CN102199179A - Method for purifying and recycling feed liquid from erythromycin produced by fermentation method - Google Patents
Method for purifying and recycling feed liquid from erythromycin produced by fermentation method Download PDFInfo
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- CN102199179A CN102199179A CN2011100607646A CN201110060764A CN102199179A CN 102199179 A CN102199179 A CN 102199179A CN 2011100607646 A CN2011100607646 A CN 2011100607646A CN 201110060764 A CN201110060764 A CN 201110060764A CN 102199179 A CN102199179 A CN 102199179A
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Abstract
The invention belongs to the field of purifying and recycling pharmaceutical wastewater and specifically relates to a method for purifying and recycling a feed liquid from erythromycin produced by the fermentation method. The method provided by the invention is characterized by adsorbing Alpha-erythromycin in the feed liquid by using multistage resin; eluting the resin by using an eluant; adjusting the eluate with its pH value being from 7 to 10 and its water content being less than or equal to 20 wt%; precipitating and crystallizing erythromycin by using a precipitating agent or the hydrolysis control method, followed by cleaning and centrifugation; and drying the solid substance produced by the centrifugation step at a low temperature to obtain erythromycin. The method provided by the invention has advantages of low operation cost, convenient operation, reliable and flexible technology control, accomplishes the purpose of effectively obtaining the target substance by the solid phase extraction (adsorption) principle, effectively separates drug residuals in pharmaceutical factory wastewater from other contained substances to highly purify the wastewater, wherein the erythromycin content is lower than 1ppm and superior to national wastewater discharge standards, is friendly to environment, and produces no second pollution.
Description
Technical field
The invention belongs to the purification and the recycling field of pharmacy waste water, be specifically related to a kind of method that purifies and recycle fermentative Production erythromycin feed liquid.
Background technology
In the technological process of fermentative Production erythromycin bulk drug, to the extraction of the fermented feed liquid operation that is absolutely necessary, the remaining fresh feed liquid of this operation (waste water), the erythromycin that contains the about 0.1 ~ 0.3%wt of residual quantity, comprehensive content is up to the amino acid of 1 ~ 3%wt, and the solvent (N-BUTYL ACETATE) that has reached solubleness saturated level 0.7 %wt.In industry with fermentative Production erythromycin bulk drug, producing this type of waste water of 300 tons every year, nearly 20,000 tons of solvent (N-BUTYL ACETATE) loss amount, and annual amino acid whose loss amount is more up to 100,000 tons.In decades, the sector is not carried out recycling to this type of waste water, and huge waste is startling.And in former all research work to this feed liquid, all be round the oxidation of waste water and the adjustment of pH value, fundamentally do not solve environmental issue, also resource has been caused huge waste.
Summary of the invention
The object of the present invention is to provide a kind of method that purifies and recycle fermentative Production erythromycin feed liquid.
The object of the present invention is achieved like this: a kind of method that purifies and recycle fermentative Production erythromycin feed liquid, it is characterized in that: adopt the α-erythromycin in the described feed liquid of multistage resin absorption, behind the described resin of eluent wash-out, the pH value of adjusting elutriant is 7 ~ 10 and adjust the water content≤20%wt of elutriant, adopt precipitation agent or control hydrolysis method to separate out and crystallization erythromycin then, cleaning, centrifugation obtain erythromycin with centrifugation gained solid substance oven drying at low temperature.
Above-mentioned control hydrolysis method separates out and the crystalline method erythromycin for Heating temperature and the time and the pH value of control elutriant after above-mentioned adjustment from elutriant.
The present invention purifies and recycles the method for fermentative Production erythromycin feed liquid, present all fermentative production erythromycin enterprise bacterium slags and a processing difficult problem that extracts the last feed liquid of erythromycin have been solved, fully recycled resources such as the protein that is rich in bacterium slag and the waste liquid, amino acid, remaining erythromycin, realized discharging simultaneously the zero environmental thing.The erythromycin instability, oxidized easily that pharmaceutical use is arranged, separation and Extraction contriver at medicinal active erythromycin in the bacterium slag has passed through great deal of experimental and theoretical analysis, finally adopted multistage resin absorption and the control hydrolysis in the inventive method the erythromycin that pharmaceutical use is arranged to be carried out separation and Extraction, obtained the high purity erythromycin of pharmaceutical use with combining of technique means such as crystallizations.
