CN102363588B - Decolouring method applied in antibiotic solvent extraction technology - Google Patents
Decolouring method applied in antibiotic solvent extraction technology Download PDFInfo
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- CN102363588B CN102363588B CN201110142249.2A CN201110142249A CN102363588B CN 102363588 B CN102363588 B CN 102363588B CN 201110142249 A CN201110142249 A CN 201110142249A CN 102363588 B CN102363588 B CN 102363588B
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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 be applicable to extraction liquid in microbiotic solid-liquid solvent extraction.
Background technology
Solvent extraction is a kind of common method in microbiotic purifying technique, is widely used.The extraction liquid that solvent extraction produces generally will carry out desolventing technology.Conventional microbiotic decoloration process route has two kinds: a kind of for extracting, being separated, concentrate, turn salt, decolouring, filtration, crystallization, another kind of for extract, be separated, decolour, filter, concentrate, turn salt, crystallization (see " microbiotic technology ", Wu Hangyan chief editor. Chemical Industry Press).This technique must add discoloring agent and decolour in special decolouring tank, and discoloring agent is separated with extraction liquid by recycling filter.The investment of this processing method is large, and technical process is complicated, and the production time is long, and product loss is also large.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of decoloring method being applied to extracting with antibiotic dissolved medium technique, and this method is without the need to increasing special decolouring and filter plant, and loss of material is little.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
Decolour in employing extraction, be separated, concentrate, turn salt, crystallization processes route, key is the method adopting the decolouring of extraction limit, limit, namely in liquid-solid extraction process, discoloring agent is added, major part discoloring agent adheres to solid phase in extraction process, a small amount of discoloring agent enters in extraction liquid, with general separating machine and separable.Specifically comprise the following steps:
(1) first fermented liquid is divided into solid-liquid two-phase by separating device, then gained solid phase (i.e. filter cake) is transferred in extractor, in extraction agent volume: solid phase weight is that the ratio of 1 ~ 2 L:1 ㎏ adds extraction liquid, open stirring and extract.
(2) Solid-Phase Extraction after 1 hour, in extraction liquid volume 0.1% ~ 1% ratio weigh needed for the weight of discoloring agent that adds, the discoloring agent weighed up directly is added in extractor and continues to stir extraction decolouring 0.5 ~ 1.5 hour, leave standstill and make solid phase natural subsidence, extraction liquid is transferred in extraction liquid basin; Add extraction liquid again to extract, until stopping extraction next time when object percentage extraction is greater than more than define objective in solid phase.
(3) add discoloring agent in proportion during first time extraction, do not need when postorder extracts to add discoloring agent again; Discoloring agent major part all adheres in solid phase, only containing little discoloring agent in extraction liquid.
(4) be separated in extractor in extraction liquid feeding separating machine, obtain qualified parting liquid, enter lower operation and carry out concentrated refining.
Above-mentioned discoloring agent can be any one or two kinds in gac, acidic white earth.
The granularity of above-mentioned discoloring agent is 60 ~ 150 orders.
Extraction liquid separating device can be any one in disk plate centrifuge, tubular-bowl centrifuge, accurate filter.
Described extraction liquid is at least one in butylacetate, ethyl acetate, butanols, isobutyl acetate, amylalcohol, chloroform, methylene dichloride.
The present invention has actively useful effect:
Instant invention overcomes traditional technology prejudice, decolorization is become process in early stage from the post-processed in purification process, decolours in extraction limit, limit, reduces facility investment, simplifies purifying technique step; Discoloring agent major part in decolorization all sticks on solid formation, is conducive to the process of useless solid formation and reduces three-protection design expense; The present invention simultaneously can reduce the purification time, increases work efficiency, and decolorizing effect is good, saves production cost.
Embodiment
The present invention is set forth further below in conjunction with specific embodiment.Raw material used in following embodiment and equipment, if no special instructions, be commercially available.
Embodiment 1: the extraction liquid decoloring method of Maduramicin, mainly comprises the following steps:
(1) Maduramicin fermented liquid obtains 2400 ㎏ filter cakes by Plate Filtration, and filter cake is transferred in extractor, adds the acetate extractant of 3000 liters in tank, opens stirring and extracts.
(2) after extracting 1 hour, it is 40% that extraction liquid transparence is surveyed in sampling, adds 5 ㎏ gacs and starts to stir decolouring, then stir 1 hour, leave standstill 0.5 hour, with vacuum transfer extraction liquid in extraction liquid basin in extractor.
(3) in extractor, add 2800 liters of ethyl acetate again and carry out reextraction, stop when Maduramicin percentage extraction is greater than more than 90% carrying out extraction next time, only add gac when first time extraction in whole extraction process, just can meet decolouring requirement.
(4) decolour in utilizing gac to extract Maduramicin filter cake with extraction rear decoloring effect and use magnitude relation:
Present invention process test is carried out simultaneous test with controlled trial (ordinary method).Get 2 ㎏ Maduramicin filter cakes, be divided into 2 parts in the container of band stirring.
