CN101659684B - Method for recovering lincomycin from waste active carbon decolorized by lincomycin - Google Patents
Method for recovering lincomycin from waste active carbon decolorized by lincomycin Download PDFInfo
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- CN101659684B CN101659684B CN200910307481XA CN200910307481A CN101659684B CN 101659684 B CN101659684 B CN 101659684B CN 200910307481X A CN200910307481X A CN 200910307481XA CN 200910307481 A CN200910307481 A CN 200910307481A CN 101659684 B CN101659684 B CN 101659684B
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- lincomycin
- butanols
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Abstract
The invention discloses a method for recovering lincomycin from waste active carbon decolorized by lincomycin. The method comprises the following steps: washing decolorized waste active carbon by neutral or acid saturated butanol water or extracted waste liquor containing 5-10% butanol liquid or alkalization liquid and filtering, regulating pH of the filtrate by NaOH solution, and extracting and refining by butanol to recover lincomycin from decolorized waste active carbon. The method can help recover lincomycin from the waste active carbon decolorized by lincomycin, increase yield of lincomycin, and has great economical benefits and social benefits.
Description
Affiliated technical field
The invention belongs to pharmaceutical chemistry technical field, particularly relate to a kind of method that from the waste active carbon after the lincomycin decolouring, reclaims lincomycin.
Background technology
At present; Produce lincomycin in the process of refining decolouring; Waste active carbon after the use still contains a large amount of lincomycins and is difficult for washing and comes out after part butanols (butanols decolouring use gac) or purified water (water takes off the gac of use) washing in its useless charcoal, the flocculating aids when adding in fermented liquids these waste active carbons as Plate Filtration then; Back and filter cake are disposed as Hazardous wastes together, and extremely not obvious to the increase of pre-treatment yield; Also caused the loss of the lincomycin in the useless charcoal.
Summary of the invention
To above-mentioned situation, for overcoming the defective of prior art, the object of the invention just provides a kind of recovery method, from the waste active carbon after the lincomycin decolouring, to reclaim this part lincomycin.
The present invention is achieved in that it promptly is with neutrality or the saturated butanols water of tart; Or contain 5-10% butanols liquid with neutrality or tart; Or with isolating waste water in neutrality or the tart recovery butanols process; Or the waste liquid behind the lincomycin in the butyl alcohol extraction alkaline solution; Waste active carbon to after the decolouring washs and filters; Behind the NaOH adjust pH, extract and make with extra care with butanols again, thereby reclaim the lincomycin product in the useless charcoal in decolouring back.
For achieving the above object; The method that from the waste active carbon after the lincomycin decolouring, reclaims lincomycin according to the invention; This method be the lincomycin liquid concentrator through behind the activated carbon decolorizing or the solution after the meal dissolving through behind the activated carbon decolorizing or the waste active carbon of anti-stripping agent behind activated carbon decolorizing; With saturated butanols water contain 5-10% butanols liquid or the butyl alcohol extraction alkaline solution in behind the lincomycin waste liquid or reclaim isolating waste water in the butanols process; Waste active carbon is washed and filters, extract and make with extra care with butanols again, thereby reclaim the lincomycin in the useless charcoal in decolouring back.
For this reason, the method that from the waste active carbon after the lincomycin decolouring, reclaims lincomycin according to the invention specifically may further comprise the steps:
1., the water that the waste active carbon after the lincomycin decolouring is contained the 5-10% butanols with neutral or acidity; With 1: the volume ratio of 40-50 is mixed, and soaks and stirs 30-60min, and its water temperature is room temperature or is heated to 25-40 ℃; With pressure filter or Plate Filtration, get neutral or acid filtrate then;
2., above-mentioned filtrating is pressed into or pumps in extraction basin or the extraction tower, and regulate pH to 10～11.5, extract with butanols with 8mol/LNaOH solution, must extraction liquid;
3., above-mentioned extraction liquid being added volume ratio is 10: the purified water of 2-4 with 10mol/LHCl adjusting pH to 1.5-2.5, gets anti-stripping agent;
4., above-mentioned anti-stripping agent concentrated after, adding volume ratio is 10: the gac of 1-1.2 decolours, in destainer, adding volume ratio then is 1: the pure butanols of 9-10 carries out crystallization, filtration, oven dry, lincomycin.
