CN103833591B - Preparation method of hydrochloric acid aureomycin - Google Patents
Preparation method of hydrochloric acid aureomycin Download PDFInfo
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- CN103833591B CN103833591B CN201410057354.XA CN201410057354A CN103833591B CN 103833591 B CN103833591 B CN 103833591B CN 201410057354 A CN201410057354 A CN 201410057354A CN 103833591 B CN103833591 B CN 103833591B
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Abstract
The invention relates to a preparation method of hydrochloric acid aureomycin; the technical steps are listed below: firstly acidifying aureomycin broth; adjusting pH to 2-2.5; standing; continuously adjusting pH to 4-4.5; standing; adding water to reduce viscosity to 3000-4000cps pretreatment; carrying out membrane filtration, nanofiltration, crystallization, washing, salt forming, leaching and drying to obtain hydrochloric acid aureomycin powders. The method can improve extraction yield of the hydrochloric acid aureomycin, reduces production cycle and cost, and improves hydrochloric acid aureomycin output.
Description
Technical field
The invention belongs to microbiotic extraction, synthesis technical field, particularly relate to a kind of preparation method of Isphamycin.
Background technology
Isphamycin belongs to tetracycline antibiotics, has broad-spectrum antibacterial action, and its antimicrobial spectrum is similar to tsiklomitsin, all has anti-microbial effect to most gram-positive microorganism and Gram-negative bacteria.In addition, they can also suppress Rickettsiae and sand holes virus and lymphogranuloma virus.
At present, domestic disclosed method of producing Isphamycin mainly contains: application number be 201210426529.0 " preparation method of Isphamycin " and application number be 201010218988.0 " a kind of novel process preparing Isphamycin ".There are the following problems for above-mentioned patent:
In 1 patent " preparation method of Isphamycin ", in filtering fermentation liquor process, adopt sheet frame as filter plant, in order to ensure to filter yield, need filter cake in a large amount of clear water repetitive scrubbing sheet frame, reduce the duomycin remained in filter cake as far as possible, so wastewater discharge is more than 2 times of fermentating liquid volume substantially, causes scale wastewater treatment cost comparatively large, cause products production cost to raise; Simultaneously owing to using plate-and-frame filter press, its floor space is large, cleans used artificial many, poor working environment.
In 2 patents " preparation method of Isphamycin ", in fermentation liquor pretreatment process, employ a large amount of ZnSO
4and oxalic acid, and in patent " a kind of novel process preparing Isphamycin ", a large amount of divalent metal salt and monohydroxy-alcohol of using in its duomycin filtrate, the use of above-mentioned substance causes duomycin production cost constantly to rise.
3 above-mentioned two kinds of patented technologies, employ a large amount of divalent metal salts in the extraction process of duomycin, and due to metallic pollution, filter cake and filtrate cannot realize recycling, cause serious pollution to local soil.
In 4 above-mentioned two kinds of patented technologies, in duomycin filtrate alkalinization, be difficult to avoid causing partial concn too high, cause the phenomenon that it is degraded.
There is the underproof problem of final product quality, mainly finished product impurity content exceeding index in 5 patented technologies " a kind of novel process preparing Isphamycin ".
In 6 above-mentioned two kinds of patented technologies, duomycin extract yield is generally 75 ~ 80%, and yield is on the low side.
Summary of the invention
Object of the present invention is just the defect overcoming above-mentioned prior art, provides one effectively to improve extract yield, reduces costs, and shortens the production cycle, reduces environmental pollution, and realization is stable, the preparation method of the Isphamycin of High-efficient Production.
Technical scheme taked for achieving the above object is:
A kind of preparation method of Isphamycin, it is characterized in that its processing step is: standing after first Aureomycin fermentation liquor being carried out acidifying, readjustment pH to 2 ~ 2.5, continuation leaves standstill and adds water after adjusting back pH to 4 ~ 4.5 and makes the pre-treatment of its viscosity drop to 3000 ~ 4000cps, obtains Isphamycin powder after then carrying out membrane filtration, nanofiltration, crystallization, washing, salify and drip washing and drying successively.
