CN101671302B - Production process of enrofloxacin antibacterial drug for fowl and livestock - Google Patents
Production process of enrofloxacin antibacterial drug for fowl and livestock Download PDFInfo
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- CN101671302B CN101671302B CN2008102207792A CN200810220779A CN101671302B CN 101671302 B CN101671302 B CN 101671302B CN 2008102207792 A CN2008102207792 A CN 2008102207792A CN 200810220779 A CN200810220779 A CN 200810220779A CN 101671302 B CN101671302 B CN 101671302B
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- ethanol
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- ciprofloxacin
- enrofloxacin
- fowl
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Abstract
The invention relates to the technical field of medicines for fowl and livestock, in particular to a production process of an enrofloxacin antibacterial drug for fowl and livestock. The production process comprises the following steps: ethylation, hydrolyzation and neutralization. The enrofloxacin antibacterial drug comprises the following raw materials in proportion by weight: 1-1.5 ciprofloxacin, 0.33-1 ethylating agent, 4-6 ethanol with the concentration of 95 percent, 20-22 distilled water, 1-1.3 potassium hydroxide and 1-1.5 sulphuric acid. In the production process of the enrofloxacin antibacterial drug for fowl and livestock, a methanol menstruum in the original process is changed into the ethanol with the concentration of 95 percent; a catalyst does not need adding so that the environmental pollution and the harm to working personnel are avoided; more importantly, the reaction yield is improved by 3 percent than that of the original process, therefore, the production cost can be greatly reduced, and the yield and the competitiveness of the product can be improved.
Description
Technical field
The present invention relates to the production technique of fowl domestic animals medicine technical field, particularly a kind of enrofloxacin antibacterial drug for fowl and livestock.
Background technology
Fowl poultry medication Enrofloxacin (Enrofloxacin) has has a broad antifungal spectrum, characteristics that antimicrbial power is strong, is subjected to user's welcome deeply.This medicine is raw material with the Ciprofloxacin, in addition ethylating agent, catalyzer, methyl alcohol, potassium hydroxide, the vitriol oil; Make Enrofloxacin through operations such as ethylization, hydrolysis, neutralizations.In existing manufacturing technique, used methyl alcohol and expensive catalysts, these material contaminate environment, and to the staff poison greatly, production cost is high, do not have competitive power.
Summary of the invention
The objective of the invention is provides a kind of free from environmental pollution, the production technique of the enrofloxacin antibacterial drug for fowl and livestock that production cost is low in order to overcome the deficiency that above-mentioned prior art exists.
For achieving the above object, the technical scheme that the present invention takes is: the production technique of this enrofloxacin antibacterial drug for fowl and livestock, comprise ethylization operation, hydrolysis and in and operation, specifically as follows:
(1) raw material and weight ratio thereof
Ciprofloxacin 1～1.5 ethylating agent 0.33～1 95% ethanol 4～6
Distilled water 20～22 potassium hydroxide 1～1.3 sulfuric acid 1～1.5
(2) production technique step in the following order:
1. vacuum suction concentration 95% ethanol in the ethylation reaction jar adds Ciprofloxacin, stirs to make it molten entirely in 50 minutes;
2. vacuum suction ethylating agent in the gauger; At room temperature, ethylating agent is added dropwise in the retort, rate of addition is 1kg/ minute;
3. drain the jacket water (J.W.) of retort, open and be steam heated to backflow, back flow reaction 1 hour;
4. decompression steams three minutes two ethanol, and the Ciprofloxacin thick liquid obtains ethylizing; The ethanol that steams is stored in the basin;
5. the ethylization Ciprofloxacin thick liquid that obtains suddenly of vacuum drawn previous step adds potassium hydroxide to hydrolysis that fills distilled water and neutralization reaction jar; Drain the water in this retort chuck, open steam and under agitation be heated to backflow, back flow reaction 1.5 hours;
6. steam off is opened jacket water (J.W.) and is cooled to 50 ℃, closes water again, drains the water in the chuck, and open cold liquid is cooled to 25 ℃;
7. the sulfuric acid of vacuum suction under agitation carries out neutralization reaction, regulates the pH value to neutral, leaves standstill 30 minutes;
8. blowing, centrifuging; Clean retort with distilled water, centrifuging is collected filtrate in waste liquid pool;
9. extremely do not contain SO with the distilled water wash filter cake
2- 4Ion, washing water are incorporated in the waste liquid pool;
10. filter cake vacuum-drying is chemically examined and is pulverized after qualified, weighing, pack finished product.
