CN113968827A - Regeneration treatment process for waste material in cephalosporin production in pharmaceutical industry - Google Patents
Regeneration treatment process for waste material in cephalosporin production in pharmaceutical industry Download PDFInfo
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- CN113968827A CN113968827A CN202010712557.3A CN202010712557A CN113968827A CN 113968827 A CN113968827 A CN 113968827A CN 202010712557 A CN202010712557 A CN 202010712557A CN 113968827 A CN113968827 A CN 113968827A
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- kettle
- hydrogen peroxide
- dibenzothiazyl disulfide
- mercaptobenzothiazole
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D277/00—Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings
- C07D277/60—Heterocyclic compounds containing 1,3-thiazole or hydrogenated 1,3-thiazole rings condensed with carbocyclic rings or ring systems
- C07D277/62—Benzothiazoles
- C07D277/68—Benzothiazoles with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached in position 2
- C07D277/70—Sulfur atoms
- C07D277/76—Sulfur atoms attached to a second hetero atom
- C07D277/78—Sulfur atoms attached to a second hetero atom to a second sulphur atom
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Cephalosporin Compounds (AREA)
Abstract
The invention discloses a regeneration treatment process for waste materials in cephalosporin production in pharmaceutical industry. Adding the recovered mercaptobenzothiazole into a dissolving kettle (ethanol, acetone or isopropanol is added into the reaction kettle), heating and dissolving, carrying out hot filter pressing on the mercaptobenzothiazole into an adsorption kettle (activated carbon, argil or nano-scale silica spheres are added into the reaction kettle), carrying out hot filter pressing on the mercaptobenzothiazole into an oxidation kettle, dripping hydrogen peroxide into the oxidation kettle at the temperature of 60-65 ℃, diluting the hydrogen peroxide to 3% by using a solvent, oxidizing the hydrogen peroxide to obtain DM (dibenzothiazyl disulfide), filtering and vacuum drying the DM which is not dissolved in the used solvent after oxidation, and recovering and reusing a mother solution. Compared with the prior art, the invention has the following advantages: the existing process is to use water phase method acid and alkali to generate sewage, sodium sulfate cannot be treated, the process is carried out under full sealing, nitrogen is used for filter pressing during filter pressing, and the set of equipment can be used for producing various products, so that the process is safe and environment-friendly.
Description
Technical Field
The invention relates to treatment of production waste in pharmaceutical industry, in particular to a regeneration treatment process of waste in cephalosporin production in pharmaceutical industry.
Background
Dibenzothiazyl disulfide (DM for short) is an important intermediate for producing cephalosporin active ester, and can react with cephalosporin side chain acid under the action of triphenylphosphine or triethyl phosphite to obtain cephalosporin active ester, such as AE-active ester, ceftazidime active ester, cefdinir active ester, cefixime active ester, etc. The utilization rate of DM in the production process of the cephalosporin active ester is only 50 percent, half of DM exists in the mother liquor of the active ester in the form of a by-product 2-mercaptobenzothiazole (M for short) and is not utilized, and the M is unstable, so that the high-purity product is difficult to obtain by concentrating and recycling the mother liquor to realize recycling. Because no effective technology is available for recycling, a large number of enterprises treat waste residues generated after mother liquor recovery as waste, which causes serious resource waste and environmental pollution.
Therefore, the development of M green recycling technology can greatly reduce the discharge amount of wastes, meet the requirement of circular economy and have important social and economic significance.
Disclosure of Invention
The invention aims to provide a waste regeneration treatment process for producing cephalosporins in pharmaceutical industry aiming at the defects in the prior art.
The technical scheme is as follows: a waste material regeneration treatment process for producing cephalosporins in pharmaceutical industry comprises the following steps:
extraction of dibenzothiazyl disulfide
(1) Adding the recovered mercaptobenzothiazole into a dissolving kettle, adding ethanol or acetone or isopropanol into the dissolving kettle, and heating for dissolving;
(2) after dissolution, hot pressing and filtering the mixture to an adsorption kettle, and adding active carbon or argil or nano-scale silicon dioxide balls into the adsorption kettle;
(3) hot filter pressing the mixture into an oxidation kettle at the temperature of between 60 and 65 ℃;
(4) dropping hydrogen peroxide into the oxidation kettle, diluting the hydrogen peroxide to 3% by using a solvent, and oxidizing to obtain dibenzothiazyl disulfide;
(5) after oxidation, dibenzothiazyl disulfide is not dissolved in the solvent, filtering, vacuum drying, and recovering mother liquor for reuse.
