CN101735247B - Process for drying 7-aminocephalosporanic acid - Google Patents
Process for drying 7-aminocephalosporanic acid Download PDFInfo
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- CN101735247B CN101735247B CN2008102307926A CN200810230792A CN101735247B CN 101735247 B CN101735247 B CN 101735247B CN 2008102307926 A CN2008102307926 A CN 2008102307926A CN 200810230792 A CN200810230792 A CN 200810230792A CN 101735247 B CN101735247 B CN 101735247B
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- cephalosporanic acid
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The invention provides a process and equipment thereof for drying 7-aminocephalosporanic acid. The equipment comprises a horizontal tank, wherein the horizontal tank is provided with a stirring device, the upper part of the horizontal tank is provided with a solvent distilling pipe and a solvent reflow pipe, the lower part of the horizontal tank is provided with a discharging pipe; the other end of the solvent distilling pipe is arranged at the lower part of a condensation device, the lower end of the condensation device is provided with a collection and distribution device, the upper end of the condensation device is provided with a vacuum pump; and the solvent reflow pipe is connected with the upper part of the collection and distribution device, and the lower end of the collection and distribution device is provided with a water outlet. Because boiling points of organic solvent and water under the vacuum state are lowered, the temperature during the whole dehydrating and drying is lower, and the products can be effectively protected from being damaged; and meanwhile, because the temperature of the solvent is lower, the volatilization is reduced, the cost is lowered, and the health of operators is protected.
Description
Technical field
The present invention relates to a kind of 7-amino-cephalosporanic acid drying process and equipment thereof.
Background technology
The abbreviation of 7-amino-cephalosporanic acid is 7-ACA, and he is the important intermediate of present domestic production cephalosporin analog antibiotic.
At present domestic common employing chemical method is produced 7-ACA, because the 7-ACA of chemical method production is having crystallization under the condition of solvent, filtration, washing, therefore its crystal formation is thicker, and contain solvent, after having filtered, moisture content is about 20%, and is dry easily, so adopt oven drying, double-cone dryer drying and boiled bed drying to come drying products more.
7-ACA with Production by Enzymes is that crystal formation is more tiny in the aqueous phase crystallization, and specific surface area is big, therefore water content is big, after having filtered, moisture is about 50%, with the 7-ACA employing traditional method drying of Production by Enzymes, reach time of drying more than 48 hours, because time of drying is longer, 7-ACA degrades, and purity descends, the look level of output product reaches (yellow or yellow-green colour) 6-8 number, does not meet existing quality standard (the look level is not more than (yellow or yellow-green colour) No. 4).And the characteristic of 7-ACA non-refractory has determined that the exsiccant temperature can not be too high, after drying temperature surpasses 45 ℃, also easily causes the look level to raise, and then the look level of subsequent product is raise, and does not meet state-promulgated pharmacopoeia.
Chemical method is produced the 7-ACA reaction process and is used solvent many, and the poisonous and harmful chemical is many, pollutes big.In the long run, Production by Enzymes 7-ACA must the substituted chemistry method produce 7-ACA.And for above-mentioned reasons, the drying process of the 7-ACA of Production by Enzymes and equipment become the bottleneck technology that restriction Production by Enzymes 7-ACA applies.Drying process and the equipment of the suitable Production by Enzymes 7-ACA of exploitation are extremely urgent.
Summary of the invention
The purpose of this invention is to provide a kind of 7-amino-cephalosporanic acid drying process and equipment thereof.
In order to achieve the above object the present invention by the following technical solutions, the 7-amino-cephalosporanic acid drying process may further comprise the steps:
A. the wet-milling with organic solvent and 7-amino-cephalosporanic acid joins in the jar that crouches, and stirs, and heats solvent with hot water, opens vacuum pump and carries out underpressure distillation, keeps organic solvent temperature to be no more than 45 ℃;
B. utilize water and solvent binary azeotropic, the water in the wet-milling is taken out of;
C. in condensing works, with the condensation of gas that distills, and collect condensed liquid, and moisture is removed, during solvent is got back to and crouched jar with the collection division box;
D. drop to 15% when following when product moisture, collect the product in crouching jar, it is dry that product is put into double-cone dryer, obtains finished product then.
Among the step a, described organic solvent is alkane, ester or benzene.
The 7-amino-cephalosporanic acid drying process, used equipment is: the jar that crouches, jar for sleeping in is provided with whipping appts, and jar top of crouching offers solvent distillation pipeline and solvent reflux line, and a jar bottom is provided with discharge nozzle crouching; The solvent distillation pipeline the other end is arranged on the bottom of condensing works, and the condensing works lower end is provided with the collection division box, and the condensing works upper end is provided with vacuum pump; The solvent reflux line is connected with collection division box top, collects the division box lower end and is provided with water outlet.
Condensing works is provided with refrigerant import and refrigerant exit.
The jar that crouches is provided with water inlet of hot water and water outlet.
