CN102363588A - Decolouring method applied in antibiotic solvent extraction technology - Google Patents
Decolouring method applied in antibiotic solvent extraction technology Download PDFInfo
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- CN102363588A CN102363588A CN2011101422492A CN201110142249A CN102363588A CN 102363588 A CN102363588 A CN 102363588A CN 2011101422492 A CN2011101422492 A CN 2011101422492A CN 201110142249 A CN201110142249 A CN 201110142249A CN 102363588 A CN102363588 A CN 102363588A
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Abstract
The invention relates to a decolouring method applied in an antibiotic solvent extraction technology. The decolouring method provided by the invention comprises the following main steps of: transferring a solid phase obtained by filtering a broth into an extraction pot, adding an extractant according to a certain proportion, stirring and extracting for one hour; Adding a decolorant which accounts for 0.1-1% the volume of an extract, followed by stirring, extraction and decolouring for 0.5-1.5 hours, standing for 0.5-1 hour, transferring the upper layer of the extract into an extract storage tank; separating the extract by a separation device, and allowing a qualified extract to enter into the next process. According to the invention, the decolouring process is transferred from a post-treatment to a preliminary treatment during the purification process, and the extraction is carried out when decolouring, thus minimizing the equipment investment and simplifying the purification technological steps. Much of the decolorant is adhered to the solid phase substance during the decolouring process, which is beneficial to process the waste solid phase substance and minimize the ''three wastes'' treatment cost. In addition, the decolouring method provided by the invention can be used to minimize the purification time, raise work efficiency, create a good decolouring effect and save the production cost.
Description
Technical field
The present invention is a kind of decoloring method, particularly a kind of decoloration process that is applicable in the microbiotic solid-liquid solvent extraction extraction liquid.
Background technology
Solvent extraction is a kind of domestic method in the microbiotic purifying technique, is widely used.The extraction liquid that solvent extraction the produces processing of generally will decolouring.Microbiotic decoloration process route commonly used has two kinds: a kind of for extracting, separate, concentrate, change salt, decolouring, filtration, crystallization; Another kind of for extraction, separate, decolouring, filter, concentrate, change salt, crystallization (referring to " microbiotic technic ", the Wu Hangyan chief editor. Chemical Industry Press).This technology must add discoloring agent in the special decolouring jar decolours, and utilizes filter that discoloring agent is separated with extraction liquid again.This process method investment is big, and technical process is complicated, and the PT is long, and product loss is also big.
Summary of the invention
The technical problem that the present invention will solve provides a kind of decoloring method that is applied to extracting with antibiotic dissolved medium technology, and this method need not to increase special decolouring and straining installation, and loss of material is little.
For solving the problems of the technologies described above, the technical scheme that the present invention adopts is:
Adopt decolouring in the extraction, separate, concentrate, change salt, crystallization processes route; Key is to adopt the method for the decolouring while extracting; Promptly in the liquid-solid extraction process, add discoloring agent; Most of discoloring agent adheres to solid phase in extraction process, a small amount of discoloring agent gets in the extraction liquid, and is promptly separable with general separating machine.Specifically may further comprise the steps:
(1) earlier fermented liquid is divided into solid-liquid two phases through separating device, transfers to gained solid phase (being filter cake) in the extractor, by the extraction agent volume: solid phase weight is that the ratio of 1～2 L:1 ㎏ adds extraction liquid, opens stirring and extracts.
(2) SPE after 1 hour; Weight in the discoloring agent of 0.1%～1% the required adding of ratio weighing of extraction liquid volume; Directly add the interior continuation of extractor to the discoloring agent that weighs up and stir extraction decolouring 0.5～1.5 hour; Leave standstill and make the solid phase natural subsidence, extraction liquid is transferred in the extraction liquid basin; Add extraction liquid again and extract, the object percentage extraction can stop the extraction next time when above greater than define objective in solid phase.
