CN107936041B - Deacetyl-7-aminocephalosporanicacid acid mother liquor reclaiming method - Google Patents
Deacetyl-7-aminocephalosporanicacid acid mother liquor reclaiming method Download PDFInfo
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- CN107936041B CN107936041B CN201711245340.0A CN201711245340A CN107936041B CN 107936041 B CN107936041 B CN 107936041B CN 201711245340 A CN201711245340 A CN 201711245340A CN 107936041 B CN107936041 B CN 107936041B
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- mother liquor
- aminocephalosporanicacid
- deacetyl
- acid
- concentrated
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D501/00—Heterocyclic compounds containing 5-thia-1-azabicyclo [4.2.0] octane ring systems, i.e. compounds containing a ring system of the formula:, e.g. cephalosporins; Such ring systems being further condensed, e.g. 2,3-condensed with an oxygen-, nitrogen- or sulfur-containing hetero ring
- C07D501/14—Compounds having a nitrogen atom directly attached in position 7
- C07D501/16—Compounds having a nitrogen atom directly attached in position 7 with a double bond between positions 2 and 3
- C07D501/18—7-Aminocephalosporanic or substituted 7-aminocephalosporanic acids
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D501/00—Heterocyclic compounds containing 5-thia-1-azabicyclo [4.2.0] octane ring systems, i.e. compounds containing a ring system of the formula:, e.g. cephalosporins; Such ring systems being further condensed, e.g. 2,3-condensed with an oxygen-, nitrogen- or sulfur-containing hetero ring
- C07D501/02—Preparation
- C07D501/12—Separation; Purification
Abstract
The invention discloses a kind of deacetyl-7-aminocephalosporanicacid acid mother liquor reclaiming methods, comprising the following steps: step 1), mother liquor are concentrated to get a concentrate by film；Then step 2, a concentrate pass through parsing agent by resin adsorption and parse desorbed solution；Step 3), desorbed solution are concentrated to get secondary concentration liquid by film；The deacetyl-7-aminocephalosporanicacid acid that step 4), secondary concentration liquid are recycled by crystallization.The beneficial effects of the present invention are: mother liquor is concentrated using film concentration technology by the present invention, improve the content of product, then it is adsorbed and is parsed using resin, achieve the purpose that purification, it is crystallized again, obtains satisfactory product, product recovery rate reaches 70% or so, with very high product income, promotional value is preferable.This technique is easy to operate at low cost, has started novel recovery process at home, compared to the advantage with essence of the same trade, therefore has very good development prospect.
Description
Technical field
The present invention relates to a kind of deacetyl-7-aminocephalosporanicacid acid mother liquor reclaiming methods, belong to resource reclaim and utilize
Technical field.
Background technique
New intermediate of the deacetyl-7-aminocephalosporanicacid acid (D7ACA) as cephalosporins, with 7-
ACA (7-amino-cephalosporanic acid) is compared, and eliminates the acetyl group on 3, in composite part cephalo kind, simplifies production work
The advantages such as skill route, and have modification simple, is easy purifying, good product quality, and production cost is low；D7ACA is in cephalosporins
Application in the products such as antibiotic product cefuroxime, Cefoxitin, Cefpodoxime ester has high income, quality feature.
Currently, obtaining D7ACA with Cephalosporin C fermentation extracting solution raw material by enzymatic lysis, then being crystallized and consolidated
Body D7ACA generates mass crystallization mother liquor in crystallization, and many D7ACA are still contained in the mother liquor after crystallization, and many enterprises will not
The portioned product is recycled, and not only has lost product in this way, reduces the economic benefit of enterprise, while increasing the place of sewage
Manage difficulty.
Summary of the invention
In order to overcome drawbacks described above, the present invention provides a kind of deacetyl-7-aminocephalosporanicacid acid mother liquor reclaiming methods.
To achieve the goals above, the technical scheme is that a kind of deacetyl-7-aminocephalosporanicacid acid mother liquor returns
Receiving method, comprising the following steps:
Step 1), mother liquor are concentrated to get a concentrate by film；
Then step 2), a concentrate pass through parsing agent by resin adsorption and parse desorbed solution；
Step 3), desorbed solution are concentrated to get secondary concentration liquid by film；
The deacetyl-7-aminocephalosporanicacid acid that step 4), secondary concentration liquid are recycled by crystallization.
