da nanofiltration membrane core, operating pressure 25bar, operating temperature is 30 DEG C, working time is 4h, obtain nanofiltration dialyzate 100L, phenylglycine crystal and nanofiltration concentrated solution, wherein, nanofiltration dialyzate phenylglycine content is lower than 1g/L, pH=6-7, desalting steps can be turned back to apply mechanically, phenylglycine crystal is discharged together with exporting with nanofiltration concentrated solution, amount to 20L, wherein phenylglycine crystal is about 400g, purity 93%, employing rotating speed is that the whizzer of 4000r/min reclaims crystal, in residue mother liquor, the concentration of phenylglycine is 10mg/mL, reuse in step pre-treatment step can be turned back to, phenylglycine crystal can be used for and methyl alcohol Reactive Synthesis Phenylglycine methyl ester.
Embodiment 3
Get enzyme process Cephalexin Monohydrate Micro/Compacted crystalline mother solution 100L; wherein Cephalexin Monohydrate Micro/Compacted content is 15-18g/L; add penicillin G acylase 10kg wherein; pH=9 is regulated with the ammoniacal liquor after dilution; temperature is react 1h under the condition of 50 DEG C; make the lysate that its cracking obtains containing 7-aminodesacetoxycephalosporanic acid and phenylglycine; wherein phenylglycine 15-18g/L; Cephalexin Monohydrate Micro/Compacted content is less than 1g/L, and ammonium sulfate is about 100g/L, specific conductivity is about 10ms/cm, biochemical oxygen demand (COD) is about 200000mg/L, ammonia nitrogen (NH
3-N) be about 30000mg/L, pH=6-7.Use dilute sulphuric acid to regulate lysate pH to pH=4, holding temperature be 30 DEG C for subsequent use.
Get lysate 100L and carry out centrifugation, rotating speed is 5000r/min, obtain 7-aminodesacetoxycephalosporanic acid crystal 1.02kg and centrifugal rear liquid is about 100L, centrifugal rear liquid is through membrane filtration (film core is the combination of rolling ultrafiltration membrane and nanofiltration membrane), operating pressure 20bar, temperature is 20 DEG C, run and add purified water 30L after 2 hours, obtain 10L concentrated solution and 120L permeate (filtration dialyzate), wherein concentrated solution COD is about 20000mg/L, ammonia nitrogen is about 10000mg/L, carries out biochemical treatment through discharge of pipes to environmental protection; Wherein permeate phenylglycine about 5g/L, ammonium sulfate about 83g/L.
Get permeate 120L and cross ion exchange resin, flow velocity is 3BV/H, runs continuously 4h and sloughs small molecules salt in dialyzate, and obtain liquid after desalination, small molecules salt is reclaimed by vaporizer crystallization, and obtain the white crystal of about 9kg, purity is about 90%.
After getting desalination liquid 120L carry out nanofiltration concentrate, use film core for 150Da-500Da nanofiltration membrane core, operating pressure 20bar, operating temperature is 30 DEG C, working time is 4h, obtain nanofiltration dialyzate 100L, phenylglycine crystal and nanofiltration concentrated solution, wherein, nanofiltration dialyzate phenylglycine content is lower than 1g/L, pH=6-7, desalting steps can be turned back to apply mechanically, phenylglycine crystal is discharged together with exporting with nanofiltration concentrated solution, amount to 20L, wherein phenylglycine crystal is about 400g, purity 93%, employing rotating speed is that the whizzer of 4000r/min reclaims crystal, in residue mother liquor, the concentration of phenylglycine is 10mg/mL, reuse in step pre-treatment step can be turned back to, phenylglycine crystal can be used for and methyl alcohol Reactive Synthesis Phenylglycine methyl ester.
Although illustrate and describe embodiments of the invention above, be understandable that, above-described embodiment is exemplary, can not be interpreted as limitation of the present invention, those of ordinary skill in the art can change above-described embodiment within the scope of the invention when not departing from principle of the present invention and aim, revising, replacing and modification.