The method that from the waste active carbon after the lincomycin decolouring, reclaims lincomycin according to the invention, can also reclaim with following concrete steps:
1., the water that the waste active carbon after the lincomycin decolouring is contained the 5-10% butanols with neutrality or tart is with 1: the volume ratio mixing of 40-50; Soak and stir 30-60min; Its water temperature is room temperature or is heated to 25-40 ℃, then with pressure filter or Plate Filtration, gets neutral or acid filtrate;
2., above-mentioned filtrating is regulated PH10-11.5 with 8mol/LNaOH be pressed into or pump in extraction basin or the extraction tower, extract with butanols, and open pressure lock and stir more than 30 minutes, the butanols extraction liquid;
3., above-mentioned butanols extraction liquid is concentrated or nanofiltration through the film under vacuum vaporizer, liquid concentrator;
4., with above-mentioned liquid concentrator again through activated carbon decolorizing, the butanols destainer;
5., with above-mentioned butanols destainer through alkali cleaning, carry out azeotropic, add the concentrated hydrochloric acid crystallization, meal (primary crystallization);
6., with after the oven dry of above-mentioned meal, with purified water it is dissolved again, add gac and carry out water and take off, water take off liquid;
7., water taken off liquid carry out the crystallization of low temperature acetone, and through oven dry, lincomycin.
Above-mentioned said recovery wash charcoal liquid, can concentrate recycling separately, also can merge recycling with the alkaline solution of normal fermentation filtered liq batch; The water of the useless charcoal of its washing can be neutrality, and also available hydrochloric acid (or oxalic acid or dilute sulphuric acid) transfers pH to become acid liquid, and simultaneously, the temperature of the useless charcoal water of washing can be a normal temperature, also can use steam-heated cal(l)andria, reclaims extracting and refining and gets product.
Wherein because the extraction solvent that uses is a butanols, then butanols extraction back waste water will reclaim butanols.
According to recovery method provided by the invention, can from the waste active carbon after the lincomycin decolouring, reclaim lincomycin, improve the output of lincomycin, have very big economic and social benefit.
Embodiment
The method that from the waste active carbon after the lincomycin decolouring, reclaims lincomycin according to the invention; This method be the lincomycin liquid concentrator through behind the activated carbon decolorizing or the solution after the meal dissolving through behind the activated carbon decolorizing or the waste active carbon of anti-stripping agent behind activated carbon decolorizing; With saturated butanols water contain 5-10% butanols liquid or the butyl alcohol extraction alkaline solution in behind the lincomycin waste liquid or reclaim isolating waste water in the butanols process; Waste active carbon is washed and filters; Extract and make with extra care with butanols again, thereby reclaim the lincomycin in the useless charcoal in decolouring back.
For this reason, the method that from the waste active carbon after the lincomycin decolouring, reclaims lincomycin according to the invention specifically may further comprise the steps:
1., the water that the waste active carbon after the lincomycin decolouring is contained the 5-10% butanols with neutral or acidity; With 1: the volume ratio of 40-50 is mixed, and soaks and stirs 30-60min, and its water temperature is room temperature or is heated to 25-40 ℃; With pressure filter or Plate Filtration, get neutral or acid filtrate then;
2., above-mentioned filtrating is pressed into or pumps in extraction basin or the extraction tower, and regulate pH to 10-11.5, extract with butanols with 8mol/LNaOH solution, must extraction liquid;
3., above-mentioned extraction liquid being added volume ratio is 10: the purified water of 2-4 with 10mol/LHCl adjusting pH to 1.5-2.5, gets anti-stripping agent;
4., above-mentioned anti-stripping agent concentrated after, adding volume ratio is 10: the gac of 1-1.2 decolours, in destainer, adding volume ratio then is 1: the pure butanols of 9-10 carries out crystallization, filtration, oven dry, lincomycin.
