CN105349608B - The recoverying and utilizing method of phenylglycine in a kind of cefalexin crystalline mother solution - Google Patents
The recoverying and utilizing method of phenylglycine in a kind of cefalexin crystalline mother solution Download PDFInfo
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- 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
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- 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
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Abstract
The present invention relates to a kind of recoverying and utilizing methods of phenylglycine in cefalexin crystalline mother solution, including cracking, centrifugation, pretreatment, desalination, nanofiltration concentration.The present invention solves the problems, such as that the waste water containing cefalexin can not directly carry out biochemical treatment, and the obtained phenylglycine of recycling can directly apply to subsequent production；The present invention does not use organic solvent, reduces production cost, is conducive to environmental protection, is a kind of recovery method of green high-efficient.
Description
Technical field
The present invention relates to organic matter disposing mother liquors to utilize technique, sweet more particularly, to benzene in a kind of cefalexin crystalline mother solution
The recoverying and utilizing method of propylhomoserin.
Background technique
Cefalexin is a kind of broad-spectrum antibiotic, and produced cefalexin mother liquor waste water contains largely in its production process
Organic matter, inorganic salts and a small amount of cefalexin product, the organic wastewater of this high salinity be difficult with routine biochemistry side
Method or simple nanofiltration processing and recycling.Cefalexin mother liquid disposal existing scheme is extracted and is chelated using organic solvent,
Cefalexin is extracted, this method not only wastes phenylglycine, but also organic solvent consumption is big, can not be emitted into environmental protection and carry out at biochemistry
Reason can only form solid waste by evaporation, reprocess solid waste, this method cost is too high and waste of resource.
Patent application CN103788115A discloses the method for a kind of integrated membrane process and concentration enzyme process concentration cefalexin, leads to
Refined filtration, ultrafiltration membrane, nanofiltration and reverse osmosis are crossed, so that original cefalexin solution is concentrated 10 times or more, but it is only merely to reach
Purpose is concentrated, does not report to specific method to how concentrate is handled；Patent CN104058537B discloses a kind of processing cephalo
The method of ammonia benzyl enzymatic clarification mother liquor waste water can only recycle the water in the mother liquor and inorganic salt crystal, still have in mother liquor
Other value components can not recycle.Patent CN102816803B disclose in a kind of mother liquor of enzymatic clarification Amoxicillin effectively at
Point recoverying and utilizing method, including hydrolysis, resin separation, ultrafiltration removal of impurities, nanofiltration concentration, isoelectric point crystallizing, recycle D- to hydroxyl
Base phenylglycine；Patent CN102392060B disclose it is a kind of using nanofiltration recycling enzymatic clarification Amoxicillin mother liquor in effectively at
The method of part, including hydrolysis, nanofiltration, isoelectric point crystallization recycle D- hydroxyphenylglycine and 6-amino-penicillanic acid, wherein nanofiltration
It also needs to adjust pH in journey.Since Amoxicillin and ampicillin mother liquor salt content are lower, simple nanofiltration can be used
Concentration, and the concentrate after concentration needs isoelectric point crystallizing that can just access product.
Summary of the invention
Problem to be solved by this invention is to overcome the shortcomings of the prior art, provides a kind of cefalexin crystalline mother solution
The recoverying and utilizing method of middle phenylglycine.