Add discoloring agent in proportion when (3) extracting for the first time, need not add discoloring agent when postorder extracts again; The discoloring agent major part all adheres on the solid phase, only contains seldom discoloring agent in the extraction liquid.
(4) extraction liquid in the extractor is sent in the separating machine separated, obtain qualified parting liquid, get into down operation and concentrate and makes with extra care.
Above-mentioned discoloring agent can be any one or two kinds in gac, the acidic white earth.
The granularity of above-mentioned discoloring agent is 60～150 orders.
The extraction liquid separating device can be any one in disk plate centrifuge, tubular-bowl centrifuge, the accurate filter.
Said extraction liquid is at least a in butylacetate, ETHYLE ACETATE, butanols, isobutyl acetate, amylalcohol, chloroform, the methylene dichloride.
The present invention has actively useful effect:
The present invention has overcome traditional technological prejudice, is become decolorization by the post-processed in the purification process and handles early stage, and the decolouring while extracting reduces facility investment, simplifies the purifying technique step; Discoloring agent major part in decolorization all sticks on the solid formation, helps the processing of useless solid formation and reduces three wastes processing costs; The present invention simultaneously can reduce the purification time, increases work efficiency, and decolorizing effect is good, saves production cost.
Embodiment
Further set forth the present invention below in conjunction with specific embodiment.Used raw material and equipment among the following embodiment if no special instructions, is commercially available.
Embodiment 1: the extraction liquid decoloring method of Maduramicin mainly may further comprise the steps:
(1) the Maduramicin fermented liquid obtains 2400 ㎏ filter cakes through Plate Filtration, transfers to filter cake in the extractor, in jar, adds 3000 liters ethyl acetate extraction agent, opens to stir to extract.
(2) extraction is after 1 hour, and it is 40% that the extraction liquid transparence is surveyed in sampling, in extractor, adds 5 ㎏ gacs and begins to stir decolouring, and restir 1 hour left standstill 0.5 hour, in vacuum transfer extraction liquid to extraction liquid basin.
(3) in extractor, add 2800 liters of ETHYLE ACETATE again and carry out reextraction, when the Maduramicin percentage extraction is above greater than 90%, stop to carry out extraction next time, only when extracting for the first time, add gac in the whole extraction process, just can satisfy the decolouring requirement.
(4) utilize gac to decolouring with extraction rear decoloring effect in the extraction of Maduramicin filter cake and using magnitude relation:
Technological test of the present invention and controlled trial (ordinary method) are compared test.Get 2 ㎏ Maduramicin filter cakes, be divided into 2 parts in the container that band stirs.
Technological test of the present invention: add ETHYLE ACETATE and carry out single extraction for 1.5 liters, stirring, sampling survey extraction liquid transparence is 38% after 1 hour, adds gac 5g, restir 1 hour, leaving standstill 0.5 hour sampling survey single extraction liquid transparence is 85%; Be transferred to container to extraction liquid, then add 1.2 liters in ETHYLE ACETATE and carry out the extraction second time, it is 90% that the extraction fluid transparence is surveyed in sampling; Recording hybrid extraction liquid transparence behind single extraction liquid and the extraction fluid hybrid filtering is 88%;
Controlled trial: add ETHYLE ACETATE and carry out single extraction for 1.5 liters; Stirred 2 hours, leaving standstill 0.5 hour sampling survey extraction liquid transparence is 36%, migrates out single extraction liquid; Then add ETHYLE ACETATE and carry out reextraction for 1.2 liters, it is 45% that sampling survey extraction fluid is passed through degree; Being transferred in the container of a band stirring after single extraction liquid and the extraction fluid mixing, add gac 5g, stirring 0.5 hour filtering and sampling survey hybrid extraction liquid transparence is 83%.
From above-mentioned simultaneous test, although can both satisfy production requirement, the complex process of controlled trial, used device is more, and man-hour is longer, takes time and effort, and production cost is very high.