The method that from the waste active carbon after the lincomycin decolouring, reclaims lincomycin according to the invention, can also reclaim with following concrete steps:
1., the water that the waste active carbon after the lincomycin decolouring is contained the 5-10% butanols with neutrality or tart is with 1: the volume ratio mixing of 40-50; Soak and stir 30-60min; Its water temperature is room temperature or is heated to 25-40 ℃, then with pressure filter or Plate Filtration, gets neutral or acid filtrate;
2., above-mentioned filtrating is regulated PH10-11.5 with 8mol/LNaOH be pressed into or pump in extraction basin or the extraction tower, extract with butanols, and open pressure lock and stir more than 30 minutes, the butanols extraction liquid;
3., above-mentioned butanols extraction liquid is concentrated or nanofiltration through the film under vacuum vaporizer, liquid concentrator;
4., with above-mentioned liquid concentrator again through activated carbon decolorizing, the butanols destainer;
5., with above-mentioned butanols destainer through the NaOH alkali cleaning, carry out azeotropic, add the concentrated hydrochloric acid crystallization, meal (primary crystallization);
6., with after the oven dry of above-mentioned meal, with purified water it is dissolved again, add gac and carry out water and take off, water take off liquid;
7., water taken off liquid carry out the crystallization of low temperature acetone, and through oven dry, lincomycin.
Above-mentioned said recovery wash charcoal liquid, can concentrate recycling separately, also can merge recycling with the alkaline solution of normal fermentation filtered liq batch; The water of the useless charcoal of its washing can be neutrality, and also available hydrochloric acid (or oxalic acid or dilute sulphuric acid) transfers pH to become acid liquid, and simultaneously, the temperature of the useless charcoal water of washing can be a normal temperature, also can use steam-heated cal(l)andria, reclaims extracting and refining and gets product.
Wherein because the extraction solvent that uses is a butanols, then butanols extraction back waste water will reclaim butanols.
According to recovery method provided by the invention, can from the waste active carbon after the lincomycin decolouring, reclaim lincomycin, improve the output of lincomycin, have very big economic and social benefit.
Claims (4)
1. method that from the waste active carbon after the lincomycin decolouring, reclaims lincomycin is characterized in that this method specifically may further comprise the steps:
1., the water that the waste active carbon after the lincomycin decolouring is contained the 5-10% butanols with neutral or acidity; With 1: the volume ratio of 40-50 is mixed, and soaks and stirs 30-60min, and its water temperature is for being heated to 25-40 ℃; With pressure filter or Plate Filtration, get neutral or acid filtrate then;
2., above-mentioned filtrating is pressed into or pumps in extraction basin or the extraction tower, and regulate pH to 10-11.5, extract with butanols with 8mol/LNaOH solution, must extraction liquid;
3., above-mentioned extraction liquid being added volume ratio is 10: the purified water of 2-4 with 10mol/LHCl adjusting pH to 1.5-2.5, gets anti-stripping agent;
4., above-mentioned anti-stripping agent concentrated after, adding volume ratio is 10: the gac of 1-1.2 decolours, in destainer, adding volume ratio then is 1: the pure butanols of 9-10 carries out crystallization, filtration, oven dry, lincomycin.
2. method that from the waste active carbon after the lincomycin decolouring, reclaims lincomycin is characterized in that this method reclaims with following concrete steps:
1., the water that the waste active carbon after the lincomycin decolouring is contained the 5-10% butanols with neutrality or tart is with 1: 40～50 volume ratio mixing; Soak and stir 30-60min; Its water temperature then with pressure filter or Plate Filtration, gets neutral or acid filtrate for being heated to 25-40 ℃;
2., above-mentioned filtrating is regulated pH 10-11.5 with 8mol/LNaOH be pressed into or pump in extraction basin or the extraction tower, extract with butanols, and open pressure lock and stir more than 30 minutes, the butanols extraction liquid;
3., above-mentioned butanols extraction liquid is concentrated or nanofiltration through the film under vacuum vaporizer, liquid concentrator;
4., with above-mentioned liquid concentrator again through activated carbon decolorizing, the butanols destainer;
5., with above-mentioned butanols destainer through alkali cleaning, carry out azeotropic, add the concentrated hydrochloric acid crystallization, meal, primary crystallization;
6., with after the oven dry of above-mentioned meal, with purified water it is dissolved again, add gac and carry out water and take off, water take off liquid;
7., water taken off liquid carry out the crystallization of low temperature acetone, and through oven dry, lincomycin.
3. according to claim 1 or the 2 said methods that from the waste active carbons after the lincomycin decolouring, reclaim lincomycin, it is characterized in that the neutral or acid water that contains the 5-10% butanols in the step 1 is for neutral or transfer pH to become acid liquid with hydrochloric acid or oxalic acid or dilute sulphuric acid.
4. according to claim 1 or the 2 said methods that from the waste active carbon after the lincomycin decolouring, reclaim lincomycin, it is characterized in that butanols extraction back waste water will reclaim butanols.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910307481XA CN101659684B (en) | 2009-09-22 | 2009-09-22 | Method for recovering lincomycin from waste active carbon decolorized by lincomycin |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910307481XA CN101659684B (en) | 2009-09-22 | 2009-09-22 | Method for recovering lincomycin from waste active carbon decolorized by lincomycin |
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| CN101659684A CN101659684A (en) | 2010-03-03 |
| CN101659684B true CN101659684B (en) | 2012-02-22 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102079607B (en) * | 2010-11-24 | 2013-05-22 | 王冰 | Lincomycin wastewater advanced treatment and water recycling technology |
| CN111233953B (en) * | 2020-03-10 | 2021-04-20 | 福安药业集团烟台只楚药业有限公司 | Method for recycling activated carbon after gentamycin sulfate decoloration |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1066074A (en) * | 1992-03-26 | 1992-11-11 | 宜昌意腾制药有限公司 | The improvement of process of lincomycin extracted by menstruum method |
| CN1239100A (en) * | 1999-07-05 | 1999-12-22 | 亓平言 | Process for recovering lincomycin from filtered dregs of its fermented liquid |
| CN1056377C (en) * | 1998-01-22 | 2000-09-13 | 清华大学 | Extracting and purifying of antibiotics using naphthenic acid extractive system |
-
2009
- 2009-09-22 CN CN200910307481XA patent/CN101659684B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1066074A (en) * | 1992-03-26 | 1992-11-11 | 宜昌意腾制药有限公司 | The improvement of process of lincomycin extracted by menstruum method |
| CN1056377C (en) * | 1998-01-22 | 2000-09-13 | 清华大学 | Extracting and purifying of antibiotics using naphthenic acid extractive system |
| CN1239100A (en) * | 1999-07-05 | 1999-12-22 | 亓平言 | Process for recovering lincomycin from filtered dregs of its fermented liquid |
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| CN101659684A (en) | 2010-03-03 |
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Inventor after: Li Jingren Inventor after: Liu Huaiju Inventor after: Zhao Qing Inventor after: Li Yanbo Inventor after: Li Hongde Inventor after: Xia Hanqing Inventor after: Zhang Jinglin Inventor after: Qu Xiuhua Inventor after: Xue Gang Inventor before: Li Jingren Inventor before: Li Yanbo Inventor before: Zhao Qing Inventor before: Li Hongde Inventor before: Qu Xiuhua Inventor before: Xue Gang |
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Free format text: CORRECT: INVENTOR; FROM: LI JINGREN LI YANBO ZHAO QING LI HONGDE QU XIUHUA XUE GANG TO: LI JINGREN LIU HUAIJU ZHAO QING LI YANBO LI HONGDE XIA HANQING ZHANG JINGLIN QU XIUHUA XUE GANG |
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Granted publication date: 20120222 Termination date: 20140922 |
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