Concrete scheme is as follows:
The recoverying and utilizing method of phenylglycine in a kind of cefalexin crystalline mother solution, comprising the following steps:
Cracking: penicillin G acylase is added into cefalexin crystalline mother solution, its cracking is made to obtain going second containing 7- amino
The lysate of acyloxy cephalosporanic acid, phenylglycine；
Centrifugation: liquid after lysate is centrifugally separating to obtain 7-aminodesacetoxycephalosporanic acid crystal and is centrifuged, wherein
Revolving speed is 4000-8000r/min, and liquid carries out lower step after centrifugation；
Pretreatment: liquid after centrifugation is filtered by film, is obtained cracking concentrate and is filtered dialyzate, filtering dialyzate carries out
Lower step；
Desalination: filtering dialyzate is passed through electric dialyzator or by ion exchange resin, sloughs small point in dialyzate
Alite class, obtains liquid after desalination, and small molecule salt is recycled by evaporative crystallization；
Nanofiltration concentration: carrying out nanofiltration concentration for liquid after desalination, obtains nanofiltration dislysate, phenylglycine crystal and nanofiltration concentration
Liquid, wherein nanofiltration dislysate is applied back to desalting steps, and phenylglycine crystal and nanofiltration concentrate are discharged together by exporting,
Remaining mother liquor is returned into reuse in upper step pre-treatment step after recycling phenylglycine crystal.
Its further technical solution is that the crack reacting condition is pH=5-9, the condition that temperature is 25-50 DEG C
Lower reaction 1-5h.
Its further technical solution is that it is 3-5 that the lysate, which adjusts its pH, and temperature is 25-30 DEG C of storage, to prevent
It is rotten.
Its further technical solution is that the film core that film filters in the preprocessing process is that rolling ultrafiltration membrane or rolling are received
Filter membrane or rolling ultrafiltration membrane are applied in combination with rolling nanofiltration membrane, operating pressure 1bar-20bar.
Its further technical solution is that electrodialysis determines supplied direct current according to film logarithm in the desalination processes
Voltage；Optional, X lies prostrate voltage to film supply 0.5X-X.
Its further technical solution is that the desalination processes ion exchange resin flow velocity is 1-3BV/H.
Its further technical solution is that it is nanofiltration membrane core, operating pressure 15- that used film core, which is concentrated, in the nanofiltration
25bar；
Its further technical solution is that the phenylglycine crystal can be mixed with commercially available phenylglycine, for
Methanol reaction synthesis Phenylglycine methyl ester, or Phenylglycine methyl ester is synthesized with methanol of reaction again after recrystallization.
Its further technical solution is the running temperature model of film in the pretreatment, desalination and nanofiltration concentration process
Enclosing is 5-30 DEG C, and single branch membrane component pressure difference is no more than 1bar.
Cefalexin crystalline mother solution used in the present invention is that Production by Enzymes cefalexin crystallizes residue after extraction in the process
Waste liquid, after penicillin G acylase acts on, cefalexin is cracked into 7-aminodesacetoxycephalosporanic acid crystal
(7ADCA) and phenylglycine need to adjust its pH=3-5, store up under conditions of 25-30 DEG C of temperature to avoid lysate rotten
It deposits.
For the 7ADCA in lysate, micron order filter bag (filter bag aperture 5um-10um) can be used after centrifuge separation
After filtering, recycled using the method for evaporative crystallization；The content for filtering phenylglycine in dialyzate is 3-7mg/mL, passes through isoelectric point
The crystallizable recycling small part phenylglycine of pH=2-7, remaining major part phenylglycine need further still in filtering dialyzate
Processing.
The cracking concentrate generated in preprocessing process can be emitted into environmentally friendly unit and do biochemical treatment, and filtering dialyzate carries out
Desalting processing sloughs small molecule salt, predominantly ammonium sulfate.Phenylglycine solution after desalination passes through nanofiltration concentration and recovery benzene
Glycine, nanofiltration dislysate part reuse to desalination system can partially be emitted into environmental protection and do biochemical treatment.
Hypertonia can shorten the service life of film, or even damage film device, hypotony filtering effect in membrane filtration processes
Fruit is bad, it may be necessary to which the long period can be only achieved set effect, time-consuming bothersome.
Electrodialysis determines that supplied DC voltage, voltage provide power, excessively high shadow for Ion transfer according to film logarithm
Product property is rung, too low migration effect is bad.
The utility model has the advantages that (1) present invention mainly handles cefalexin crystalline mother solution using embrane method, the final COD that discharges is low, can be straight
It connects and gives environmentally friendly unit progress biochemical treatment；(2) on the one hand method provided by the present invention avoids evaporation to form solid waste, another party
Face reduces processing cost, while recycling valuable substance, and recycling obtained phenylglycine can also directly apply to subsequent life
It produces, increases benefit, be conducive to maximally utilizing for resource；(3) present invention reduces production costs, are conducive to environmental protection,
It is a kind of recovery method of green high-efficient.
The present invention mainly uses embrane method to handle cefalexin crystalline mother solution, and the final COD that discharges is about 20000mg/L, ammonia nitrogen
About 10000mg/L, environmentally friendly unit are discharged after can carrying out biochemical treatment.
Detailed description of the invention
Fig. 1 is process flow chart of the invention.
Specific embodiment
Technical solution of the present invention is further elaborated with reference to the accompanying drawings and examples.Specific skill is not specified in embodiment
Art or condition person described technology or conditions or carry out according to the literature in the art according to product description.Examination used
Production firm person is not specified in agent or instrument, and being can be with conventional products that are commercially available.
Fig. 1 is process flow chart of the invention, the recoverying and utilizing method of phenylglycine in a kind of cefalexin crystalline mother solution,
Including cracking, centrifugation, pretreatment, desalination, nanofiltration concentration, mainly undertaking cefalexin mother liquor is cracked into 7ADCA (crystal) for cracking
With the effect of phenylglycine, after centrifuge recycles, cefalexin lysate is pre-processed 7ADCA, is concentrated after pretreatment
Liquid contains high molecular weight protein and other impurities are emitted into environmentally friendly processed in units, and filtering dialyzate contains phenylglycine and small molecule salt
Class carries out desalting processing, so that phenylglycine is separated with small molecule salt, small molecule saline solution passes through evaporation recycling small molecule
Salt crystal, phenylglycine solution after desalination carry out nanofiltration concentration and recovery phenylglycine, nanofiltration dislysate can reuse to desalination system
System, redundance can also be emitted into environmentally friendly unit and do deep biochemical processing.
Embodiment 1
Enzyme process cefalexin crystalline mother solution 100L is taken, wherein cefalexin content is 15-18g/L, and mould is added thereto
Plain G acylase 10kg, adjusts pH=7, and temperature reacts 2h under conditions of being 40 DEG C, obtains its cracking containing 7- aminodeacetoxy
The lysate of oxygroup cephalosporanic acid and phenylglycine, wherein phenylglycine 15-18g/L, cefalexin content are less than 1g/L, sulfuric acid
Ammonium is about 100g/L, conductivity is about 10ms/cm, bod (COD) is about 200000mg/L, ammonia nitrogen (NH3- N) about
30000mg/L, pH=6-7.Lysate pH to pH=4 is adjusted using dilute sulfuric acid, holding temperature is 30 DEG C spare.
Lysate 100L is taken to be centrifuged, revolving speed 4000r/min obtains 7-aminodesacetoxycephalosporanic acid
Crystal 1.02kg and liquid about 100L after centrifugation, liquid is filtered by the rolling ultrafiltration membrane of 2KDa-20KDa after centrifugation, operating pressure
3bar, temperature add purified water 30L after operation 2 hours less than 30 DEG C, obtain 10L concentrate and (the filtering dialysis of 120L permeate
Liquid), wherein concentrate COD is about 20000mg/L, and ammonia nitrogen is about 10000mg/L, is carried out at biochemistry by discharge of pipes to environmental protection
Reason；Wherein permeate phenylglycine 5g/L or so, ammonium sulfate 83g/L or so.
Permeate 120L is taken to be passed through electric dialyzator, electric dialyzator uses 120 pairs of films, is passed through voltage 120V, continuous operation 4h
The small molecule salt in dialyzate is sloughed, liquid after desalination is obtained, small molecule salt is crystallized by evaporator and recycled, and the left side 9kg is obtained
Right white crystal, purity is about 90%.
Liquid 120L after desalination is taken to carry out nanofiltration concentration, used film core is 150Da-500Da nanofiltration membrane core, operating pressure
15bar, running temperature are 25 DEG C, runing time 4h, obtain nanofiltration dislysate 100L, phenylglycine crystal and nanofiltration concentration
Liquid, wherein nanofiltration dislysate phenylglycine content is lower than 1g/L, pH=6-7, can return to desalting steps and applies, phenylglycine
Crystal and nanofiltration concentrate are discharged together by exporting, and amount to 20L, and wherein phenylglycine crystal is about 400g, and purity 93% uses
The centrifuge that revolving speed is 4000r/min recycles crystal, and the concentration of phenylglycine is 10mg/mL in remaining mother liquor, can return to
Reuse in pre-treatment step is walked, can be used for reacting synthesis Phenylglycine methyl ester after phenylglycine crystal recrystallization with methanol.
Embodiment 2
Enzyme process cefalexin crystalline mother solution 100L is taken, wherein cefalexin content is 15-18g/L, and mould is added thereto
Plain G acylase 10kg adjusts pH=5 with dilute sulfuric acid, and temperature reacts 5h under conditions of being 25 DEG C, obtains its cracking containing 7- ammonia
The lysate of base desacetoxycephalosporanic acid and phenylglycine, wherein phenylglycine 15-18g/L, cefalexin content are less than
1g/L, ammonium sulfate is about 100g/L, conductivity is about 10ms/cm, bod (COD) is about 200000mg/L, ammonia nitrogen
(NH3- N) it is about 30000mg/L, pH=6-7.Lysate pH to pH=3 is adjusted using dilute sulfuric acid, holding temperature is 25 DEG C standby
With.
Lysate 100L is taken to be centrifuged, revolving speed 8000r/min obtains 7-aminodesacetoxycephalosporanic acid
Crystal 1.35kg and liquid about 100L after centrifugation, liquid passes through rolling nanofiltration membrane after centrifugation, and operating pressure 3bar, temperature is less than 30
DEG C, add purified water 30L after operation 2 hours, obtains 10L concentrate and 120L permeate (filtering dialyzate), wherein concentrate COD
About 20000mg/L, ammonia nitrogen are about 10000mg/L, carry out biochemical treatment by discharge of pipes to environmental protection；Wherein permeate benzene is sweet
Propylhomoserin 5g/L or so, ammonium sulfate 83g/L or so.
Permeate 120L is taken to be passed through electric dialyzator, electric dialyzator uses 120 pairs of films, is passed through voltage 60V, and continuous operation 8h is de-
The small molecule salt in dialyzate is removed, liquid after desalination is obtained, small molecule salt is crystallized by evaporator and recycled, and 9kg or so is obtained
White crystal, purity is about 90%.
Liquid 120L after desalination is taken to carry out nanofiltration concentration, used film core is 150Da-500Da nanofiltration membrane core, operating pressure
25bar, running temperature are 30 DEG C, runing time 4h, obtain nanofiltration dislysate 100L, phenylglycine crystal and nanofiltration concentration
Liquid, wherein nanofiltration dislysate phenylglycine content is lower than 1g/L, pH=6-7, can return to desalting steps and applies, phenylglycine
Crystal and nanofiltration concentrate are discharged together by exporting, and amount to 20L, and wherein phenylglycine crystal is about 400g, and purity 93% uses
The centrifuge that revolving speed is 4000r/min recycles crystal, and the concentration of phenylglycine is 10mg/mL in remaining mother liquor, can return to
Reuse in pre-treatment step is walked, phenylglycine crystal can be used for reacting synthesis Phenylglycine methyl ester with methanol.
Embodiment 3
Enzyme process cefalexin crystalline mother solution 100L is taken, wherein cefalexin content is 15-18g/L, and mould is added thereto
Plain G acylase 10kg adjusts pH=9 with the ammonium hydroxide after dilution, and temperature reacts 1h under conditions of being 50 DEG C, contains its cracking
There is the lysate of 7-aminodesacetoxycephalosporanic acid and phenylglycine, wherein phenylglycine 15-18g/L, cefalexin contains
Amount be less than 1g/L, ammonium sulfate is about 100g/L, conductivity is about 10ms/cm, bod (COD) be about 200000mg/L,
Ammonia nitrogen (NH3- N) it is about 30000mg/L, pH=6-7.Lysate pH to pH=4 is adjusted using dilute sulfuric acid, holding temperature is 30 DEG C
It is spare.
Lysate 100L is taken to be centrifuged, revolving speed 5000r/min obtains 7-aminodesacetoxycephalosporanic acid
Crystal 1.02kg and liquid about 100L after centrifugation, by film filtering, (film core is the group of rolling ultrafiltration membrane and nanofiltration membrane to liquid after centrifugation
Close), operating pressure 20bar, temperature is 20 DEG C, adds purified water 30L after operation 2 hours, obtains 10L concentrate and 120L permeate
(filtering dialyzate), wherein concentrate COD is about 20000mg/L, and ammonia nitrogen is about 10000mg/L, by discharge of pipes to environmental protection
Carry out biochemical treatment；Wherein permeate phenylglycine 5g/L or so, ammonium sulfate 83g/L or so.
Permeate 120L is taken to cross ion exchange resin, flow velocity 3BV/H, continuous operation 4h sloughs the small molecule in dialyzate
Salt obtains liquid after desalination, and small molecule salt is crystallized by evaporator and recycled, and obtains the white crystal of 9kg or so, purity is about
90%.
Liquid 120L after desalination is taken to carry out nanofiltration concentration, used film core is 150Da-500Da nanofiltration membrane core, operating pressure
20bar, running temperature are 30 DEG C, runing time 4h, obtain nanofiltration dislysate 100L, phenylglycine crystal and nanofiltration concentration
Liquid, wherein nanofiltration dislysate phenylglycine content is lower than 1g/L, pH=6-7, can return to desalting steps and applies, phenylglycine
Crystal and nanofiltration concentrate are discharged together by exporting, and amount to 20L, and wherein phenylglycine crystal is about 400g, and purity 93% uses
The centrifuge that revolving speed is 4000r/min recycles crystal, and the concentration of phenylglycine is 10mg/mL in remaining mother liquor, can return to
Reuse in pre-treatment step is walked, phenylglycine crystal can be used for reacting synthesis Phenylglycine methyl ester with methanol.
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art are not departing from the principle of the present invention and objective
In the case where can make changes, modifications, alterations, and variations to the above described embodiments within the scope of the invention.
Claims (10)
1. the recoverying and utilizing method of phenylglycine in a kind of cefalexin crystalline mother solution, it is characterised in that: the following steps are included:
Cracking: penicillin G acylase is added into cefalexin crystalline mother solution, obtains its cracking containing 7- aminodeacetoxy oxygen
The lysate of base cephalosporanic acid, phenylglycine；The pH of lysate is adjusted to 3-5；
Centrifugation: lysate is centrifugally separating to obtain 7-aminodesacetoxycephalosporanic acid crystal and liquid after centrifugation, wherein revolving speed
For 4000-8000r/min, liquid carries out lower step after centrifugation；
Pretreatment: liquid after centrifugation is filtered by film, is obtained cracking concentrate and is filtered dialyzate, filtering dialyzate carries out down
Step；
Desalination: filtering dialyzate is passed through electric dialyzator or by ion exchange resin, sloughs the small molecule salt in dialyzate
Class, obtains liquid after desalination, and small molecule salt is recycled by evaporative crystallization；
Nanofiltration concentration: carrying out nanofiltration concentration for liquid after desalination, obtain nanofiltration dislysate, phenylglycine crystal and nanofiltration concentrate,
Wherein, nanofiltration dislysate is applied back to desalting steps, and phenylglycine crystal and nanofiltration concentrate are discharged together by exporting, recycling
Remaining mother liquor is returned into reuse in upper step pre-treatment step after phenylglycine crystal.
2. the recoverying and utilizing method of phenylglycine, feature in a kind of cefalexin crystalline mother solution according to claim 1
Be: the crack reacting condition is pH=5-9, and temperature reacts 1-5h under conditions of being 25-50 DEG C.
3. the recoverying and utilizing method of phenylglycine, feature in a kind of cefalexin crystalline mother solution according to claim 1
Be: it is 3-5 that the lysate, which adjusts its pH, and temperature is 25-30 DEG C of storage, with anti-metamorphic.
4. the recoverying and utilizing method of phenylglycine, feature in a kind of cefalexin crystalline mother solution according to claim 1
Be: the film core that film filters in the preprocessing process is that rolling ultrafiltration membrane or rolling nanofiltration membrane or rolling ultrafiltration membrane are received with rolling
Filter membrane is applied in combination, operating pressure 1bar-20bar.
5. the recoverying and utilizing method of phenylglycine, feature in a kind of cefalexin crystalline mother solution according to claim 1
Be: electrodialysis determines supplied DC voltage according to film logarithm in the desalination processes.
6. the recoverying and utilizing method of phenylglycine, feature in a kind of cefalexin crystalline mother solution according to claim 1
Be: X is to film supply 0.5X-X volt voltage.
7. the recoverying and utilizing method of phenylglycine, feature in a kind of cefalexin crystalline mother solution according to claim 1
Be: the desalination processes ion exchange resin flow velocity is 1-3BV/H.
8. the recoverying and utilizing method of phenylglycine, feature in a kind of cefalexin crystalline mother solution according to claim 1
Be: it is nanofiltration membrane core, operating pressure 15-25bar that used film core, which is concentrated, in the nanofiltration.
9. the recoverying and utilizing method of phenylglycine, feature in a kind of cefalexin crystalline mother solution according to claim 1
Be: the phenylglycine crystal is mixed with commercially available phenylglycine, synthesizes Phenylglycine methyl ester for reacting with methanol, or
React synthesis Phenylglycine methyl ester after recrystallization with methanol again.
10. the recoverying and utilizing method of phenylglycine, feature in a kind of cefalexin crystalline mother solution according to claim 1
Be: the temperature range of operation of film is 5-30 DEG C in the pretreatment, desalination and nanofiltration concentration process, single branch membrane component pressure difference
No more than 1bar.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105294734B (en) * | 2015-10-16 | 2018-02-13 | 华北制药河北华民药业有限责任公司 | A kind of method for preparing cefonicid dibenzylethylenediamsalt salt |
| CN106220646B (en) * | 2016-07-29 | 2018-08-24 | 华北制药河北华民药业有限责任公司 | A kind of method of enzymatic clarification cefalexin mother liquor recycled |
| CN110002650B (en) * | 2019-04-16 | 2020-05-08 | 同舟纵横（厦门）流体技术有限公司 | Method for treating nanofiltration dialysate of amoxicillin crystal mother liquor and/or 6-aminopenicillanic acid crystal mother liquor |
| CN110922417B (en) * | 2019-11-06 | 2022-03-15 | 天津大学 | Method for recovering cefalexin crystallization mother liquor |
| CN110922416B (en) * | 2019-11-06 | 2022-03-15 | 天津大学 | Method for recovering and purifying 7-aminodesacetoxycephalosporanic acid and phenylglycine in 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 |
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| 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 |
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| CN104058537A (en) * | 2014-04-30 | 2014-09-24 | 浙江工业大学 | Method for treating cefalexin enzyme-process synthesizing mother liquor wastewater |
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