Described raw material and weight ratio thereof are:
Ciprofloxacin 1 ethylating agent 0.33 95% ethanol 4
Distilled water 20 potassium hydroxide 1.2 sulfuric acid 1
The production technique of enrofloxacin antibacterial drug for fowl and livestock of the present invention, with the solvent in original technology--it is 95% ethanol that methyl alcohol changes concentration into; Need not add catalyzer, avoid environmental pollution and, the more important thing is the raising 3% of reaction yield, therefore can reduce production costs significantly, improve output, thereby improved competitiveness of product than original technology to staff's infringement.
Description of drawings
Fig. 1 is a process flow sheet of the present invention.
Embodiment
Raw material of the present invention: Ciprofloxacin (content 〉=99%), ethylating agent (industry), 95% ethanol (industry), potassium hydroxide (industry), 〉=90% sulfuric acid (industry), batching is got all the ready, begins to feed intake under equipment operation is normal.Production craft step is as follows:
(1) vacuum suction 300kg concentration is 95% ethanol in the ethylation reaction jar, adds the 75kg Ciprofloxacin, stirs to make it molten entirely in 50 minutes;
(2) vacuum suction 25kg ethylating agent in the gauger, at room temperature condition is added dropwise to the 25kg ethylating agent in the retort, and rate of addition is the 1kg/ per minute;
(3) drain the retort jacket water (J.W.), open and be steam heated to backflow, back flow reaction 1 hour;
(4) (vacuum tightness 0.04～0.08Mpa) steams 200kg ethanol, and the Ciprofloxacin thick liquid obtains ethylizing in decompression; The 200kg ethanol that collection steams is in accumulator tanks;
(5) the ethylization Ciprofloxacin thick liquid that obtains suddenly of vacuum drawn previous step to hydrolysis that fills 1500kg distilled water and neutralization reaction jar, adds 90kg potassium hydroxide; Drain the water in this retort chuck, open steam, reflux under agitation, back flow reaction 1.5 hours;
(6) steam off is opened jacket water (J.W.) and is cooled to 50 ℃, closes water again, drains the water in the chuck, and open cold liquid is cooled to 25 ℃;
(7) under agitation, vacuum suction 75kg sulfuric acid (concentration 〉=90%) carries out neutralization reaction, and regulates its pH value to neutral, leaves standstill 30 minutes;
(8) blowing, centrifuging; Clean retort with distilled water,, collect filtrate in waste liquid pool through centrifuging;
(9) extremely do not contain SO with the distilled water wash filter cake
2- 4Ion, washing water are incorporated in the waste liquid pool;
(10) filter cake vacuum-drying is 6 hours; Chemical examination water content 0.8% behind the salable product of content 99.1%, is pulverized; Get the 77.5kg Enrofloxacin, pack.
Finished product recovery rate calculation formula:
By formula calculating finished product output is 77.5kg, and yield is 95.2%.
