CN1534012A - Method recovering butylacetate in antibiotic production process - Google Patents

Method recovering butylacetate in antibiotic production process Download PDF

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Publication number
CN1534012A
CN1534012A CNA031214088A CN03121408A CN1534012A CN 1534012 A CN1534012 A CN 1534012A CN A031214088 A CNA031214088 A CN A031214088A CN 03121408 A CN03121408 A CN 03121408A CN 1534012 A CN1534012 A CN 1534012A
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China
Prior art keywords
butyl acetate
production
resin
antibiotics
resin column
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CNA031214088A
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CN1227211C (en
Inventor
平志存
刘庆芬
杨志杰
徐更
王佳玉
刘会洲
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Huabei Pharmaceutical Co., Ltd.
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HUABEI PHARMACEUTICAL GROUP CO Ltd
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Priority to CNB031214088A priority Critical patent/CN1227211C/en
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00Technologies relating to chemical industry
    • Y02P20/50Improvements relating to the production of bulk chemicals

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  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
  • Water Treatment By Sorption (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

A process for recovering the butyl acetate generated during production of antibiotics includes resin adsorption of the solution containing the butyl acetate, water washing, analyzing the saturated resin by saturated steam, condensing the analyzed liquid, laying asid, and phase separation. Its advantages are high recovery rate, less energy consumption and low cost.