Preferably, the parsing agent is that organic solvent is added in sodium bicarbonate solution.
Preferably, the mass fraction of the sodium bicarbonate solution is 4%,
Preferably, the organic solvent is the one or more of methanol, acetone or isopropanol.
Preferably, mass fraction of the organic solvent in parsing agent is 4-5%,
Preferably, the organic solvent is acetone, and the mass fraction in parsing agent is 4%.
The present invention is concentrated mother liquor using film device, solves because mother liquor potency is low, the difficult problem of subsequent purification；
And film concentration ability is big, product yield is high；It is purified later using resin, the removal rate of impurity is high, so that product matter
It measures guaranteed.It is concentrated again with film after parsing simultaneously, after concentration, improves crystalline product yield；In addition parsing of the invention
The problem of hangover is serious when agent proportion solves conventional formulation parsing, and rewinding is not concentrated, and is not able to satisfy production requirement.
The beneficial effects of the present invention are: mother liquor is concentrated using film concentration technology by the present invention, the content of product is improved,
Then it is adsorbed and is parsed using resin, achieve the purpose that purification, remove a large amount of pigments and impurity in mother liquor, then tied
Crystalline substance obtains satisfactory product, and product recovery rate reaches 70% or so, has very high product income, and promotional value is preferable.
This technique is easy to operate at low cost, and reduces the difficulty of sewage treatment, has started novel recovery process at home, compared to the same industry
Advantage with essence, therefore there is very good development prospect.
Detailed description of the invention
Fig. 1 is the process flow chart of the embodiment of the present invention.
Specific embodiment
Technical solution of the present invention is clearly and completely described below in conjunction with attached drawing, it is clear that described implementation
Example is a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill
Personnel's every other embodiment obtained without making creative work, shall fall within the protection scope of the present invention.
Embodiment 1
As shown in Figure 1, a kind of deacetyl-7-aminocephalosporanicacid acid (D7ACA) mother liquor reclaiming method, including following step
It is rapid:
Step 1), D7ACA mother liquor are concentrated to get a concentrate by TJ-10G-8040 film；
Then step 2), a concentrate pass through parsing agent by LX-4207 resin adsorption and parse desorbed solution, parse agent
For 4% sodium bicarbonate solution, wherein being added with 4% acetone, the parsing agent is it is possible to prevente effectively from parsing hangover；
Step 3), desorbed solution are concentrated to get secondary concentration liquid by film；
The deacetyl-7-aminocephalosporanicacid acid that step 4), secondary concentration liquid are recycled by crystallization.
D7ACA mother liquor is after the step 1) of the application-step 3) processing, as shown in table 1, product in secondary concentration liquid
D7ACA purity reaches 78.8% or so, and after step 4) crystallization, D7ACA yield can reach 70% or more, not only improves product and receives
Benefit reduces enterprise's production cost, reduces enterprise's sewage treatment difficulty, promotes enterprise competitiveness.
Table 1:
As shown in table 2, the D7ACA final product quality parameter comparison of the D7ACA finished product and disposing mother liquor normally produced, mother liquor return
The finished product purity of receipts, impurity, product light transmission are normal, and content, purity, DO7ACA (removing acetyl oxygen -7-amino-cephalosporanic acid) are miscellaneous
Matter content is superior to the product normally produced.
Table 2:
Embodiment 2
Other steps of the present embodiment and technical effect are same as Example 1, the sodium bicarbonate solution that parsing agent is 4%,
In be added with 4% isopropanol, the parsing agent it is possible to prevente effectively from parsing hangover,
Embodiment 3
Other steps of the present embodiment and technical effect are same as Example 1, the sodium bicarbonate solution that parsing agent is 4%,
In be added with 5% acetone, the parsing agent it is possible to prevente effectively from parsing hangover.
The limitation that technical solution of the present invention is not limited to the above specific embodiments, it is all to do according to the technique and scheme of the present invention
Technology deformation out, falls within the scope of protection of the present invention.
Claims (6)
1. a kind of deacetyl-7-aminocephalosporanicacid acid mother liquor reclaiming method, it is characterised in that: the following steps are included:
Step 1), mother liquor are concentrated to get a concentrate by film, the mother liquor be with Cephalosporin C fermentation extracting solution raw material,
D7ACA is obtained by enzymatic lysis, is then crystallized to obtain the crystalline mother solution after solid D7ACA；
Then step 2, a concentrate pass through parsing agent by resin adsorption and parse desorbed solution；
Step 3), desorbed solution are concentrated to get secondary concentration liquid by film；
The deacetyl-7-aminocephalosporanicacid acid that step 4), secondary concentration liquid are recycled by crystallization.
