CN1526706A - Process of recovering 2-mercaptan benzothiazole from cefotaxime producing slag - Google Patents
Process of recovering 2-mercaptan benzothiazole from cefotaxime producing slag Download PDFInfo
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- CN1526706A CN1526706A CNA031326242A CN03132624A CN1526706A CN 1526706 A CN1526706 A CN 1526706A CN A031326242 A CNA031326242 A CN A031326242A CN 03132624 A CN03132624 A CN 03132624A CN 1526706 A CN1526706 A CN 1526706A
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- benzothiazolyl mercaptan
- waste residue
- cefotaxime sodium
- mercaptan
- cefotaxime
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Abstract
The present invention relates to recovering of slag in pharmaceutical industry. The process of recovering 2-mercaptan benzothiazole from cefotaxime producing slag includes leaching cefotaxime producing slag in alkali sodium hydroxide solution; filtering; separation; filtering; dissolving; purification; and drying to obtain 2-mercaptan benzothiazole. The said recovering process uses organic solvent acetone and adding water in the purification, so that it has high recovered product purity, high yield and low cost.
Description
Technical field: the recovery method that the present invention relates to the waste residue that produces in a kind of pharmaceutical industry.
Background technology: cefotaxime sodium is the third generation cephalosporin analog antibiotic medicine that at present how tame at home pharmaceutical factory produces, and this medicine is strong because of its anti-microbial effect, and multiple disease is had better curative effect and good use prospect is arranged.Cefotaxime sodium produces a large amount of waste residues in the esterification and the condensation workshop section of its production, contains multiple pungency, corrodibility, toxic component in the waste residue, therefore not only causes environmental pollution, and HUMAN HEALTH is caused serious harm; And the existing method cost height that from cefotaxime sodium production waste residue, reclaims the 2-benzothiazolyl mercaptan, products obtained therefrom purity is low, and the rate of recovery is low.
Summary of the invention: the object of the present invention is to provide a kind of simple to operate, cost is low and product recovery rate is high produces the method that reclaims the 2-benzothiazolyl mercaptan the waste residue from cefotaxime sodium, its recovery method is: a. leaching: cefotaxime sodium is produced waste residue put into basic solution and leach, the used basic solution of leaching process is a sodium hydroxide solution; B. filter: leach liquor is filtered; C. separate out: in leach liquor, add concentration and be 1～2% sulphuric acid soln the 2-benzothiazolyl mercaptan is separated out; D. filter: get crude product 2-benzothiazolyl mercaptan after the filtration; E. dissolving: crude product 2-benzothiazolyl mercaptan is put into organic solvent fully dissolve; F. purify: add water in lysate, the 2-benzothiazolyl mercaptan is separated out again can purify; G. dry: as will promptly to get the 2-benzothiazolyl mercaptan after the gained crystal drying.Produce recovery 2-benzothiazolyl mercaptan the waste residue with method of the present invention from cefotaxime sodium, its purity can reach national technical grade product standard, the rate of recovery reaches more than 90%, method of the present invention has not only reduced waste discharge, alleviate environmental pollution, and brought remarkable economic efficiency for enterprise.With respect in the past use sodium carbonate solution at leaching process, the present invention produces waste residue with cefotaxime sodium and puts into sodium hydroxide solution and leach, can improve the purity of 2-benzothiazolyl mercaptan, improve the rate of recovery of 2-benzothiazolyl mercaptan, and can reduce cost; The present invention is an acetone at the used organic solvent of the dissolution process of e., compares with the ethanol that adopts in the past, uses acetone can improve the purity of 2-benzothiazolyl mercaptan; Add water at purification process, can improve the purity of 2-benzothiazolyl mercaptan equally.Adopt method of the present invention to produce the 2-benzothiazolyl mercaptan quality that reclaims the waste residue and can reach the HGB2-157-61 standard, have good popularizing application prospect from cefotaxime sodium.
Embodiment: the recovery method of present embodiment is: a. leaching: cefotaxime sodium is produced waste residue put into basic solution and leach, the used basic solution of leaching process is a sodium hydroxide solution, sodium hydroxide solution 11～the 12ml that adds 0.4～0.5mol/L in every 1g waste residue, leaching temperature is 60～65 ℃, and leaching time is 25～35 minutes; B. filter: leach liquor filters, and will soak the back slag and discharge, and gets leach liquor, leach liquor can be stored for some time; C. separate out: add concentration and be 1～2% sulphuric acid soln in leach liquor the 2-benzothiazolyl mercaptan is separated out, it is 3.0～4.0 that precipitation process needs the pH value; D. filter: get crude product 2-benzothiazolyl mercaptan after the filtration, in the filtrate and back is discharged; E. dissolving: crude product 2-benzothiazolyl mercaptan is put into organic solvent fully dissolve, used organic solvent is an acetone, and the weight that adds acetone is 3～4 times of crude product 2-benzothiazolyl mercaptan weight; F. purify: add water in lysate, the 2-benzothiazolyl mercaptan is separated out again can purify, and the weight that adds entry is 5～7 times of acetone weight, leach desired substance after, the aqueous solution of gained acetone acetone after Separation and Recovery goes out acetone can be reused; G. dry: as promptly to get the 2-benzothiazolyl mercaptan after the gained crystal drying.