Description

A kind of method that reclaims the N-BUTYL ACETATE in the production of antibiotics process
Technical field:
The present invention relates to the recovery of organic solvent, specifically a kind of method that reclaims the N-BUTYL ACETATE in the production of antibiotics process.
Background technology:
The microbiotic that many employing microbial fermentations such as penicillin, erythromycin are produced, its production process includes steps such as fermentation, filtration, extraction, back extraction, crystallization.These microbiotic exist with different chemical state (free acid, alkali or salification) under different pH conditions, they water and with the immiscible solvent of water in different solubility, utilize this character that these microbiotic are transferred to the another kind of liquid from a kind of liquid state and go, to reach the purpose that concentrates and purify.So in antibiotic production process, usually utilize N-BUTYL ACETATE to extract or back extraction.Owing in antibiotic fermentation liquid, there are impurity such as many degraded products, pigment, protein, thereby, when extracting penicillin with N-BUTYL ACETATE, a large amount of impurity in the fermented liquid, organism particularly, comprise that the N-BUTYL ACETATE about 1% is present in aqueous phase, its COD value can be up to 25000-30000mg/L.After from these factory effluents, reclaiming N-BUTYL ACETATE earlier, carry out waste water treatment again, not only can reduce the COD value of waste water, reduce the processing pressure of waste water, also the N-BUTYL ACETATE that reclaims can be continued use simultaneously, reduce antibiotic production cost.In addition, in antibiotic back extraction process, also have a certain amount of N-BUTYL ACETATE to be dissolved in aqueous phase, and along with the increase of antibiotic concentration, the mutual solubility of N-BUTYL ACETATE and water obviously increases,, will impact to post-order process if not with its recovery.As in penicillin back extraction process, must there be a certain amount of N-BUTYL ACETATE to be dissolved in aqueous phase, under the normal circumstances, the mutual solubility of water and N-BUTYL ACETATE is little, (being about about 0.6%), but when penicillin existed, mutual solubility obviously increased (can reach 5-15%).The N-BUTYL ACETATE of this part can make the solvent that uses in the penicillin crystallisation process---and be mixed with N-BUTYL ACETATE in the propyl carbinol, thereby make it destroyed for butanols in the solution removal process.Thereby strengthened its production cost.At present, the recovery method of N-BUTYL ACETATE is to adopt distillation method, promptly utilizes the different of N-BUTYL ACETATE and water boiling point, and part vaporization and condensation by repeatedly make N-BUTYL ACETATE and water sepn, thereby reach the purpose of recovery N-BUTYL ACETATE.Its still-process is achieved in that waste water is preheated to about 90 ℃ through preheater earlier in the storage tank, enters distillation tower again and distills, and the control column bottom temperature is not less than 102 ℃ in the still-process.Gasifying liquid enters phase separation tank through condenser, because N-BUTYL ACETATE and water have azeotropic point, contain the water about 28% in the liquid that cat head steams, thereby, after the liquid that steams leaves standstill cooling, make heavy phase (water) and light (N-BUTYL ACETATE) phase-splitting mutually, light phase N-BUTYL ACETATE enters rectifying tower and carries out rectifying, and heavy phase is mixed distillation again with waste water.A large amount of waste water in the tower still enter waste water processing station and handle.
The shortcoming of this method is: steam consumption is big, need carry out twice distillation; The recovery yield of N-BUTYL ACETATE is low, is generally 90-91%; The cost recovery height; Waste water forms many high polymers through pyrogenic distillation, has increased the intractability of waste water; Hot wastewater is to the distillation plant seriously corroded, and service life of equipment is short.
Summary of the invention:
The object of the present invention is to provide a kind of method that reclaims the N-BUTYL ACETATE in the production of antibiotics process, this method can improve the rate of recovery of N-BUTYL ACETATE, reduces cost recovery, and saves energy consumption.
The object of the present invention is achieved like this: reclaim the method for the N-BUTYL ACETATE in the production of antibiotics process, adopt resin to reclaim, it may further comprise the steps:
A. with the aqueous solution that contains N-BUTYL ACETATE in the production of antibiotics process after resin column absorption, washing;
B. the saturated resin after will adsorbing is resolved with saturation steam;
C. desorbed solution is carried out condensation, static, phase-splitting, recovery.
The inventive method is applicable to the recovery of the N-BUTYL ACETATE in all production of antibiotics processes.It is to the concentration and the not concrete qualification of antibiotic concentration of the N-BUTYL ACETATE in the microbiotic production process, that is to say, this method is fit to the N-BUTYL ACETATE of any concentration in the microbiotic production process is recycled, and the concentration of microbiotic self is to its not influence.For example: this method can reclaim the N-BUTYL ACETATE in beta-lactam and the macrolide antibiotics production process, N-BUTYL ACETATE concentration in this production process in the waste water is usually at 0.1%-5%, and beta-lactam and macrolide antibiotics are any concentration; Extract aqueous phase at penicillin G, penicillin v and remove the N-BUTYL ACETATE process, its N-BUTYL ACETATE concentration is usually at 2%-30%, and penicillin G, penicillin v are any concentration; Containing the process that penicillin G, penicillin v system remove N-BUTYL ACETATE, its N-BUTYL ACETATE concentration is usually at 0.1%-99%, and penicillin G, penicillin v are any concentration.
The inventive method is when absorption, and adsorption temp can be controlled in the suitable scope of resin, generally can be at-10 ℃-50 ℃.For helping energy-conservation and environmental protection, can carry out at normal temperatures usually; Flow velocity during absorption can suitably be controlled according to the concentration of handled N-BUTYL ACETATE, and promptly when the concentration of N-BUTYL ACETATE was high, flow velocity can slow down, and when the concentration of N-BUTYL ACETATE was low, flow velocity can be accelerated; When resolving, can adopt direct heating also can adopt indirect heating; Temperature during parsing and vapor pressure can adopt conventional parameter.
Resin of the present invention can be macroporous adsorbent resin (as: BD-1, BD-2, D312), also can be aliphatic hydrocarbon gel-like resin (S-1, S-2), its preferred resin is the crosslinked lipid acid lipid of a diene macroporous adsorbent resin, this resin having better effect in the present invention; The resin Type of equipment can adopt any one equipment such as pot type, pillar, tubular type.
The N-BUTYL ACETATE aqueous solution can be the waste water that contains N-BUTYL ACETATE in the production of antibiotics process in the said production of antibiotics process of the inventive method, also can be strip liquor or the N-BUTYL ACETATE mother liquor that contains N-BUTYL ACETATE in the production of antibiotics process.