In order to adsorb the α-erythromycin in the fermentative Production erythromycin feed liquid waste water better, the preferred macropore nonpolar adsorption resin of above-mentioned multistage resin preferably adopts D-1300, D-4020, XDA-1 or XD-61 macroporous adsorbent resin; For the activity of the erythromycin that keeps having pharmaceutical use better, further preferred XDA-1 or the D-4020 resin of adopting of described macroporous adsorbent resin.
In order to obtain higher, the active erythromycin that better has pharmaceutical use of purity, above-mentioned eluent preferably adopts methyl alcohol, ethanol or acetone, further preferably adds the eluent that accounts for the preparation of acetone volume 10 ~ 20% distilled water in other acetone of analytical pure level.
In order further to obtain higher, the active erythromycin that better has pharmaceutical use of purity, the water content of above-mentioned adjustment elutriant is preferably 15～20%wt; Above-mentioned control hydrolysis method is preferably adjusted pH value to 9 ~ 10.5 of elutriant, and elutriant is heated to 40 ~ 50 ℃ and be incubated 2 ~ 4h, separates out and crystallization erythromycin; Above-mentioned cleaning is preferably carried out secondary with 50 ℃ of distilled water and is cleaned; The temperature condition of above-mentioned oven drying at low temperature preferably is not higher than 50 ℃, further preferably obtains erythromycin with Vacuumdrier oven dry under not being higher than 50 ℃.
In order fully to reclaim and the resource of utilizing in the erythromycin feed liquid, preferably will go out amino acid with membrane separating through feed liquid waste water behind above-mentioned multistage resin absorption α-erythromycin and above-mentioned centrifugation gained liquid, the fractional distillation method is isolated N-BUTYL ACETATE and eluent, and gained liquid enters water discharging up to standard pond after the membrane separating; When above-mentioned eluent was acetone, the temperature range of described fractional distillation method was 50 ~ 130 ℃.
Specifically, a kind of method that purifies and recycle fermentative Production erythromycin feed liquid, carry out as follows: adopt the α-erythromycin in XDA-1 or the described feed liquid of D-4020 resin absorption, behind the described resin of eluent wash-out that in other acetone of analytical pure level, adds the distilled water preparation that accounts for acetone volume 10 ~ 20%, the pH value of adjusting elutriant 7 ~ 10 and the water content of adjusting elutriant at 15～20%wt, adjust pH value to 9 ~ 10.5 of elutriant again, elutriant is heated to 40 ~ 50 ℃ and be incubated 2 ~ 4h, separate out and crystallization erythromycin, carrying out secondary with 50 ℃ of distilled water at last cleans, centrifugation obtains erythromycin with the oven dry under Vacuumdrier is not higher than 50 ℃ of centrifugation gained solid substance.
The beneficial effect that the present invention has:
The inventive method running cost is low, handled easily, technology controlling and process is reliably flexible, adopts Solid-Phase Extraction (absorption) principle, has realized effectively seizing the purpose of target substance, carried out effective the separation to the medicine in pharmaceutical factory's " waste water " is residual with other contained material, make waste water obtain high purification, wherein erythromycin content is lower than 1ppm, is better than national wastewater discharge standard, environmentally friendly, non-secondary pollution produces.
The inventive method has also realized the innoxious recycling all sidedly of fermentative Production erythromycin feed liquid, it is pure to separate the erythromycin and the amino acid product that obtain by the inventive method, effectively separation and Extraction the solvent N-BUTYL ACETATE, reclaimed eluent, saved resource.
Description of drawings
Fig. 1 is the schematic flow sheet of the inventive method.
Embodiment
In conjunction with the accompanying drawings; below by embodiment the present invention is carried out concrete description; be necessary to be pointed out that at this following examples only are used for the present invention is further specified; can not be interpreted as limiting the scope of the invention, those skilled in the art can make some nonessential improvement and adjustment to the present invention according to the invention described above content.
Embodiment 1A kind of method that purifies and recycle fermentative Production erythromycin feed liquid, it is characterized in that: adopt the α-erythromycin in the described feed liquid of XDA-1 resin absorption, after in other acetone of analytical pure level, adding the described resin of eluent wash-out that accounts for the preparation of acetone volume 15% distilled water, the pH value of adjusting elutriant be 8 and the water content of adjusting elutriant be 18%wt, adjust the pH value to 9.5 of elutriant again, elutriant is heated to 45 ℃ and be incubated 3h, separate out and crystallization erythromycin, carrying out secondary with 50 ℃ of distilled water at last cleans, centrifugation obtains erythromycin with centrifugation gained solid substance in Vacuumdrier oven dry under 50 ℃.
Purity and hygienic requirements in view of product, fermentative Production erythromycin feed liquid extraction wastewater is from the extraction process (extractor) of pharmaceutical factory is transported to material liquid tank in the processing technological flow by closed conduct in, the follow-up treatment process of this example is totally-enclosed process, do not bring secondary pollution, health is reliable, simultaneously, erythromycin content is lower than 1ppm in the fermentative Production erythromycin feed liquid waste water after this example is handled, and is better than national wastewater discharge standard.
Embodiment 2A kind of method that purifies and recycle fermentative Production erythromycin feed liquid, it is characterized in that: adopt the α-erythromycin in the described feed liquid of D-4020 resin absorption, after in other acetone of analytical pure level, adding the described resin of eluent wash-out that accounts for the preparation of acetone volume 10% distilled water, the pH value of adjusting elutriant 7 and the water content of adjusting elutriant at 15%wt, adjust the pH value to 9 of elutriant again, elutriant is heated to 50 ℃ and be incubated 2h, separate out and crystallization erythromycin, carrying out secondary with 50 ℃ of distilled water at last cleans, centrifugation obtains erythromycin with the oven dry under not being higher than 50 ℃ of centrifugation gained solid substance.
Purity and hygienic requirements in view of product, fermentative Production erythromycin feed liquid extraction wastewater is from the extraction process (extractor) of pharmaceutical factory is transported to material liquid tank in the processing technological flow by closed conduct in, the follow-up treatment process of this example is totally-enclosed process, do not bring secondary pollution, health is reliable, simultaneously, erythromycin content is lower than 1ppm in the fermentative Production erythromycin feed liquid waste water after this example is handled, and is better than national wastewater discharge standard.
Embodiment 3A kind of method that purifies and recycle fermentative Production erythromycin feed liquid, it is characterized in that: adopt the α-erythromycin in the described feed liquid of D-1300 resin absorption, after in other acetone of analytical pure level, adding the described resin of eluent wash-out that accounts for the preparation of acetone volume 20% distilled water, the pH value of adjusting elutriant 10 and the water content of adjusting elutriant at 20%wt, adjust the pH value to 10.5 of elutriant again, elutriant is heated to 40 ℃ and be incubated 4h, separate out and crystallization erythromycin, carrying out secondary with 50 ℃ of distilled water at last cleans, centrifugation obtains erythromycin with the oven dry under Vacuumdrier is not higher than 50 ℃ of centrifugation gained solid substance.
Purity and hygienic requirements in view of product, fermentative Production erythromycin feed liquid extraction wastewater is from the extraction process (extractor) of pharmaceutical factory is transported to material liquid tank in the processing technological flow by closed conduct in, the follow-up treatment process of this example is totally-enclosed process, do not bring secondary pollution, health is reliable, simultaneously, erythromycin content is lower than 1ppm in the fermentative Production erythromycin feed liquid waste water after this example is handled, and is better than national wastewater discharge standard.
Embodiment 4A kind of method that purifies and recycle fermentative Production erythromycin feed liquid, it is characterized in that: adopt the α-erythromycin in the described feed liquid of XD-61 resin absorption, behind the described resin of methanol-eluted fractions, the pH value of adjusting elutriant 8 and the water content of adjusting elutriant at 12%wt, add precipitation agent lactic acid, separate out and crystallization erythromycin, cleaning, centrifugation obtain erythromycin with the oven dry under 35 ℃ of centrifugation gained solid substance.
Purity and hygienic requirements in view of product, fermentative Production erythromycin feed liquid extraction wastewater is from the extraction process (extractor) of pharmaceutical factory is transported to material liquid tank in the processing technological flow by closed conduct in, the follow-up treatment process of this example is totally-enclosed process, do not bring secondary pollution, health is reliable, simultaneously, erythromycin content is lower than 1ppm in the fermentative Production erythromycin feed liquid waste water after this example is handled, and is better than national wastewater discharge standard.
Embodiment 5A kind of method that purifies and recycle fermentative Production erythromycin feed liquid, it is characterized in that: adopt the α-erythromycin in the described feed liquid of XD-61 resin absorption, behind the described resin of ethanol elution, the pH value of adjusting elutriant 8 and the water content of adjusting elutriant at 19%wt, again elutriant is heated to 38 ℃ and be incubated 4.5h, separate out and crystallization erythromycin, cleaning, centrifugation obtain erythromycin with the oven dry under 35 ℃ of centrifugation gained solid substance.
Purity and hygienic requirements in view of product, fermentative Production erythromycin feed liquid extraction wastewater is from the extraction process (extractor) of pharmaceutical factory is transported to material liquid tank in the processing technological flow by closed conduct in, the follow-up treatment process of this example is totally-enclosed process, do not bring secondary pollution, health is reliable, simultaneously, erythromycin content is lower than 1ppm in the fermentative Production erythromycin feed liquid waste water after this example is handled, and is better than national wastewater discharge standard.
Embodiment 6A kind of method that purifies and recycle fermentative Production erythromycin feed liquid, it is characterized in that: adopt the α-erythromycin in the described feed liquid of XDA-1 resin absorption, behind the described resin of ethanol elution, the pH value of adjusting elutriant 8 and the water content of adjusting elutriant at 19%wt, adjust the pH value to 8.5 of elutriant again, elutriant is heated to 38 ℃ and be incubated 4.5h, separate out and crystallization erythromycin, cleaning, centrifugation obtain erythromycin with the oven dry under 35 ℃ of centrifugation gained solid substance.
Purity and hygienic requirements in view of product, fermentative Production erythromycin feed liquid extraction wastewater is from the extraction process (extractor) of pharmaceutical factory is transported to material liquid tank in the processing technological flow by closed conduct in, the follow-up treatment process of this example is totally-enclosed process, do not bring secondary pollution, health is reliable, simultaneously, erythromycin content is lower than 1ppm in the fermentative Production erythromycin feed liquid waste water after this example is handled, and is better than national wastewater discharge standard.
Embodiment 7A kind of method that purifies and recycle fermentative Production erythromycin feed liquid, it is characterized in that: adopt the α-erythromycin in the described feed liquid of XDA-1 resin absorption, after in other acetone of analytical pure level, adding the described resin of eluent wash-out that accounts for the preparation of acetone volume 10 ~ 20% distilled water, the pH value of adjusting elutriant 8 and the water content of adjusting elutriant at 19%wt, adjust the pH value to 8.5 of elutriant again, elutriant is heated to 38 ℃ and be incubated 4.5h, separate out and crystallization erythromycin, clean, centrifugation obtains erythromycin with the oven dry under 35 ℃ of centrifugation gained solid substance.
Purity and hygienic requirements in view of product, fermentative Production erythromycin feed liquid extraction wastewater is from the extraction process (extractor) of pharmaceutical factory is transported to material liquid tank in the processing technological flow by closed conduct in, the follow-up treatment process of this example is totally-enclosed process, do not bring secondary pollution, health is reliable, simultaneously, erythromycin content is lower than 1ppm in the fermentative Production erythromycin feed liquid waste water after this example is handled, and is better than national wastewater discharge standard.
Embodiment 8A kind of method that purifies and recycle fermentative Production erythromycin feed liquid, it is characterized in that: adopt the α-erythromycin in the described feed liquid of XDA-1 resin absorption, after in other acetone of analytical pure level, adding the described resin of eluent wash-out that accounts for the preparation of acetone volume 13% distilled water, the pH value of adjusting elutriant 8 and the water content of adjusting elutriant at 17%wt, adjust the pH value to 8.5 of elutriant again, elutriant is heated to 38 ℃ and be incubated 4.5h, separate out and crystallization erythromycin, carrying out secondary with 50 ℃ of distilled water at last cleans, centrifugation obtains erythromycin with the oven dry under 40 ℃ of centrifugation gained solid substance.
Purity and hygienic requirements in view of product, fermentative Production erythromycin feed liquid extraction wastewater is from the extraction process (extractor) of pharmaceutical factory is transported to material liquid tank in the processing technological flow by closed conduct in, the follow-up treatment process of this example is totally-enclosed process, do not bring secondary pollution, health is reliable, simultaneously, erythromycin content is lower than 1ppm in the fermentative Production erythromycin feed liquid waste water after this example is handled, and is better than national wastewater discharge standard.
Embodiment 9A kind of method that purifies and recycle fermentative Production erythromycin feed liquid, it is characterized in that: adopt the α-erythromycin in the described feed liquid of XDA-1 resin absorption, behind the described resin of acetone wash-out, the pH value of adjusting elutriant be 8 and the water content of adjusting elutriant be 18%wt, adjust the pH value to 9.5 of elutriant again, elutriant is heated to 45 ℃ and be incubated 3h, separate out and crystallization erythromycin, cleaning, centrifugation obtain erythromycin with centrifugation gained solid substance in Vacuumdrier oven dry under 50 ℃; To go out wherein a small amount of amino acid with membrane separating through the feed liquid waste water behind described multistage resin absorption α-erythromycin and described centrifugation gained liquid, adopt the fractional distillation method to isolate N-BUTYL ACETATE and eluent at 50 ~ 130 ℃, gained liquid enters water discharging up to standard pond after the membrane separating.
Purity and hygienic requirements in view of product, fermentative Production erythromycin feed liquid extraction wastewater is from the extraction process (extractor) of pharmaceutical factory is transported to material liquid tank in the processing technological flow by closed conduct in, the follow-up treatment process of this example is totally-enclosed process, do not bring secondary pollution, health is reliable, simultaneously, erythromycin content is lower than 1ppm in the fermentative Production erythromycin feed liquid waste water after this example is handled, and is better than national wastewater discharge standard.
Claims (10)
1. method that purifies and recycle fermentative Production erythromycin feed liquid, it is characterized in that: adopt the α-erythromycin in the described feed liquid of multistage resin absorption, behind the described resin of eluent wash-out, the pH value of adjusting elutriant is 7 ~ 10 and adjust the water content≤20%wt of elutriant, adopt precipitation agent or control hydrolysis method to separate out and crystallization erythromycin then, cleaning, centrifugation obtain erythromycin with centrifugation gained solid substance oven drying at low temperature.
2. the method for purification as claimed in claim 1 and recycling fermentative Production erythromycin feed liquid, it is characterized in that: described multistage resin is the macropore nonpolar adsorption resin, described eluent is methyl alcohol, ethanol or acetone.
3. the method for purification as claimed in claim 1 or 2 and recycling fermentative Production erythromycin feed liquid, it is characterized in that: described multistage resin is D-1300, D-4020, XDA-1 or XD-61 macroporous adsorbent resin, and described eluent is for adding the solution that accounts for the preparation of acetone volume 10 ~ 20% distilled water in other acetone of analytical pure level.
4. the method for purification as claimed in claim 1 or 2 and recycling fermentative Production erythromycin feed liquid, it is characterized in that: the water content of described adjustment elutriant is at 15～20%wt; Described control hydrolysis method is for adjusting pH value to 9 ~ 10.5 of elutriant, and elutriant is heated to 40 ~ 50 ℃ and be incubated 2 ~ 4h; The temperature condition of described oven drying at low temperature is not for being higher than 50 ℃.
5. the method for purification as claimed in claim 3 and recycling fermentative Production erythromycin feed liquid, it is characterized in that: the water content of described adjustment elutriant is at 15～20%wt; Described control hydrolysis method is for adjusting pH value to 9 ~ 10.5 of elutriant, and elutriant is heated to 40 ~ 50 ℃ and be incubated 2 ~ 4h; The temperature condition of described oven drying at low temperature is not for being higher than 50 ℃.
6. the method for purification as claimed in claim 4 and recycling fermentative Production erythromycin feed liquid, it is characterized in that: will go out amino acid with membrane separating through feed liquid waste water behind described multistage resin absorption α-erythromycin and described centrifugation gained liquid, the fractional distillation method is isolated N-BUTYL ACETATE and eluent, and gained liquid enters water discharging up to standard pond after the membrane separating.
7. the method for purification as claimed in claim 5 and recycling fermentative Production erythromycin feed liquid, it is characterized in that: will go out amino acid with membrane separating through feed liquid waste water behind described multistage resin absorption α-erythromycin and described centrifugation gained liquid, the fractional distillation method is isolated N-BUTYL ACETATE and eluent, and gained liquid enters water discharging up to standard pond after the membrane separating.
8. the method for purification as claimed in claim 6 and recycling fermentative Production erythromycin feed liquid, it is characterized in that: when described eluent was acetone, the temperature range of described fractional distillation method was 50 ~ 130 ℃.
9. the method for purification as claimed in claim 7 and recycling fermentative Production erythromycin feed liquid, it is characterized in that: when described eluent was acetone, the temperature range of described fractional distillation method was 50 ~ 130 ℃.
10. the method for purification as claimed in claim 1 and recycling fermentative Production erythromycin feed liquid, it is characterized in that: adopt the α-erythromycin in XDA-1 or the described feed liquid of D-4020 resin absorption, after in other acetone of analytical pure level, adding the described resin of eluent wash-out that accounts for the preparation of acetone volume 10 ~ 20% distilled water, the pH value of adjusting elutriant 7 ~ 10 and the water content of adjusting elutriant at 15～20%wt, adjust pH value to 9 ~ 10.5 of elutriant again, elutriant is heated to 40 ~ 50 ℃ and be incubated 2 ~ 4h, separate out and crystallization erythromycin, carrying out secondary with 50 ℃ of distilled water at last cleans, centrifugation obtains erythromycin with the oven dry under Vacuumdrier is not higher than 50 ℃ of centrifugation gained solid substance.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105237600A (en) * | 2015-10-23 | 2016-01-13 | 伊犁川宁生物技术有限公司 | Method for recovering erythromycin from erythromycin-containing wastewater |
| CN112978993A (en) * | 2021-02-25 | 2021-06-18 | 宜昌东阳光生化制药有限公司 | Method for recovering thiocyanate ions from rectification waste liquid of erythromycin thiocyanate crystallization mother liquor and application |
Citations (2)
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| GB1301389A (en) * | 1969-09-15 | 1972-12-29 | ||
| CN101724000A (en) * | 2008-10-29 | 2010-06-09 | 广东东阳光药业有限公司 | Crystallization method of erythrocin |
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2011
- 2011-03-14 CN CN 201110060764 patent/CN102199179B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1301389A (en) * | 1969-09-15 | 1972-12-29 | ||
| CN101724000A (en) * | 2008-10-29 | 2010-06-09 | 广东东阳光药业有限公司 | Crystallization method of erythrocin |
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| 周磊，等: "红霉素生产废水的树脂吸附法处理研究", 《离子交换与吸附》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105237600A (en) * | 2015-10-23 | 2016-01-13 | 伊犁川宁生物技术有限公司 | Method for recovering erythromycin from erythromycin-containing wastewater |
| CN112978993A (en) * | 2021-02-25 | 2021-06-18 | 宜昌东阳光生化制药有限公司 | Method for recovering thiocyanate ions from rectification waste liquid of erythromycin thiocyanate crystallization mother liquor and application |
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