Claims (9)
1. the recoverying and utilizing method of phenylglycine in Cephalexin Monohydrate Micro/Compacted crystalline mother solution, is characterized in that: comprise the following steps:
Cracking: add penicillin G acylase in Cephalexin Monohydrate Micro/Compacted crystalline mother solution, makes the lysate that its cracking obtains containing 7-aminodesacetoxycephalosporanic acid, phenylglycine;
Centrifugal: lysate centrifugation is obtained 7-aminodesacetoxycephalosporanic acid crystal and centrifugal rear liquid, its medium speed is 4000-8000r/min, and centrifugal rear liquid carries out lower step;
Pre-treatment: by centrifugal rear liquid by membrane filtration, obtains cracking concentrated solution and filters dialyzate, filters dialyzate and carries out lower step;
Desalination: filtration dialyzate is passed into electrodialyzer or by ion exchange resin, sloughs the small molecules salt in dialyzate, obtain liquid after desalination, small molecules salt is reclaimed by evaporative crystallization;
Nanofiltration concentrates: liquid after desalination is carried out nanofiltration and concentrates, obtain nanofiltration dialyzate, phenylglycine crystal and nanofiltration concentrated solution, wherein, nanofiltration dialyzate turns back to desalting steps and applies mechanically, phenylglycine crystal is discharged together with exporting with nanofiltration concentrated solution, after reclaiming phenylglycine crystal, residue mother liquor is turned back to reuse in upper step pre-treatment step.
2. the recoverying and utilizing method of phenylglycine in a kind of Cephalexin Monohydrate Micro/Compacted crystalline mother solution according to claim 1, it is characterized in that: described crack reacting condition is, pH=5-9, temperature is react 1-5h under the condition of 25-50 DEG C.
3. the recoverying and utilizing method of phenylglycine in a kind of Cephalexin Monohydrate Micro/Compacted crystalline mother solution according to claim 1, it is characterized in that: described lysate regulates its pH to be 3-5, temperature is 25-30 DEG C of storage, with anti-metamorphic.
4. the recoverying and utilizing method of phenylglycine in a kind of Cephalexin Monohydrate Micro/Compacted crystalline mother solution according to claim 1, it is characterized in that: in described preprocessing process, the film core of membrane filtration is that rolling ultrafiltration membrane or rolling nanofiltration membrane or rolling ultrafiltration membrane and rolling nanofiltration membrane combinationally use, and operating pressure is 1bar-20bar.
5. the recoverying and utilizing method of phenylglycine in a kind of Cephalexin Monohydrate Micro/Compacted crystalline mother solution according to claim 1, is characterized in that: in described demineralising process, electrodialysis determines supplied DC voltage according to film logarithm;
Optional, X lies prostrate voltage to film supply 0.5X-X.
6. the recoverying and utilizing method of phenylglycine in a kind of Cephalexin Monohydrate Micro/Compacted crystalline mother solution according to claim 1, is characterized in that: described demineralising process ion exchange resin flow velocity is 1-3BV/H.
7. the recoverying and utilizing method of phenylglycine in a kind of Cephalexin Monohydrate Micro/Compacted crystalline mother solution according to claim 1, is characterized in that: described nanofiltration concentrated use film core for nanofiltration membrane core, operating pressure is 15-25bar;
8. the recoverying and utilizing method of phenylglycine in a kind of Cephalexin Monohydrate Micro/Compacted crystalline mother solution according to claim 1, it is characterized in that: described phenylglycine crystal can mix with commercially available phenylglycine, for with methyl alcohol Reactive Synthesis Phenylglycine methyl ester, or after recrystallization again with methyl alcohol Reactive Synthesis Phenylglycine methyl ester.