Described acidifying refers to that employing mass percent concentration is the acidic substance tune pH 0.5 ~ 1.5 of 15% ~ 20%, and pH regulator speed is every 4 ~ 6min, and pH value changes 1 unit.
Described acidic substance are hydrochloric acid, sulfuric acid or phosphoric acid.
Described readjustment refers to that employing mass percent concentration is the alkaline matter tune pH of 15% ~ 20%, and pH regulator speed is every 4 ~ 6min, and pH value changes 1 unit.
The described time left standstill for twice is 20 ~ 30min.
Described membrane filtration refers under 60 ~ 70 DEG C of conditions, and adopt high speed cross-current flow to carry out membrane filtration to pretreated duomycin filtrate, in filtration procedure, pressure-controlling is at 2.5-3.5bar, and flow rate control is at 0.3 ~ 0.5m
3/ m
2.h.
The filtering membrane that described membrane filtration adopts is inorganic metal micropore microfiltration membrane, and membrane pore size 0.1 ~ 0.5um, material is zirconium dioxide, and the support material of membrane filtration system is 316SS stainless steel.
Described nanofiltration refers under 30 ~ 40 DEG C of conditions, carries out nanofiltration to the first filtrate after membrane filtration, and in nanofiltration process, pressure-controlling is at 2 ~ 2.5MPa, and the concentrated volume multiple of nanofiltration is 3 ~ 5 times.
Described nanofiltration membrane module used is can block molecular weight to be less than the hollow-fibre membrane that 1000 are greater than the material of 100, and material is mixed type composite nanometer filtering film.
Described crystallization refers at the temperature of 10 ~ 20 DEG C, with alkali lye, the pH of nanofiltration filtrate is adjusted to 6 ~ 6.5, then adds the acetone of 60 ~ 80% of filtrate volume, separates out solid-state duomycin crystal, and leave standstill 10 ~ 20min, then solid-liquid separation obtains solid-state duomycin;
Described alkali lye is ammoniacal liquor or sodium hydroxide.
Described washing adds purified water in the solid-state duomycin pointing to described crystallization gained, and fully stir solid-liquid separation after 5 ~ 10min, wash 2 ~ 3 times, the ratio of adding water is 2 ~ 3L/kg.
Described salify refers to and starts crystallizer whipping device, and rotating speed controls at 20 ~ 30r/min, adds 8 ~ 16% technical hydrochloric acids, solution warms to 45 ~ 50 DEG C, regulates pH to 2.3 ~ 3.3, insulation 50 ~ 60min, and then to obtain hydrochloric acid gold mould for solid-liquid separation.
Described drip washing refers to uses ethanol rinse 2 ~ 3min again with after purified water drip washing 3 ~ 5min.
Described drying refers to that enabling bipyramid mixes powder machine, and regulate inlet temperature to 90 ~ 130 DEG C, temperature of outgoing air to 50 ~ 80 DEG C, add wet-milling in charging opening, after 8 ~ 12 order stainless steel meshs, with air-flow to cyclonic separator, arrives powder shifter and obtains Isphamycin through sieving.
Technical superiority of the present invention:
1 the present invention can effectively improve Isphamycin extract yield, reach 85 ~ 90%, higher than domestic similar level.
2 present invention, avoiding the pollution problem of heavy metal to environment.
3 production costs of the present invention are low, are conducive to the competitive power of the domestic and international market strengthening product.
4 present invention process are simple, time saving and energy saving.
specific implementation method
Be explained the present invention with example below, it should be understood that example is for illustration of the present invention instead of limitation of the present invention.Scope of the present invention and core content are determined according to claims.
embodiment 1
Pre-treatment
Aureomycin fermentation liquor 50m
3, initially tire 26307u/ml.