The said resin column of the inventive method is preferably the twin columns tandem, its preferred adsorption process is the aqueous solution that contains N-BUTYL ACETATE in the production of antibiotics process, feed among the resin column A, behind the resin absorption N-BUTYL ACETATE, go out from the post underflow, wait to flow out have N-BUTYL ACETATE to reveal in the solution after, B is connected in series with resin column, treat that resin column B effluent liquid has N-BUTYL ACETATE to reveal after, stop charging, after resin column A washed, enter the b step process.
, when reclaiming N-BUTYL ACETATE,,, help environment-protection wastewater and handle with the inventive method so can avoid the protein denaturation in the waste water and form high polymer because of its waste water solution is to carry out adsorption treatment at normal temperatures; Reduced the corrosion of hot wastewater, prolonged service life of equipment equipment; A large amount of steam have been saved simultaneously.
The inventive method can make the rate of recovery of N-BUTYL ACETATE improve more than 4%, and save energy 80% reduces cost recovery 80%, and the first-time qualification rate that reclaims N-BUTYL ACETATE is 100%.
Embodiment:
Further specify the present invention by the following examples.
Embodiment 1:
The inventive method reclaims the application of N-BUTYL ACETATE in waste water produced from penicillin production
With the factory effluent (N-BUTYL ACETATE content is 1%) that produces in the penicillin leaching process, after transferring pH4, with 280 liters of/hour flow velocitys from overhead stream through the resin column of the crosslinked fatty acid ester macroporous copolymer of BD-1 type diene resin (resin processing plant of University Of Tianjin) is housed, when the effluent liquid of resin column bottom has N-BUTYL ACETATE to flow out with the acid base titration detection, stop charging, effusive waste water enters sewage works.Treat to wash saturated resin earlier with water after the waste water emptying in the post, carrying out pyrolysis from resin column bottom feeding saturation steam again analyses, vapor pressure is controlled at below the 0.05Mpa, and when column top temperature reached 90 ℃, the N-BUTYL ACETATE that adsorbs on the resin and the steam of feeding formed azeotrope and begins to overflow from the resin column top, after condenser condenses, enter phase splitter, static phase-splitting gently enters the N-BUTYL ACETATE storage tank mutually, continues after the assay was approved to use, heavy phase enters the waste water storage tank, handles again.The rate of recovery of N-BUTYL ACETATE reaches 95.2%.When column top temperature reaches 100 ℃, get condensed effluent liquid, leave standstill, stop logical steam when not having obvious layering, stand-by behind the resin column naturally cooling.
Embodiment 2:
The inventive method reclaims the application of N-BUTYL ACETATE in waste erythromycin producing water
With the factory effluent (N-BUTYL ACETATE content is 0.5%) that produces in the erythromycin leaching process, after transferring pH4, with 350 liters of/hour flow velocitys from overhead stream through the resin column of S-1 type aliphatic hydrocarbon gel resin (resin processing plant of University Of Tianjin) is housed, when the effluent liquid of resin column bottom has N-BUTYL ACETATE to flow out with the acid base titration detection, stop charging, effusive waste water enters sewage works.Treat to wash saturated resin earlier with water extremely after the waste water emptying in the post, carrying out pyrolysis from resin column bottom feeding saturation steam again analyses, vapor pressure is controlled at below the 0.05Mpa, and when column top temperature reached 90 ℃, the N-BUTYL ACETATE that adsorbs on the resin and the steam of feeding formed common expense thing and begins to overflow from the resin column top, after condenser condenses, enter phase splitter, static phase-splitting gently enters the N-BUTYL ACETATE storage tank mutually, continues after the assay was approved to use, heavy phase enters the waste water storage tank, handles again.The rate of recovery of N-BUTYL ACETATE reaches 96.1%.When column top temperature reaches 100 ℃, get condensed effluent liquid, leave standstill, stop logical steam when not having obvious layering, stand-by behind the resin column naturally cooling.
Embodiment 3:
The inventive method removes the application of N-BUTYL ACETATE in the penicillin strip liquor
Concentration is the penicillin stripping workshop of 0.5g/ml, wherein N-BUTYL ACETATE content is 17%, flow through from the column top with 100 liters/hour flow velocitys the resin column of the crosslinked fatty acid ester macroporous copolymer of BD-2 type resin (resin processing plant of University Of Tianjin) is housed, when the effluent liquid of resin column bottom has N-BUTYL ACETATE to flow out with the acid base titration detection, stop charging, effluent liquid enters penicillin and extracts operation down.With feed liquid emptying in the post, water cleans saturated resin post to the penicillin that sees through and reaches more than 99%, carrying out pyrolysis from resin column bottom feeding saturation steam again analyses, vapor pressure is controlled at below the 0.05Mpa, when column top temperature reaches 93 ℃, the azeotrope that the N-BUTYL ACETATE that adsorbs on the resin and the steam of feeding form begins to overflow from the resin column top, after condenser condenses, enter phase splitter, static phase-splitting, gently enter the N-BUTYL ACETATE storage tank mutually, continue after the assay was approved to use, heavy phase enters the waste water storage tank, handles again.The rate of recovery of N-BUTYL ACETATE reaches 97.2%.When column top temperature reaches 100 ℃, get condensed effluent liquid, leave standstill, stop logical steam when not having obvious layering, stand-by behind the resin column naturally cooling.
Embodiment 4:
The inventive method adopts the twin columns tandem to carry out the application that N-BUTYL ACETATE reclaims.
The factory effluent that produces in the erythromycin leaching process (N-BUTYL ACETATE content is 1.0%), after the adjustment pH value is 3.5, feed among the resin column A (macroporous resin D-312 type) with 280 liters of/hour flows, go out from the post underflow behind the resin absorption N-BUTYL ACETATE, waiting to flow out has N-BUTYL ACETATE to reveal the back (at this moment in the waste acid water, total wastewater flow rate that feeds is approximately about 2240 liters), connect with resin column B (macroporous resin D-312 type), treat that resin column B effluent liquid has N-BUTYL ACETATE to reveal back (wastewater flow rate that feeds resin column B is about 2240 liters) and stops charging, to resin column A washing and dissection process.That is: with the waste acid water emptying in the resin column A, water directly feeds steam after cleaning resin, and pressure-controlling when column top temperature reaches 90 ℃, begins discharging and enters water distributing can below 0.05Mpa, gently advances the finished product jar mutually, and heavy phase is returned the waste acid water storage tank.After column top temperature reaches 100 ℃, get the effluent liquid sample, stop steam after not having obvious layering, the cooling back is stand-by.After this, as second post, post B continues to feed waste acid water as first post, repeats aforesaid operations post A.Press aforesaid operations, the N-BUTYL ACETATE rate of recovery can reach 97.16%, and the N-BUTYL ACETATE first-time qualification rate is 100%, steam consumption 24.26KG/ ton waste acid water, save energy 80%.