9. the recoverying and utilizing method of phenylglycine in a kind of Cephalexin Monohydrate Micro/Compacted crystalline mother solution according to claim 1, it is characterized in that: in described pre-treatment, desalination and nanofiltration concentration process, the temperature range of operation of film is 5-30 DEG C, single membrane element pressure reduction is no more than 1bar.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510940748.4A CN105349608B (en) | 2015-12-16 | 2015-12-16 | The recoverying and utilizing method of phenylglycine in a kind of cefalexin crystalline mother solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510940748.4A CN105349608B (en) | 2015-12-16 | 2015-12-16 | The recoverying and utilizing method of phenylglycine in a kind of cefalexin crystalline mother solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105349608A true CN105349608A (en) | 2016-02-24 |
| CN105349608B CN105349608B (en) | 2019-01-25 |
Family
ID=55325670
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510940748.4A Active CN105349608B (en) | 2015-12-16 | 2015-12-16 | The recoverying and utilizing method of phenylglycine in a kind of cefalexin crystalline mother solution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105349608B (en) |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105294734A (en) * | 2015-10-16 | 2016-02-03 | 华北制药河北华民药业有限责任公司 | Method for preparing cefonicid dibenzyl ethylenediamine salt |
| CN106220646A (en) * | 2016-07-29 | 2016-12-14 | 华北制药河北华民药业有限责任公司 | A kind of method that recycling of enzymatic clarification cefalexin mother solution |
| CN110002650A (en) * | 2019-04-16 | 2019-07-12 | 同舟纵横（厦门）流体技术有限公司 | A kind of processing method of the nanofiltration dislysate of Amoxicillin crystalline mother solution and/or 6-amino-penicillanic acid crystalline mother solution |
| CN110922416A (en) * | 2019-11-06 | 2020-03-27 | 天津大学 | Method for recovering and purifying 7-aminodesacetoxycephalosporanic acid and phenylglycine in cefalexin crystallization mother liquor |
| CN110922417A (en) * | 2019-11-06 | 2020-03-27 | 天津大学 | Method for recovering cefalexin crystallization mother liquor |
| CN111118097A (en) * | 2019-12-18 | 2020-05-08 | 华北制药河北华民药业有限责任公司 | Method for preparing 7-ADCA by using ultrasonic-assisted cephalexin lyase |
| CN111392819A (en) * | 2020-04-01 | 2020-07-10 | 大连理工大学 | Method for multi-stage separation of cephalosporin crystallization waste liquid by adopting nanofiltration membrane |
| CN111484182A (en) * | 2020-05-12 | 2020-08-04 | 华北制药股份有限公司 | 7-ADCA mother liquor recovery processing method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102392060A (en) * | 2011-09-16 | 2012-03-28 | 石药集团中润制药(内蒙古)有限公司 | Recovering method of effective components in amoxicillin enzymatic synthesis mother liquor by utilizing nanofiltration |
| CN102816803A (en) * | 2012-09-10 | 2012-12-12 | 华北制药集团先泰药业有限公司 | Method for recycling active ingredients in amoxicillin mother liquor synthesized by enzymatic method |
| CN104058537A (en) * | 2014-04-30 | 2014-09-24 | 浙江工业大学 | Method for treating cefalexin enzyme-process synthesizing mother liquor wastewater |
-
2015
- 2015-12-16 CN CN201510940748.4A patent/CN105349608B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102392060A (en) * | 2011-09-16 | 2012-03-28 | 石药集团中润制药(内蒙古)有限公司 | Recovering method of effective components in amoxicillin enzymatic synthesis mother liquor by utilizing nanofiltration |
| CN102816803A (en) * | 2012-09-10 | 2012-12-12 | 华北制药集团先泰药业有限公司 | Method for recycling active ingredients in amoxicillin mother liquor synthesized by enzymatic method |
| CN104058537A (en) * | 2014-04-30 | 2014-09-24 | 浙江工业大学 | Method for treating cefalexin enzyme-process synthesizing mother liquor wastewater |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105294734A (en) * | 2015-10-16 | 2016-02-03 | 华北制药河北华民药业有限责任公司 | Method for preparing cefonicid dibenzyl ethylenediamine salt |