Second, refined dibenzothiazyl disulfide
(1) And (3) adding the recovered DM into a dissolving kettle, dissolving the dissolved M in a solvent, and removing other impurities by filtering, wherein the other impurities are insoluble in the solvent.
(2) Filter-pressing into an adsorption kettle, adding an adsorbent to remove color, removing micro particles, and filtering to remove the adsorbent into an oxidation kettle.
(3) Adding hydrogen peroxide into the oxidation kettle to oxidize M into DM which is insoluble in the solvents, filtering and drying to obtain qualified product refined DM, taking away the solvent in a small amount of the cephalosporin mother liquor in the recovered M by the solvent, separating and recovering the mother liquor, and treating and discharging a small amount of wastewater produced by hydrogen peroxide.
Compared with the prior art, the invention has the following advantages: the existing process is to use water phase method acid and alkali to generate sewage, sodium sulfate cannot be treated, the process is carried out under full sealing, nitrogen is used for filter pressing during filter pressing, and the set of equipment can be used for producing various products, so that the process is safe and environment-friendly.
Drawings
FIG. 1 is a schematic flow chart of the steps of the present invention.
Detailed Description
Furthermore, the terms "first", "second" and "first" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implicitly indicating the number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
Adding the recovered mercaptobenzothiazole into a dissolving kettle (ethanol, acetone or isopropanol is added in the reaction kettle), heating and dissolving, carrying out hot filter pressing on the mercaptobenzothiazole to an adsorption kettle (activated carbon or argil or nano-scale silica spheres are added in the reaction kettle), carrying out hot filter pressing on the mercaptobenzothiazole to an oxidation kettle, dripping hydrogen peroxide into the oxidation kettle at the temperature of 60-65 ℃, diluting the hydrogen peroxide to 3% by using a solvent, oxidizing the hydrogen peroxide to obtain DM (dibenzothiazyl disulfide), dissolving the DM in the used solvent after oxidation, filtering, vacuum drying, and recycling the mother liquor.
The process can also be used for producing refined DM by using normally produced high-purity M, producing byproducts of cephalosporin production, and having a lot of impurities in M, because the cephalosporin production uses mixed solvents, the products are different, the solvents are different, the recovery is difficult to purify, then 49 cephalosporin exist, 29 AE-activities exist, the AE-active substances are used for producing cephalosporin, and M and DM are recovered, and the process is used for secondarily purifying the recovered M to produce DM.
1. And (3) adding the recovered DM into a dissolving kettle, dissolving the dissolved M in a solvent, and removing other impurities by filtering, wherein the other impurities are insoluble in the solvent.
2. Filter-pressing into an adsorption kettle, adding an adsorbent to remove color, removing micro particles, and filtering to remove the adsorbent into an oxidation kettle.
3. Adding hydrogen peroxide into the oxidation kettle to oxidize M into DM which is insoluble in the solvents, filtering and drying to obtain qualified product refined DM, taking away the solvent in a small amount of the cephalosporin mother liquor in the recovered M by the solvent, separating and recovering the mother liquor, and treating and discharging a small amount of wastewater produced by hydrogen peroxide.
The existing process is to use water phase method acid and alkali to generate sewage, sodium sulfate cannot be treated, the process is carried out under full sealing, nitrogen is used for filter pressing during filter pressing, and the set of equipment can be used for producing various products, so that the process is safe and environment-friendly.