Because organic solvent and water boiling point lowering under vacuum state, therefore the whole drying process temperature that dewaters is lower, can effectively protect product not to be damaged; simultaneously because the temperature of solvent is lower; reduce volatilization, reduced cost, also protected operator's health simultaneously.
Description of drawings
Accompanying drawing is the synoptic diagram of 7-amino-cephalosporanic acid drying process equipment flow process of the present invention.
Embodiment
Embodiment
The 7-amino-cephalosporanic acid drying process, used equipment is: the jar 1 that crouches, jar for sleeping in is provided with whipping appts 2, and jar top of crouching offers solvent distillation pipeline 6 and solvent reflux line 7, and a jar bottom is provided with discharge nozzle 10 crouching; The solvent distillation pipeline the other end is arranged on the bottom of condensing works 3, and the condensing works lower end is provided with collects division box 4, and the condensing works upper end is provided with vacuum pump 5; The solvent reflux line is connected with collection division box top, collects the division box lower end and is provided with water outlet 13.Condensing works is provided with refrigerant import 9 and refrigerant exit 8.The jar that crouches is provided with water inlet of hot water 11 and water outlet 12.
The 7-ACA wet-milling of certain amount of organic solvent (volatile alkanes, ester class, benzene class etc.) and water content 50% is joined in the jar that crouches, stir, heat solvent, open vacuum pump and carry out underpressure distillation, keep the temperature of organic solvent to be no more than 45 ℃ with hot water.Utilize solvent and water binary azeotropic principle, the water in the wet-milling is taken out of, utilize condensing works and collect division box with the condensation of gas collection that distills out, by water trap moisture is removed, solvent is got back to the jar that crouches, and carries out recycle.Because this operation is carried out under vacuum state, so temperature is lower, can effectively protect product.When moisture drops to 15% when following, collect product, cooperate the double-cone dryer drying, product moisture can be reduced in 1%.The product purity that obtains is more than 98%, and the look level is below No. 3, and other indexs also all meet quality standard.
Claims (4)
1. 7-amino-cephalosporanic acid drying process is characterized in that may further comprise the steps:
A. the wet-milling with organic solvent and 7-amino-cephalosporanic acid joins in the jar that crouches, and stirs, and heats solvent with hot water, opens vacuum pump and carries out underpressure distillation, keeps organic solvent temperature to be no more than 45 ℃; Described organic solvent is alkane, ester or benzene;
B. utilize water and solvent binary azeotropic, the water in the wet-milling is taken out of;
C. in condensing works, with the condensation of gas that distills, and collect condensed liquid, and moisture is removed, during solvent is got back to and crouched jar with the collection division box;
D. drop to 15% when following when product moisture, collect the product in crouching jar, it is dry that product is put into double-cone dryer, obtains finished product then.
2. want the 7-amino-cephalosporanic acid drying process described in 1 according to right, it is characterized in that used equipment is: the jar that crouches, jar for sleeping in is provided with whipping appts, and jar top of crouching offers solvent distillation pipeline and solvent reflux line, and a jar bottom is provided with discharge nozzle crouching; The solvent distillation pipeline the other end is arranged on the bottom of condensing works, and the condensing works lower end is provided with the collection division box, and the condensing works upper end is provided with vacuum pump; The solvent reflux line is connected with collection division box top, collects the division box lower end and is provided with water outlet.
3. 7-amino-cephalosporanic acid drying process according to claim 2 is characterized in that: condensing works is provided with refrigerant import and refrigerant exit.
4. 7-amino-cephalosporanic acid drying process according to claim 2 is characterized in that: the jar that crouches is provided with water inlet of hot water and water outlet.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102307926A CN101735247B (en) | 2008-11-07 | 2008-11-07 | Process for drying 7-aminocephalosporanic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2008102307926A CN101735247B (en) | 2008-11-07 | 2008-11-07 | Process for drying 7-aminocephalosporanic acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101735247A CN101735247A (en) | 2010-06-16 |
| CN101735247B true CN101735247B (en) | 2011-08-10 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008102307926A Active CN101735247B (en) | 2008-11-07 | 2008-11-07 | Process for drying 7-aminocephalosporanic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101735247B (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1085904A (en) * | 1993-08-11 | 1994-04-27 | 东北制药总厂 | The process for purification of 7-amino-cephalosporanic acid |
| CN1557962A (en) * | 2004-02-10 | 2004-12-29 | 清华大学 | Production method of 7-amino cephalosporanic acid |
-
2008
- 2008-11-07 CN CN2008102307926A patent/CN101735247B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1085904A (en) * | 1993-08-11 | 1994-04-27 | 东北制药总厂 | The process for purification of 7-amino-cephalosporanic acid |
| CN1557962A (en) * | 2004-02-10 | 2004-12-29 | 清华大学 | Production method of 7-amino cephalosporanic acid |
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| Publication number | Publication date |
|---|---|
| CN101735247A (en) | 2010-06-16 |
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