2. deacetyl-7-aminocephalosporanicacid acid mother liquor reclaiming method according to claim 1, it is characterised in that: described
Parsing agent is that organic solvent is added in sodium bicarbonate solution.
3. deacetyl-7-aminocephalosporanicacid acid mother liquor reclaiming method according to claim 2, it is characterised in that: described
The mass fraction of sodium bicarbonate solution is 4%.
4. deacetyl-7-aminocephalosporanicacid acid mother liquor reclaiming method according to claim 2 or 3, it is characterised in that: institute
State the one or more that organic solvent is methanol, acetone or isopropanol.
5. deacetyl-7-aminocephalosporanicacid acid mother liquor reclaiming method according to claim 4, it is characterised in that: described
Mass fraction of the organic solvent in parsing agent is 4-5%.
6. deacetyl-7-aminocephalosporanicacid acid mother liquor reclaiming method according to claim 5, it is characterised in that: described
Organic solvent is acetone, and the mass fraction in parsing agent is 4%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711245340.0A CN107936041B (en) | 2017-12-01 | 2017-12-01 | Deacetyl-7-aminocephalosporanicacid acid mother liquor reclaiming method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711245340.0A CN107936041B (en) | 2017-12-01 | 2017-12-01 | Deacetyl-7-aminocephalosporanicacid acid mother liquor reclaiming method |
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| CN107936041A CN107936041A (en) | 2018-04-20 |
| CN107936041B true CN107936041B (en) | 2019-08-23 |
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| CN201711245340.0A Active CN107936041B (en) | 2017-12-01 | 2017-12-01 | Deacetyl-7-aminocephalosporanicacid acid mother liquor reclaiming method |
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| CN110317215A (en) * | 2019-07-26 | 2019-10-11 | 伊犁川宁生物技术有限公司 | A method of reducing DO-7-ACA impurity content in D-7-ACA |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6465233B1 (en) * | 1998-01-28 | 2002-10-15 | Biochemie Gesellschaft M.B.H. | Nucleic acid molecule encoding a cephalosporin acetylesterase |
| CN102584561A (en) * | 2011-12-14 | 2012-07-18 | 伊犁川宁生物技术有限公司 | Method for recovering glutaric acid by-products produced in enzymic method prepared 7-aminocephalosporin acid process |
| CN102702231A (en) * | 2012-06-18 | 2012-10-03 | 山东大学 | Method for preparing 3-descarbamoyl-cefuroxime acid |
| CN103193800A (en) * | 2013-04-08 | 2013-07-10 | 中国医药集团总公司四川抗菌素工业研究所 | Method for separating and purifying various components from cefaclor enzymatic reaction solution |
| CN104402905A (en) * | 2014-10-30 | 2015-03-11 | 华北制药河北华民药业有限责任公司 | Method for recovering 7-aminocephalosporanic acid (7-ACA) from 7-ACA mother liquor |
-
2017
- 2017-12-01 CN CN201711245340.0A patent/CN107936041B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6465233B1 (en) * | 1998-01-28 | 2002-10-15 | Biochemie Gesellschaft M.B.H. | Nucleic acid molecule encoding a cephalosporin acetylesterase |
| CN102584561A (en) * | 2011-12-14 | 2012-07-18 | 伊犁川宁生物技术有限公司 | Method for recovering glutaric acid by-products produced in enzymic method prepared 7-aminocephalosporin acid process |
| CN102702231A (en) * | 2012-06-18 | 2012-10-03 | 山东大学 | Method for preparing 3-descarbamoyl-cefuroxime acid |
| CN103193800A (en) * | 2013-04-08 | 2013-07-10 | 中国医药集团总公司四川抗菌素工业研究所 | Method for separating and purifying various components from cefaclor enzymatic reaction solution |
| CN104402905A (en) * | 2014-10-30 | 2015-03-11 | 华北制药河北华民药业有限责任公司 | Method for recovering 7-aminocephalosporanic acid (7-ACA) from 7-ACA mother liquor |
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| CN107936041A (en) | 2018-04-20 |
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