Claims (7)
1, a kind ofly produce the method that reclaims the 2-benzothiazolyl mercaptan the waste residue from cefotaxime sodium, its recovery method is: a. leaching: cefotaxime sodium is produced waste residue put into basic solution and leach; B. filter: leach liquor is filtered; C. separate out: in leach liquor, add concentration and be 1～2% sulphuric acid soln the 2-benzothiazolyl mercaptan is separated out; D. filter: get crude product 2-benzothiazolyl mercaptan after the filtration; E. dissolving: crude product 2-benzothiazolyl mercaptan is put into organic solvent fully dissolve; F. purify: add water in lysate, the 2-benzothiazolyl mercaptan is separated out again can purify; G. dry: as will promptly to get the 2-benzothiazolyl mercaptan after the gained crystal drying, it is characterized in that the used basic solution of a. leaching process is a sodium hydroxide solution.
2, according to claim 1ly produce the method that reclaims the 2-benzothiazolyl mercaptan the waste residue, it is characterized in that putting in every 1g waste residue sodium hydroxide solution 11～12ml of 0.4～0.5mol/L from cefotaxime sodium.
3, method of producing recovery 2-benzothiazolyl mercaptan the waste residue from cefotaxime sodium according to claim 1 is characterized in that organic solvent used in the e. dissolution process is an acetone.
4, according to claim 3ly produce the method that reclaims the 2-benzothiazolyl mercaptan the waste residue from cefotaxime sodium, the weight that it is characterized in that adding acetone is 3～4 times of crude product 2-benzothiazolyl mercaptan weight.
5, method of producing recovery 2-benzothiazolyl mercaptan the waste residue from cefotaxime sodium according to claim 3 is characterized in that in the f. purification process that the weight that adds water is 5～7 times of acetone weight.
6, according to claim 1,2,3,4 or 5 described methods of producing recovery 2-benzothiazolyl mercaptan the waste residue from cefotaxime sodium, it is characterized in that leaching temperature is 60～65 ℃ in a. leaching process, leaching time is 25～35 minutes.
7, according to claim 1,2,3,4 or 5 described methods of producing recovery 2-benzothiazolyl mercaptan the waste residue, it is characterized in that it is 3.0～4.0 that the c. precipitation process needs the pH value from cefotaxime sodium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03132624 CN1242998C (en) | 2003-09-19 | 2003-09-19 | Process of recovering 2-mercaptan benzothiazole from cefotaxime producing slag |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 03132624 CN1242998C (en) | 2003-09-19 | 2003-09-19 | Process of recovering 2-mercaptan benzothiazole from cefotaxime producing slag |
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| CN1526706A true CN1526706A (en) | 2004-09-08 |
| CN1242998C CN1242998C (en) | 2006-02-22 |
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| CN 03132624 Expired - Fee Related CN1242998C (en) | 2003-09-19 | 2003-09-19 | Process of recovering 2-mercaptan benzothiazole from cefotaxime producing slag |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102690243A (en) * | 2012-05-25 | 2012-09-26 | 伊犁川宁生物技术有限公司 | Method for recovering raw materials in preparation process of 7-phenylacetamide-3-chloromethyl-3-cephem-4-carboxylic acid p-methoxybenzyl |
| CN115403827A (en) * | 2022-08-02 | 2022-11-29 | 山东戴瑞克新材料有限公司 | M resin treatment method |
-
2003
- 2003-09-19 CN CN 03132624 patent/CN1242998C/en not_active Expired - Fee Related
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102690243A (en) * | 2012-05-25 | 2012-09-26 | 伊犁川宁生物技术有限公司 | Method for recovering raw materials in preparation process of 7-phenylacetamide-3-chloromethyl-3-cephem-4-carboxylic acid p-methoxybenzyl |
| CN102690243B (en) * | 2012-05-25 | 2014-07-16 | 伊犁川宁生物技术有限公司 | Method for recovering raw materials in preparation process of 7-phenylacetamide-3-chloromethyl-3-cephem-4-carboxylic acid p-methoxybenzyl |
| CN115403827A (en) * | 2022-08-02 | 2022-11-29 | 山东戴瑞克新材料有限公司 | M resin treatment method |
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| CN1242998C (en) | 2006-02-22 |
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