Claims (2)
1. the production technique of an enrofloxacin antibacterial drug for fowl and livestock, comprise ethylization operation, hydrolysis and in and operation, it is characterized in that as follows:
(1) raw material and weight ratio thereof
Ciprofloxacin 1～1.5 ethylating agent 0.33～1 95% ethanol 4～6
Distilled water 20～22 potassium hydroxide 1～1.3 sulfuric acid 1～1.5
(2) production technique step in the following order:
1. vacuum suction concentration 95% ethanol in the ethylation reaction jar adds Ciprofloxacin, stirs to make it molten entirely in 50 minutes;
2. vacuum suction ethylating agent in the gauger; At room temperature, ethylating agent is added dropwise in the retort, rate of addition is 1kg/ minute;
3. drain the jacket water (J.W.) of retort, open and be steam heated to backflow, back flow reaction 1 hour;
4. decompression steams 2/3rds ethanol, and the Ciprofloxacin thick liquid obtains ethylizing; The ethanol that steams is stored in the basin;
5. the ethylization Ciprofloxacin thick liquid that obtains suddenly of vacuum drawn previous step adds potassium hydroxide to hydrolysis that fills distilled water and neutralization reaction jar; Drain the water in this retort chuck, open steam and under agitation be heated to backflow, back flow reaction 1.5 hours;
6. steam off is opened jacket water (J.W.) and is cooled to 50 ℃, closes water again, drains the water in the chuck, and open cold liquid is cooled to 25 ℃;
7. the sulfuric acid of vacuum suction under agitation carries out neutralization reaction, regulates the pH value to neutral, leaves standstill 30 minutes;
8. blowing, centrifuging; Clean retort with distilled water, centrifuging is collected filtrate in waste liquid pool;
9. extremely do not contain SO with the distilled water wash filter cake
4 2-Ion, washing water are incorporated in the waste liquid pool;
10. filter cake vacuum-drying is chemically examined and is pulverized after qualified, weighing, pack finished product.
2. according to the production technique of the described enrofloxacin antibacterial drug for fowl and livestock of claim 1, it is characterized in that described raw material and weight ratio thereof are:
Ciprofloxacin 1 ethylating agent 0.33 95% ethanol 4
Distilled water 20 potassium hydroxide 1.2 sulfuric acid 1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102207792A CN101671302B (en) | 2008-12-30 | 2008-12-30 | Production process of enrofloxacin antibacterial drug for fowl and livestock |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102207792A CN101671302B (en) | 2008-12-30 | 2008-12-30 | Production process of enrofloxacin antibacterial drug for fowl and livestock |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101671302A CN101671302A (en) | 2010-03-17 |
| CN101671302B true CN101671302B (en) | 2011-03-30 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2008102207792A Expired - Fee Related CN101671302B (en) | 2008-12-30 | 2008-12-30 | Production process of enrofloxacin antibacterial drug for fowl and livestock |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109574924A (en) * | 2019-01-16 | 2019-04-05 | 浙江国邦药业有限公司 | A kind of Enrofloxacin raffinate recoverying and utilizing method |
| CN113717101A (en) * | 2021-08-30 | 2021-11-30 | 深圳市博林达科技有限公司 | Purification process for enrofloxacin |
| CN115166077A (en) * | 2022-07-01 | 2022-10-11 | 中国水产科学研究院东海水产研究所 | Double internal standard reagent for determination of enrofloxacin residue in aquatic product and detection method |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0274033A1 (en) * | 1986-12-03 | 1988-07-13 | Bayer Ag | Process for the preparation of quinolinecarboxylic acids |
| CN88101907A (en) * | 1987-04-08 | 1988-10-26 | 奇诺英药物化学工厂有限公司 | Process for preparing quinoline carboxylic acids |
| CN1097751A (en) * | 1994-06-10 | 1995-01-25 | 南京药物研究所 | The 6-fluoro quinoline keto-acid antibiotic derivative |
| US20040073030A1 (en) * | 2000-05-09 | 2004-04-15 | Pulla Reddy Muddasani | Process for the preparation of quinolone derivatives |
-
2008
- 2008-12-30 CN CN2008102207792A patent/CN101671302B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0274033A1 (en) * | 1986-12-03 | 1988-07-13 | Bayer Ag | Process for the preparation of quinolinecarboxylic acids |
| CN88101907A (en) * | 1987-04-08 | 1988-10-26 | 奇诺英药物化学工厂有限公司 | Process for preparing quinoline carboxylic acids |
| CN1097751A (en) * | 1994-06-10 | 1995-01-25 | 南京药物研究所 | The 6-fluoro quinoline keto-acid antibiotic derivative |
| US20040073030A1 (en) * | 2000-05-09 | 2004-04-15 | Pulla Reddy Muddasani | Process for the preparation of quinolone derivatives |
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| CN101671302A (en) | 2010-03-17 |
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Granted publication date: 20110330 Termination date: 20121230 |