First Aureomycin fermentation liquor is carried out acidifying, the hydrochloric acid soln of 15% regulates pH to 0.5, secondly, adopts the sodium hydroxide solution of 15% to be adjusted to pH to 2 and 4 respectively; Leave standstill 20min, finally add tap water, the near 3847cps of fermentation broth viscosity.
Membrane filtration
Fermentation liquor pretreatment terminates, and filtrate is warming up to 61 DEG C, enters membrane filter plant, and use inorganic metal micropore microfiltration membrane, material is zirconium dioxide, and the support material of membrane filtration system is 316SS stainless steel.Filter type adopts high speed cross-current flow, membrane pore size 0.1um.In filtration procedure, pressure-controlling is at 2.5-3.5bar, and flow rate control is at 0.3 ~ 0.5m
3/ m
2.h.
Membrane filtration terminates, and filtrate volume is 49.6m
3, tire 28720u/ml, and yield is 108.3%.
Nanofiltration
Filtrate temperature controls at 31 DEG C, and in nanofiltration process, pressure-controlling is at 2-2.5MPa.The concentrated volume multiple of nanofiltration is 3.4 times.Nanofiltration terminates, and volume is 20m
3, tire 70456u/ml, and yield is 98.9%.
Crystallization
Filtrate temperature controls at 12 DEG C, and filtrate pH is adjusted to 6.1 by the sodium hydroxide with 15%, adds 12m
3acetone, separates out solid-state duomycin crystal, and solid-liquid separation obtains solid-state duomycin 1282kg, and yield is 91.2%.
Washing
Add 2564L purified water in solid duomycin, stir duomycin mixing solutions 5min, then solid-liquid separation.Obtain solid duomycin 1205kg.
Salify
Start crystallizer whipping device, rotating speed controls at 20r/min, adds 8% technical hydrochloric acid, solution warms to 45 DEG C, regulates pH to 2.3, and insulation 50min, then solid-liquid separation, obtain Isphamycin 1232kg, yield is 95%.
Drip washing and drying
With purified water drip washing Isphamycin 3min, then use ethanol rinse 2min.Enable bipyramid and mix powder machine, regulate inlet temperature to 90 ~ 130 DEG C, temperature of outgoing air to 50 ~ 80 DEG C, add wet-milling in charging opening, after 8 ~ 12 order stainless steel meshs, with air-flow to cyclonic separator, arrive powder shifter (machine having filled 60 order stainless steel meshs) and obtain Isphamycin 1214.8kg through sieving, its yield is 98.6%.
It is 85.8% that Isphamycin always extracts total recovery.
embodiment 2
Pre-treatment
Ferment of DM 50m
3, initially tire 25861u/ml.
First Aureomycin fermentation liquor is carried out acidifying, the sulphuric acid soln of 16% regulates pH to 0.7, secondly, adopts the ammonia soln of 16% to be adjusted to pH to 2.2 and 4.1 respectively; Leave standstill 23min, finally add tap water, the near 3643cps of fermentation broth viscosity.
Membrane filtration
Fermentation liquor pretreatment terminates, and filtrate is warming up to 63 DEG C, enters membrane filter plant, and use inorganic metal micropore microfiltration membrane, material is zirconium dioxide, and the support material of membrane filtration system is 316SS stainless steel.Filter type adopts high speed cross-current flow, membrane pore size 0.2um.In filtration procedure, pressure-controlling is at 2.5-3.5bar, and flow rate control is at 0.3 ~ 0.5m
3/ m
2.h.
Membrane filtration terminates, and filtrate volume is 48.8m
3, tire 28590u/ml, and yield is 107.9%.
Nanofiltration
Filtrate temperature controls at 32 DEG C, and in nanofiltration process, pressure-controlling is at 2-2.5MPa.The concentrated volume multiple of nanofiltration is 3.6 times.Nanofiltration terminates, and volume is 16.2m
3, tire 85260u/ml, and yield is 99%.
Crystallization
Filtrate temperature controls at 12 DEG C, and filtrate pH is adjusted to 6.2 by the ammoniacal liquor with 16%, adds 10.5m
3acetone, separates out solid-state duomycin crystal, and solid-liquid separation obtains solid-state duomycin 1262.4kg, and yield is 91.4%.