(5) extraction liquid gets in the disc separator through blast and separates, and obtains qualified parting liquid, and it is 91% that the parting liquid transparence is surveyed in sampling, and parting liquid concentrates, changes salt, crystallization etc.;
Embodiment 2: the extraction liquid decoloring method of Maduramicin mainly may further comprise the steps:
(1) the Maduramicin fermented liquid obtains 2000 ㎏ filter cakes through Plate Filtration, transfers to filter cake in the extractor, in jar, adds 2500 liters ethyl acetate extraction agent, opens to stir to extract.
(2) extraction is 1 hour, and sampling detects extraction liquid transparence 38%, in extractor, adds 15 ㎏ acidic white earths, stirs decolouring 1 hour, leaves standstill 0.5 hour, in vacuum transfer extraction liquid to extraction liquid basin.
(3) in extractor, add 2000 liters of ETHYLE ACETATE and carry out two collections,, no longer carry out extraction next time when maduramicin ammonium percentage extraction 92% (required standard) greater than 90%.
(4) utilize acidic white earth to decolouring with extraction rear decoloring effect in the extraction of Maduramicin filter cake and using magnitude relation
Technological test of the present invention and controlled trial (ordinary method) are compared test.Get 2 ㎏ Maduramicin filter cakes, be divided into 2 parts in the container that band stirs.
Technological test of the present invention: adding ETHYLE ACETATE carries out single extraction for 1.5 liters, and stirring the survey extraction liquid transparence of taking a sample after 1 hour is 35%, adds acidic white earth 10g, restir 1 hour, and leaving standstill 0.5 hour sampling survey single extraction liquid transparence is 83%; Be transferred to container to extraction liquid, then add 1.2 liters in ETHYLE ACETATE and carry out the extraction second time, it is 88% that the extraction fluid transparence is surveyed in sampling; Recording hybrid extraction liquid transparence behind single extraction liquid and the extraction fluid hybrid filtering is 85%;
Controlled trial: add ETHYLE ACETATE and carry out single extraction for 1.5 liters; Stirred 2 hours, leaving standstill 0.5 hour sampling survey extraction liquid transparence is 34%, migrates out single extraction liquid; Then add ETHYLE ACETATE and carry out reextraction for 1.2 liters, it is 42% that sampling survey extraction fluid is passed through degree; Being transferred in the container of a band stirring after single extraction liquid and the extraction fluid mixing, add acidic white earth 10g, stirring 0.5 hour filtering and sampling survey hybrid extraction liquid transparence is 82%.
From two tests, can both satisfy production requirement, but the controlled trial complex process, used device is more, and man-hour is longer, and technological test technology of the present invention is better than technology aborning.
(5) extraction liquid gets into the accurate filter filtration through blast, obtains qualified parting liquid, and detecting the parting liquid transparence is 89%, and entering operation is down handled.
Though, the present invention has been done detailed description in the preceding text with general explanation and specific embodiments, on basis of the present invention, can to some modifications of do or improvement, this will be apparent to those skilled in the art.Therefore, these modifications or the improvement on the basis of not departing from spirit of the present invention, made all belong to the scope that requirement of the present invention is protected.
Claims (8)
1. decoloring method that is applied to extracting with antibiotic dissolved medium technology may further comprise the steps:
(1) extraction: will cross by the antibiotic fermentation liquid of ordinary method preparation earlier and filter solid phase, and be transferred to solid phase in the extractor, and add extraction agent by a certain percentage, beginning is stirred extraction with 60～150 rev/mins rotating speed;
(2) add discoloring agent: stir extraction after 1～2 hour, press 0.1%～1% of extraction liquid volume and add discoloring agent, stir extraction decolouring 0.5～1.5 hour, left standstill 0.5～1 hour, upper layer of extraction liquid is transferred in the extraction liquid basin;
(3) extraction liquid separates: separate extraction liquid through tripping device, obtain qualified extraction liquid and get into next procedure.