Present invention process is tested: add ethyl acetate 1.5 liters and carry out single extraction, stirs, and after 1 hour, extraction liquid transparence is surveyed in sampling is 38%, adds gac 5g, then stirs 1 hour, and it is 85% that single extraction liquid transparence is surveyed in sampling in standing 0.5 hour; Extraction liquid is transferred to container, and then add ethyl acetate 1.2 liters and carry out second time extraction, it is 90% that extraction fluid transparence is surveyed in sampling; Recording hybrid extraction liquid transparence after single extraction liquid and extraction fluid hybrid filtering is 88%;
Controlled trial: add ethyl acetate 1.5 liters and carry out single extraction, stir 2 hours, leaving standstill 0.5 hour sampling survey extraction liquid transparence is 36%, migrates out single extraction liquid, then add ethyl acetate 1.2 liters and carry out reextraction, it is 45% that sampling survey extraction fluid is spent thoroughly; Be transferred in the container of a band stirring after single extraction liquid and 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 meet 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 is entered in disc separator by blast and is separated, and obtains qualified parting liquid, and it is 91% that parting liquid transparence is surveyed in sampling, and parting liquid carries out concentrating, turning salt, crystallization etc.;
Embodiment 2: the extraction liquid decoloring method of Maduramicin, mainly comprises the following steps:
(1) Maduramicin fermented liquid obtains 2000 ㎏ filter cakes by Plate Filtration, and filter cake is transferred in extractor, adds the acetate extractant of 2500 liters in tank, opens stirring and extracts.
(2) extract 1 hour, sampling detects extraction liquid transparence 38%, adds 15 ㎏ acidic white earths in extractor, stirs decolouring 1 hour, leaves standstill 0.5 hour, with vacuum transfer extraction liquid in extraction liquid basin.
(3) in extractor, add 2000 liters of ethyl acetate and carry out two extractions, when the required standard that maduramicin ammonium percentage extraction 92%(is greater than 90%), no longer carry out extraction next time.
(4) utilize acidic white earth to decolouring in the extraction of Maduramicin filter cake and extraction rear decoloring effect and use magnitude relation
Present invention process test is carried out simultaneous test with controlled trial (ordinary method).Get 2 ㎏ Maduramicin filter cakes, be divided into 2 parts in the container of band stirring.
Present invention process is tested: add ethyl acetate 1.5 liters and carry out single extraction, and stirring sampling survey extraction liquid transparence after 1 hour is 35%, and add acidic white earth 10g, then stir 1 hour, it is 83% that single extraction liquid transparence is surveyed in sampling in standing 0.5 hour; Extraction liquid is transferred to container, and then add ethyl acetate 1.2 liters and carry out second time extraction, it is 88% that extraction fluid transparence is surveyed in sampling; Recording hybrid extraction liquid transparence after single extraction liquid and extraction fluid hybrid filtering is 85%;
Controlled trial: add ethyl acetate 1.5 liters and carry out single extraction, stir 2 hours, leaving standstill 0.5 hour sampling survey extraction liquid transparence is 34%, migrates out single extraction liquid, then add ethyl acetate 1.2 liters and carry out reextraction, it is 42% that sampling survey extraction fluid is spent thoroughly; Be transferred in the container of a band stirring after single extraction liquid and 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 production requirement be met, but controlled trial complex process, and used device is more, and man-hour is longer, and present invention process test technology is better than technique aborning.
(5) extraction liquid enters accurate filter filtration by blast, obtains qualified parting liquid, and detecting parting liquid transparence is 89%, enters lower operation process.
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (4)
1. be applied to a decoloring method for extracting with antibiotic dissolved medium technique, comprise the following steps:
(1) extract: first the antibiotic fermentation liquid prepared according to a conventional method is filtered to obtain solid phase, again solid phase is transferred in extractor, in extraction agent volume: solid phase weight is that the ratio of 1 ~ 2L:1 ㎏ adds extraction agent, start to stir extraction with the rotating speed of 60 ~ 150 revs/min;
(2) add discoloring agent: stir extraction after 1 ~ 2 hour, add discoloring agent by 0.1% ~ 1% of extraction liquid volume, stir extraction decolouring 0.5 ~ 1.5 hour, leave standstill 0.5 ~ 1 hour, upper layer of extraction liquid is transferred in extraction liquid basin; Described discoloring agent is at least one in gac, acidic white earth, and its granularity is 60 ~ 150 orders;
(3) extraction liquid is separated: by blast or mechanical transport, extraction liquid press-in tripping device is separated, obtains qualified extraction liquid and enter next procedure.
2. the decoloring method being applied to extracting with antibiotic dissolved medium technique according to claim 1, is characterized in that, in described step (2), carries out 1 ~ 3 extraction as required, only adds discoloring agent in proportion when first time extraction.
3. the decoloring method being applied to extracting with antibiotic dissolved medium technique according to claim 1, is characterized in that, described tripping device is any one in disk plate centrifuge, tubular-bowl centrifuge, accurate filter.
4. the decoloring method being applied to extracting with antibiotic dissolved medium technique according to claim 1, is characterized in that, described extraction liquid is at least one in butylacetate, ethyl acetate, butanols, isobutyl acetate, amylalcohol, chloroform, methylene dichloride.
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| Application Number | Priority Date | Filing Date | Title |
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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 (1)
| Title |
|---|
| 抗生素提取过程中溶剂萃取技术新方法――超滤/萃取法;李十中等;《中国抗生素杂志》;20000228;第25卷(第1期);第12-15页 * |
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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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