| CN106220646A (en) * | 2016-07-29 | 2016-12-14 | 华北制药河北华民药业有限责任公司 | A kind of method that recycling of enzymatic clarification cefalexin mother solution |
| CN110002650A (en) * | 2019-04-16 | 2019-07-12 | 同舟纵横（厦门）流体技术有限公司 | A kind of processing method of the nanofiltration dislysate of Amoxicillin crystalline mother solution and/or 6-amino-penicillanic acid crystalline mother solution |
| CN110922416A (en) * | 2019-11-06 | 2020-03-27 | 天津大学 | Method for recovering and purifying 7-aminodesacetoxycephalosporanic acid and phenylglycine in cefalexin crystallization mother liquor |
| CN110922417A (en) * | 2019-11-06 | 2020-03-27 | 天津大学 | Method for recovering cefalexin crystallization mother liquor |
| CN111118097A (en) * | 2019-12-18 | 2020-05-08 | 华北制药河北华民药业有限责任公司 | Method for preparing 7-ADCA by using ultrasonic-assisted cephalexin lyase |
| CN111392819A (en) * | 2020-04-01 | 2020-07-10 | 大连理工大学 | Method for multi-stage separation of cephalosporin crystallization waste liquid by adopting nanofiltration membrane |
| CN111484182A (en) * | 2020-05-12 | 2020-08-04 | 华北制药股份有限公司 | 7-ADCA mother liquor recovery processing method |
Also Published As
| Publication number | Publication date |
|---|---|
| CN105349608B (en) | 2019-01-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105349608B (en) | The recoverying and utilizing method of phenylglycine in a kind of cefalexin crystalline mother solution | |
| CN104445788B (en) | High slat-containing wastewater treatment for reuse zero-emission integrated technique | |
| CN101503353B (en) | Technique for purifying crude terephthalic acid from alkali deweighting wastewater | |
| CN105645439A (en) | System for preparing potassium sulfate from high-salt-content industrial wastewater and technology of system | |
| CN108117207B (en) | Zero-discharge treatment process method for salt-containing wastewater | |
| CN100427184C (en) | Process for concentrating pesticide mother liquor by film method | |
| CN108117206B (en) | Zero-discharge treatment process method for salt-containing wastewater | |
| CN104803448A (en) | Forward osmosis treatment method of wastewater with high salinity and high organic matter concentration | |
| CN205500801U (en) | System for utilize high salt industrial waste water of containing preparation potassium sulphide | |
| CN102295392A (en) | Method for treating and reusing calcium chloride wastewater | |
| CN105461157A (en) | High-salinity high-organic-matter contentwastewater zero discharge method | |
| CN205603386U (en) | Strong brine zero release membrane concentrator | |
| CN108658345A (en) | A kind of method and system of high-salt wastewater purified salt | |
| CN205258463U (en) | Equipment of phenylglycine among recovery cephalexin mother liquor | |
| CN108793517A (en) | A kind for the treatment of process of high COD leather-making waste waters with high salt | |
| Zhang et al. | Study of a hybrid process combining PACs and membrane operations for antibiotic wastewater treatment | |
| CN103232353A (en) | Method for separating and extracting L-valine from broth with high efficiency | |
| CN103172212A (en) | Treatment method of lignin production waste water | |
| CN105198142A (en) | High-salinity wastewater zero-discharging method | |
| CN101870639A (en) | Method for producing kelp mannitol with low energy consumption | |
| CN203360192U (en) | Treatment device for difficultly degradable industrial wastewater | |
| CN104291501B (en) | A kind of Integrated Membrane Technology processes the method for ammonium nitrate wastewater | |
| CN206204088U (en) | A kind of vitamin B2 waste water reclaiming Integrated Processing Unit | |
| CN112174445A (en) | Zero-emission treatment method for high-concentration brine in metallurgical industry | |
| CN103896457A (en) | Fine chemical wastewater treatment process |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |