CN101774709A - Treating method of ceftazidime mother liquor - Google Patents
Treating method of ceftazidime mother liquor Download PDFInfo
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- CN101774709A CN101774709A CN201010011645A CN201010011645A CN101774709A CN 101774709 A CN101774709 A CN 101774709A CN 201010011645 A CN201010011645 A CN 201010011645A CN 201010011645 A CN201010011645 A CN 201010011645A CN 101774709 A CN101774709 A CN 101774709A
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Abstract
The invention discloses a treating method for concentrating and separating ceftazidime mother liquor by using a membrane separation technology. The treating method mainly comprises the following steps: (1) carrying out pretreatment on the ceftazidime mother liquor to be treated, and removing fine suspended matters in the mother liquor; and (2) under the condition that the operation pressure is 0.5 to 4.0MPa, and the temperature is 10 to 80 DEG C, carrying out concentration and separation to a nanofiltration component for the ceftazidime mother liquor after pretreatment, obtaining concentrated liquor with the mass fraction of ceftazidime of more than 10 percent, collecting and then carrying out crystallization treatment; and the obtained permeate is discharged into a sewage treatment station for treatment. The treating method has the advantages of: effectively concentrating the ceftazidime mother liquor, not only recovering effective ingredient in the mother liquor, namely the ceftazidime, ensuring the quality of the ceftazidime, but also reducing the indexes of COD and BOD and the like discharged by the mother liquor, reducing the pollution and energy consumption, and having obvious economical and social benefits. The treating method can be widely applied in occasions needing to concentrate and recover the ceftazidime.
Description
Technical field
The present invention relates to a kind of method of utilizing membrane separation technique concentrating and separating solution, be specifically related to a kind of treatment process of ceftazidime mother liquor.
Background technology
Ceftazime is a third generation cephalosporin analog antibiotic, and sterilizing power is strong, and has a broad antifungal spectrum has the title of super broad-spectrum cephalosporin; In the antibiotic of clinical application at present, the strongest to the killing action of Pseudomonas aeruginosa, highly stable to β-Nei Xiananmei, its stability is apparently higher than Kefzol, cefuroxime, cefoperazone, cefotaxime etc.; Better tolerance, side effect is little, and indication is wide, comprises respiratory tract infection, urinary tract infection, gastrointestinal tract infection, biliary tract infection, abdominal infection, skin and soft tissue infection, otorhinolaryngology infection, B﹠J infection etc.; The patient who is used for moderate and severe infections is treatment gram positive bacterial infection urgent patient's a choice drug.Its medical injection is the aseptic mixture of ceftazidime pentahydrate and yellow soda ash.
The important compound of synthetic ceftazime is the ceftazime tert-butyl ester, and its synthetic method has active ester method, chloride method, mixed anhydride method, vilsmeier method and DCC condensation method.The at present normal active ester method that adopts, this method can be divided into two portions: the synthetic and bulk drug of side chain ester synthetic: with methyl aceto acetate process oximate, bromination, cyclization, etherificate, hydrolysis, dehydration, become technology such as ester, obtain BPTA; Synthesizing of bulk drug: reacted with pyridine under the effect of Iodotrimethylsilane by 7-ACA, generate 7-ACP, the latter is prepared into the 7-ACAP dihydrochloride through recrystallization, reacts with BPTA again, obtains the ceftazime tert-butyl ester.This method reaction conditions gentleness does not need the very low temperature reaction, and simple to operate, product is promptly separated out in the reaction process, and reaction solvent is single relatively.The ceftazime tert-butyl ester generates the ceftazime dihydrochloride through hydrolysis.Through further reaction, crystallization makes ceftazidime pentahydrate again.
Because synthesis route is long, the cost height, three-waste pollution is serious.Therefore cost of development is low, the yield height, and synthesis technique simple to operate, significant to the development of China's medicine industry.Ceftazime generally adopts the crystalline method to separate out from mother liquor, but the mother liquor of isolating after the crystallization still contains a certain amount of ceftazime, if directly as discharging of waste liquid, not only cause the waste of ceftazime, and because the existence of ceftazime causes COD and BOD higher, thereby the cost of increase sewage disposal.Adopt method of evaporating to concentrate to reclaim very big and quality product of ceftazime energy consumption to be affected.
Summary of the invention
At above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of treatment process of ceftazidime mother liquor, effectively concentrated solution, cut down the consumption of energy, reduce environmental pollution.
The present invention is achieved by the following technical solutions:
The treatment process of described ceftazidime mother liquor may further comprise the steps:
(1) pending ceftazidime mother liquor is carried out pre-treatment, remove the fine suspension in the mother liquor;
(2) be 0.5～4.0MPa at working pressure, temperature is under 10～80 ℃ the condition, pretreated ceftazidime mother liquor is carried out concentrating and separating with the nanofiltration assembly, and the massfraction of ceftazime reaches more than 10% in the gained concentrated solution, carries out crystallization treatment after the collection; Gained sees through liquid and discharges after solvent is reclaimed in rectifying, or directly enters the sewage works processing.
Above-mentioned pre-treatment is the tandem arrangement that adopts micro-filtration or micro-filtration and ultra-filtration equipment, and mother liquor is filtered; The working pressure of described pretreatment unit is 0.1-1.0MPa, and temperature is 10～80 ℃, and filtering accuracy is 1-10 μ m.Micro-filtration herein can adopt mechanical filter, accurate filter, deep bed filter, ceramic pipe type film or metal pipe type membrane filtration, ultra-filtration equipment can adopt hollow fiber film assembly, ceramic pipe type membrane module or rolling hyperfiltration membrane assembly, and its key is to guarantee to enter the membrane module that the ceftazidime mother liquor of concentrating and separating device can reach in the not serious polluting device and is as the criterion.
Described nanofiltration assembly comprises one-level nanofiltration assembly and secondary nanofiltration assembly, ceftazidime mother liquor is after one-level nanofiltration circulation concentrates, the ceftazime massfraction reaches the crystallization treatment of proceeding more than 10% in the concentrated solution, after the one-level nanofiltration sees through the liquid discharge, enter secondary nanofiltration assembly and carry out concentrating and separating, return one-level nanofiltration assembly after the concentrated solution circulation of secondary nanofiltration concentrates and continue to handle, the secondary nanofiltration enters sewage plant and handles after discharging through liquid.
Nanofiltration membrane material used among the present invention has: cellulose acetate, polymeric amide, polyimide, polysulfones, polyethersulfone, polyacrylonitrile, polyvinyl alcohol, polyvinylidene difluoride (PVDF), ceramic membrane or metallic membrane.
The method of the above-mentioned integrated membrane separation technique concentrating and separating of a kind of usefulness ceftazidime mother liquor, in order to make the operation steady in a long-term better of concentrating and separating device, behind the operation certain hour, can carry out routine cleaning to the major parts in the concentrating and separating device (being the nanofiltration assembly) with auxiliary cleaning system, can alleviate the pollution of film like this, promote the recovery of film properties.Auxiliary cleaning system is in stopped status when the concentrating and separating device normally moves; and when the concentrating and separating device moves for some time or pollutes to a certain degree; then out of service; starting auxiliary cleaning system cleans concentrated separation system; to recover the operating performance of concentrating and separating device, what each installed closes, moves by the valve automatic or manual.
One-level of the present invention or secondary nanofiltration concentrating and separating technology can concentrate well and reclaim in the ceftazidime mother liquor
Effective constituent is increased economic efficiency, and reduces cost of sewage disposal, reduces production costs.When handling the ceftazidime mother liquor of different concns, different membrane modules and process choice can be arranged, handle as proceeding the secondary nanofiltration one-level nanofiltration concentrated solution, to continue to improve the cycles of concentration of ceftazime, and other technical process is constant, this depends on the concentration of ceftazidime mother liquor, and the cost of the whole process flow operation many-sided factor of economic dispatch whether.
The invention has the beneficial effects as follows: can effectively concentrate ceftazidime mother liquor, effective constituent ceftazime in the both recyclable mother liquor, guarantee the quality of ceftazime, can reduce indexs such as the COD of mother liquor discharging and BOD again, reduce pollution and reduced energy consumption, had remarkable economic efficiency and social benefit.The present invention can be widely used in the occasion that needs concentrated and reclaimed ceftazime.
Description of drawings
Fig. 1 is an one-level concentrating and separating process flow sheet of the present invention.
Fig. 2 is a secondary concentrating and separating process flow sheet of the present invention.
Wherein, 1 raw water box, 2 topping-up pumps, 3 pretreatment units, 4 one-level cyclic water tanks, 5 one-level high-pressure pump, 6 one-level nanofiltration assemblies, 7 one-level nanofiltration concentrated solutions, 8 one-level nanofiltrations see through liquid, 9 secondary cyclic water tanks, 10 secondary high-pressure pump, 11 secondary nanofiltration assemblies, 12 secondary nanofiltration concentrated solutions, 13 secondary nanofiltrations see through liquid.
Embodiment
The invention will be further described below in conjunction with specific embodiment.
Embodiment 1
With content is 2%, pH=4, temperature is that 25 ℃ ceftazidime mother liquor places in the raw water box, with NaOH mother liquor pH is transferred to 8, this mother liquor is pumped into filtering accuracy by topping-up pump under the operational condition of pressure 0.2MPa be that the accurate filter of 5 μ m carries out pre-treatment, the mother liquor that comes out through pre-treatment enters the one-level cyclic water tank, under the working pressure of 1.8MPa, pump into one-level nanofiltration assembly by high-pressure pump again, ceftazime concentration can reach about 10% in the one-level nanofiltration concentrated solution, proceed crystallization treatment after the discharge system, the one-level nanofiltration sees through liquid and enters the secondary cyclic water tank, be forced into 1.5MPa by the secondary high-pressure pump again, enter secondary nanofiltration assembly and handle, return the one-level cyclic water tank after the concentrated solution circulation of secondary nanofiltration concentrates and handle again as feeding liquid, the secondary nanofiltration sees through liquid and enters the sewage plant processing.Move after one day, film is cleaned once, can recover the processing power more than 90%.
Embodiment 2
With content is 1%, pH=3.5, temperature is that 20 ℃ ceftazidime mother liquor places in the raw water box, with NaOH with mother liquor pH
Transfer to 7.5, this mother liquor is pumped into filtering accuracy by topping-up pump under the operational condition of pressure 0.3MPa be that the cloth envelop collector of 5 μ m carries out pre-treatment, the mother liquor that comes out through pre-treatment enters the one-level cyclic water tank, under the working pressure of 2.0MPa, pump into one-level nanofiltration assembly by high-pressure pump again, ceftazime concentration can reach about 10% in the one-level nanofiltration concentrated solution, proceed crystallization treatment after the discharge system, the one-level nanofiltration sees through liquid and enters the secondary cyclic water tank, be forced into 1.6MPa by the secondary high-pressure pump again, entering secondary nanofiltration assembly handles, return the one-level cyclic water tank after the concentrated solution circulation of secondary nanofiltration concentrates and handle again as feeding liquid, the secondary nanofiltration sees through liquid and enters the sewage plant processing.After moving a collection of feed liquid, to the film flushing once, can recover the processing power more than 90%.
Embodiment 3
With content is 1%, pH=4.5, temperature is that 30 ℃ ceftazidime mother liquor places in the raw water box, with NaOH mother liquor pH is transferred to 7.5, this ceftazidime mother liquor is pumped into filtering accuracy by topping-up pump under the operational condition of pressure 1.0MPa be that the ceramic membrane filter device of 0.5 μ m carries out pre-treatment, the mother liquor that comes out through pre-treatment enters the one-level cyclic water tank, under the working pressure of 2.3MPa, pump into one-level nanofiltration assembly by high-pressure pump again, ceftazime concentration can reach about 10% in the one-level nanofiltration concentrated solution, proceed crystallization treatment after the discharge system, the one-level nanofiltration sees through liquid and enters the sewage plant processing.After moving three batch of material liquid, film is cleaned once, can recover the processing power more than 90%.
What more than enumerate only is specific embodiments of the invention.Obviously, the invention is not restricted to the foregoing description, many operative combination can also be arranged.The all scenario that those of ordinary skill in the art can directly derive or associate from content disclosed by the invention all should be thought protection scope of the present invention.
Claims (4)
1. the treatment process of a ceftazidime mother liquor is characterized in that may further comprise the steps:
(1) pending ceftazidime mother liquor is carried out pre-treatment, remove the fine suspension in the mother liquor;
(2) be 0.5～4.0MPa at working pressure, temperature is under 10～80 ℃ the condition, pretreated mother liquor to be carried out concentrating and desalinating with the nanofiltration assembly, and the massfraction of ceftazime reaches more than 10% in the gained concentrated solution, proceeds crystallization treatment; Gained sees through liquid and discharges after treatment.
2. the treatment process of ceftazidime mother liquor according to claim 1, it is characterized in that: described pretreated device is a micro-filtration, or the tandem arrangement of micro-filtration and ultra-filtration equipment.
3. the treatment process of ceftazidime mother liquor according to claim 1 and 2, it is characterized in that: the working pressure of described pretreatment unit is 0.1-1.0MPa, and temperature is 10～80 ℃, and filtering accuracy is 1-10 μ m.
4. the treatment process of ceftazidime mother liquor according to claim 3, it is characterized in that: described nanofiltration assembly comprises one-level nanofiltration assembly and secondary nanofiltration assembly, ceftazidime mother liquor is after one-level nanofiltration circulation concentrates, the ceftazime massfraction reaches the crystallization treatment of proceeding more than 10% in the concentrated solution, after the one-level nanofiltration sees through the liquid discharge, enter secondary nanofiltration assembly and carry out concentrating and separating, return one-level nanofiltration assembly after the concentrated solution circulation of secondary nanofiltration concentrates and continue to handle, the secondary nanofiltration enters sewage plant through liquid and handles.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201010011645A CN101774709A (en) | 2010-01-21 | 2010-01-21 | Treating method of ceftazidime mother liquor |
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| CN201010011645A CN101774709A (en) | 2010-01-21 | 2010-01-21 | Treating method of ceftazidime mother liquor |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102060861A (en) * | 2010-11-04 | 2011-05-18 | 浙江工业大学 | Desalination concentration method for cephalo mother liquor |
| CN103788115A (en) * | 2014-03-03 | 2014-05-14 | 哈尔滨工业大学 | Method for concentrating cefalexin through membrane method and enzyme concentration method |
| CN105622617A (en) * | 2016-03-30 | 2016-06-01 | 广州白云山医药集团股份有限公司白云山化学制药厂 | Method for performing clean recovery on sildenafil citrate mother liquor |
| CN107722040A (en) * | 2017-10-10 | 2018-02-23 | 南京志坤环保科技有限公司 | A kind of membrane separating method and device for recycling ceftazidime mother liquor |
| CN108558908A (en) * | 2018-06-06 | 2018-09-21 | 华北制药河北华民药业有限责任公司 | A kind of desalination method of ceftazidime mother liquor and the preparation method of cefotaxime |
| CN108976246A (en) * | 2018-07-27 | 2018-12-11 | 华北制药河北华民药业有限责任公司 | A kind of processing method of ceftazidime mother liquor |
| CN110372115A (en) * | 2019-07-08 | 2019-10-25 | 伊犁川宁生物技术有限公司 | A kind of cephalo purifying process of waste water |
| CN110790460A (en) * | 2019-12-02 | 2020-02-14 | 中化(宁波)润沃膜科技有限公司 | Method for treating waste water in production of cephalosporin pharmaceutical intermediates |
| 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 |
-
2010
- 2010-01-21 CN CN201010011645A patent/CN101774709A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102060861A (en) * | 2010-11-04 | 2011-05-18 | 浙江工业大学 | Desalination concentration method for cephalo mother liquor |
| CN102060861B (en) * | 2010-11-04 | 2012-12-12 | 浙江工业大学 | Desalination concentration method for cephalo mother liquor |
| CN103788115A (en) * | 2014-03-03 | 2014-05-14 | 哈尔滨工业大学 | Method for concentrating cefalexin through membrane method and enzyme concentration method |
| CN103788115B (en) * | 2014-03-03 | 2016-03-16 | 哈尔滨工业大学 | A kind of integrated membrane process and concentrated enzyme process concentrate the method for Cephalexin Monohydrate Micro/Compacted |
| CN105622617B (en) * | 2016-03-30 | 2018-09-11 | 广州白云山医药集团股份有限公司白云山化学制药厂 | A method of sildenafil citrate mother liquor is subjected to cleaning recycling |
| CN105622617A (en) * | 2016-03-30 | 2016-06-01 | 广州白云山医药集团股份有限公司白云山化学制药厂 | Method for performing clean recovery on sildenafil citrate mother liquor |
| CN107722040A (en) * | 2017-10-10 | 2018-02-23 | 南京志坤环保科技有限公司 | A kind of membrane separating method and device for recycling ceftazidime mother liquor |
| CN108558908A (en) * | 2018-06-06 | 2018-09-21 | 华北制药河北华民药业有限责任公司 | A kind of desalination method of ceftazidime mother liquor and the preparation method of cefotaxime |
| CN108558908B (en) * | 2018-06-06 | 2019-11-29 | 华北制药河北华民药业有限责任公司 | A kind of desalination method of ceftazidime mother liquor and the preparation method of cefotaxime |
| CN108976246A (en) * | 2018-07-27 | 2018-12-11 | 华北制药河北华民药业有限责任公司 | A kind of processing method of ceftazidime mother liquor |
| CN110372115A (en) * | 2019-07-08 | 2019-10-25 | 伊犁川宁生物技术有限公司 | A kind of cephalo purifying process of waste water |
| CN110790460A (en) * | 2019-12-02 | 2020-02-14 | 中化(宁波)润沃膜科技有限公司 | Method for treating waste water in production of cephalosporin pharmaceutical intermediates |
| 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 |
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Open date: 20100714 |