2. the decoloring method that is applied to extracting with antibiotic dissolved medium technology according to claim 1 is characterized in that, in said step (1), in the extraction agent volume: solid phase weight is after the ratio of 1～2L:1 ㎏ adds extraction liquid, to stir extraction.
3. the decoloring method that is applied to extracting with antibiotic dissolved medium technology according to claim 1 is characterized in that, said discoloring agent is at least a in gac, the acidic white earth.
4. the decoloring method that is applied to extracting with antibiotic dissolved medium technology according to claim 1 is characterized in that, the granularity of said discoloring agent is 60～150 orders.
5. the decoloring method that is applied to extracting with antibiotic dissolved medium technology according to claim 1 is characterized in that, in the said step (2), carries out 1～3 extraction as required, only when extracting for the first time, adds discoloring agent in proportion.
6. the decoloring method that is applied to extracting with antibiotic dissolved medium technology according to claim 1; It is characterized in that; In said step (3); Be pressed into extraction liquid in the extractor in the tripping device through blast or mechanical transport and separate, obtain qualified parting liquid, get into down operation and produce standard compliant finished product.
7. the decoloring method that is applied to extracting with antibiotic dissolved medium technology according to claim 1 is characterized in that, said tripping device is any one in disk plate centrifuge, tubular-bowl centrifuge, the accurate filter.
8. the decoloring method that is applied to extracting with antibiotic dissolved medium technology according to claim 1 is characterized in that, said extraction liquid is at least a in butylacetate, ETHYLE ACETATE, butanols, isobutyl acetate, amylalcohol, chloroform, the methylene dichloride.
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| CN201110142249.2A CN102363588B (en) | 2011-05-30 | 2011-05-30 | Decolouring method applied in antibiotic solvent extraction technology |
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| CN201110142249.2A CN102363588B (en) | 2011-05-30 | 2011-05-30 | Decolouring method applied in antibiotic solvent extraction technology |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1034758A (en) * | 1987-10-29 | 1989-08-16 | 福州市抗菌素厂 | Emulsion-breaking process by extracting with antibiotic dissolved medium |
| CN1232034A (en) * | 1999-04-02 | 1999-10-20 | 清华大学 | Process for direct preparing penicillin sodium salt from fermentation liquid |
| CN101643758A (en) * | 2008-08-06 | 2010-02-10 | 山东金洋药业有限公司 | Method for extracting monensin sodium by methanol extraction method |
-
2011
- 2011-05-30 CN CN201110142249.2A patent/CN102363588B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1034758A (en) * | 1987-10-29 | 1989-08-16 | 福州市抗菌素厂 | Emulsion-breaking process by extracting with antibiotic dissolved medium |
| CN1232034A (en) * | 1999-04-02 | 1999-10-20 | 清华大学 | Process for direct preparing penicillin sodium salt from fermentation liquid |
| CN101643758A (en) * | 2008-08-06 | 2010-02-10 | 山东金洋药业有限公司 | Method for extracting monensin sodium by methanol extraction method |
Non-Patent Citations (2)
| Title |
|---|
| 《中国抗生素杂志》 20000228 李十中等 抗生素提取过程中溶剂萃取技术新方法__超滤/萃取法 第12-15页 1-8 第25卷, 第1期 * |
| 李十中等: "抗生素提取过程中溶剂萃取技术新方法――超滤/萃取法", 《中国抗生素杂志》, vol. 25, no. 1, 28 February 2000 (2000-02-28), pages 12 - 15 * |
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Application publication date: 20120229 Assignee: Ju Xin bio tech ltd, Dancheng Assignor: Puyang Hotway Pharmaceuticals Co., Ltd. Contract record no.: 2015410000028 Denomination of invention: Decolouring method applied in antibiotic solvent extraction technology Granted publication date: 20141231 License type: Exclusive License Record date: 20150423 |
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