Nothing is mentioned about the common general knowledge.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (1)
1. A regeneration treatment process for waste materials in cephalosporin production in pharmaceutical industry is characterized in that: the method comprises the following steps:
step one, extracting dibenzothiazyl disulfide:
(1) adding the recovered 2-mercaptobenzothiazole into a dissolving kettle, adding ethanol or acetone or isopropanol into the dissolving kettle, and heating for dissolving;
(2) after dissolution, hot pressing and filtering the mixture to an adsorption kettle, and adding active carbon or argil or nano-scale silicon dioxide balls into the adsorption kettle;
(3) hot filter pressing the mixture into an oxidation kettle at the temperature of between 60 and 65 ℃;
(4) dropping hydrogen peroxide into the oxidation kettle, diluting the hydrogen peroxide to 3% by using a solvent, and oxidizing to obtain dibenzothiazyl disulfide;
(5) after oxidation, dibenzothiazyl disulfide is not dissolved in the used solvent, filtering, vacuum drying, and recycling the mother liquor;
step two, refining dibenzothiazyl disulfide:
(1) adding the recovered dibenzothiazyl disulfide into a dissolving kettle, dissolving the 2-mercaptobenzothiazole in a solvent, and removing other impurities by filtering, wherein the other impurities are insoluble in the solvent;
(2) filter-pressing into an adsorption kettle, adding an adsorbent to remove color, removing micro particles, and filtering to remove the adsorbent to oxygen;
(3) adding hydrogen peroxide into the oxidation kettle, oxidizing the 2-mercaptobenzothiazole into dibenzothiazyl disulfide, wherein the dibenzothiazyl disulfide is insoluble in the solvents, filtering and drying to obtain qualified refined dibenzothiazyl disulfide, taking away the solvents in a small amount of cephalosporin mother liquor in the recovered 2-mercaptobenzothiazole by the solvents, separating and recovering the mother liquor, and discharging a small amount of wastewater produced by hydrogen peroxide after treatment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010712557.3A CN113968827A (en) | 2020-07-22 | 2020-07-22 | Regeneration treatment process for waste material in cephalosporin production in pharmaceutical industry |
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| CN202010712557.3A CN113968827A (en) | 2020-07-22 | 2020-07-22 | Regeneration treatment process for waste material in cephalosporin production in pharmaceutical industry |
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Citations (9)
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| CN102807533A (en) * | 2012-08-25 | 2012-12-05 | 华北制药河北华民药业有限责任公司 | Method utilizing cefotaxime acid waste-liquor to prepare 2, 2'-dithio-dibenzo thiazole |
| CN102850293A (en) * | 2012-09-14 | 2013-01-02 | 温州市嘉力化工有限公司 | Refining method of dibenzothiazole disulfide (DM) |
| CN105418536A (en) * | 2015-12-29 | 2016-03-23 | 河北合佳医药科技集团有限公司 | Method for preparing 2,2'-dithiodibenzothiazole from waste residues generated during process of AE-active ester production |
| CN107879995A (en) * | 2017-10-26 | 2018-04-06 | 淄博鑫泉医药技术服务有限公司 | The method that the M synthesis DM reclaimed in raffinate is synthesized using cefotaxime acid |
| CN109111409A (en) * | 2018-10-18 | 2019-01-01 | 河南省化工研究所有限责任公司 | A method of benzothiazole is produced from the waste material of production 2-mercaptobenzothiazole |
| CN109810075A (en) * | 2019-03-03 | 2019-05-28 | 朝阳天铭工贸有限公司 | A kind of technique of isopropanol method purification DM |
| CN110330466A (en) * | 2019-07-25 | 2019-10-15 | 山东金城医药化工有限公司 | The method of curing di-mercaptobenzothiazolby is recycled from cephalo active ester production mother liquor |
| CN110746373A (en) * | 2019-12-06 | 2020-02-04 | 广东省生物医药技术研究所 | Method for preparing 2, 2' -dithiodibenzothiazole from crude pinosylvin sodium mother liquor and application thereof |
| CN111039894A (en) * | 2019-11-07 | 2020-04-21 | *** | Method for producing DM (direct methanol gasoline) by utilizing recycled rubber accelerator M waste |
-
2020
- 2020-07-22 CN CN202010712557.3A patent/CN113968827A/en active Pending
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| CN111039894A (en) * | 2019-11-07 | 2020-04-21 | *** | Method for producing DM (direct methanol gasoline) by utilizing recycled rubber accelerator M waste |
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