Claims (5)

1. a method that reclaims the N-BUTYL ACETATE in the production of antibiotics process is characterized in that its employing resin reclaims, and it may further comprise the steps:
A. with the aqueous solution that contains N-BUTYL ACETATE in the production of antibiotics process after resin column absorption, washing;
B. the saturated resin after will adsorbing is resolved with saturation steam;
C. desorbed solution is carried out condensation, static, phase-splitting, recovery.
2. the method for the N-BUTYL ACETATE in the recovery production of antibiotics process according to claim 1 is characterized in that said resin is the crosslinked lipid acid lipid of a diene macroporous adsorbent resin.
3. the method for the N-BUTYL ACETATE in the recovery production of antibiotics process according to claim 1 is characterized in that the N-BUTYL ACETATE aqueous solution is the waste water that contains N-BUTYL ACETATE in the production of antibiotics process in the said production of antibiotics process.
4, the method for the N-BUTYL ACETATE in the recovery production of antibiotics process according to claim 1 is characterized in that the N-BUTYL ACETATE aqueous solution is strip liquor or the N-BUTYL ACETATE mother liquor that contains vinegar tincture butyl ester in the production of antibiotics process in the said production of antibiotics process.
5, the method for the N-BUTYL ACETATE in the recovery production of antibiotics process according to claim 1, it is characterized in that said resin column is the twin columns tandem, its adsorption process is the aqueous solution that contains acetate butyl in the production of antibiotics, feeds among the resin column A, behind the absorption N-BUTYL ACETATE, go out from the post underflow, wait to flow out have acetate butyrate to reveal in the solution after, B is connected in series with resin column, after treating that resin column B effluent liquid has N-BUTYL ACETATE to reveal, stop charging, after resin column A is washed, enter the b step process.
CNB031214088A 2003-03-28 2003-03-28 Method recovering butylacetate in antibiotic production process Expired - Fee Related CN1227211C (en)

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CN1227211C CN1227211C (en) 2005-11-16

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1304358C (en) * 2005-04-22 2007-03-14 清华大学 Method for preparing high pure methyl acetate through adsorption of liquid phase
CN101575288B (en) * 2009-06-18 2012-04-04 孙宗长 Method for recovering ethyl acetate from wastewater containing ethyl acetate
CN113230830A (en) * 2021-04-14 2021-08-10 内蒙古常盛制药有限公司 Treatment method of industrial waste gas containing butyl acetate
CN114380352A (en) * 2022-01-26 2022-04-22 山东微研生物科技有限公司 Recovery device and recovery method for ethyl acetate in beta-carotene extraction wastewater

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1304358C (en) * 2005-04-22 2007-03-14 清华大学 Method for preparing high pure methyl acetate through adsorption of liquid phase
CN101575288B (en) * 2009-06-18 2012-04-04 孙宗长 Method for recovering ethyl acetate from wastewater containing ethyl acetate
CN113230830A (en) * 2021-04-14 2021-08-10 内蒙古常盛制药有限公司 Treatment method of industrial waste gas containing butyl acetate
CN114380352A (en) * 2022-01-26 2022-04-22 山东微研生物科技有限公司 Recovery device and recovery method for ethyl acetate in beta-carotene extraction wastewater
CN114380352B (en) * 2022-01-26 2023-10-13 山东微研生物科技有限公司 Recovery device and recovery method for ethyl acetate in beta-carotene extraction wastewater

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