Washing
Add 2780L purified water in solid duomycin, stir duomycin mixing solutions 6min, then solid-liquid separation.Obtain solid duomycin 1185.4kg.
Salify
Start crystallizer whipping device, rotating speed controls at 22r/min, adds 10% technical hydrochloric acid, solution warms to 47 DEG C, regulates pH to 2.5, and insulation 52min, then solid-liquid separation, obtain Isphamycin 1214.5kg, yield is 95.2%.
Drip washing and drying
With purified water drip washing Isphamycin 2min, then use ethanol rinse 2min.Enable bipyramid and mix powder machine, regulate inlet temperature to 90 ~ 130 DEG C, temperature of outgoing air to 50 ~ 80 DEG C, add wet-milling in charging opening, after 8 ~ 12 order stainless steel meshs, with air-flow to cyclonic separator, arrive powder shifter (machine having filled 60 order stainless steel meshs) and obtain Isphamycin 1193.9kg through sieving, its yield is 98.3%.
It is 87.8% that Isphamycin always extracts total recovery.
embodiment 3
Pre-treatment
Ferment of DM 50m
3, initially tire 26024u/ml.
First Aureomycin fermentation liquor is carried out acidifying, the phosphoric acid solution of 17% regulates pH to 1.1, secondly, adopts the sodium hydroxide solution of 18% to be adjusted to pH to 2.3 and 4.3 respectively; Leave standstill 25min, finally add tap water, the near 3587cps of fermentation broth viscosity.
Membrane filtration
Fermentation liquor pretreatment terminates, and filtrate is warming up to 65 DEG C, enters membrane filter plant, and use inorganic metal micropore microfiltration membrane, material is zirconium dioxide, and the support material of membrane filtration system is 316SS stainless steel.Filter type adopts high speed cross-current flow, membrane pore size 0.3um.In filtration procedure, pressure-controlling is at 2.5-3.5bar, and flow rate control is at 0.3 ~ 0.5m
3/ m
2.h.
Membrane filtration terminates, and filtrate volume is 50.2m
3, tire 28098u/ml, and yield is 108.4%.
Nanofiltration
Filtrate temperature controls at 35 DEG C, and in nanofiltration process, pressure-controlling is at 2-2.5MPa.The concentrated volume multiple of nanofiltration is 3.8 times.Nanofiltration terminates, and volume is 13.3m
3, tire 104781u/ml, and yield is 98.8%.
Crystallization
Filtrate temperature controls at 15 DEG C, and filtrate pH is adjusted to 6.3 by the sodium hydroxide with 17%, adds 9.3m
3acetone, separates out solid-state duomycin crystal, and solid-liquid separation obtains solid-state duomycin 1282.1kg, and yield is 92%.
Washing
Add 3210L purified water in solid duomycin, stir duomycin mixing solutions 7min, then solid-liquid separation.Obtain solid duomycin 1212.9kg.
Salify
Start crystallizer whipping device, rotating speed controls at 25r/min, adds 12% technical hydrochloric acid, solution warms to 48 DEG C, regulates pH to 2.8, and insulation 55min, then solid-liquid separation, obtain Isphamycin 1260kg, yield is 96%.
Drip washing and drying
With purified water drip washing Isphamycin 3min, then use ethanol rinse 3min.Enable bipyramid and mix powder machine, regulate inlet temperature to 90 ~ 130 DEG C, temperature of outgoing air to 50 ~ 80 DEG C, add wet-milling in charging opening, after 8 ~ 12 order stainless steel meshs, with air-flow to cyclonic separator, arrive powder shifter (machine having filled 60 order stainless steel meshs) and obtain Isphamycin 1240kg through sieving, its yield is 98.4%.
It is 88.5% that Isphamycin always extracts total recovery.
embodiment 4
Pre-treatment
Ferment of DM 50m
3, initially tire 25734u/ml.
First Aureomycin fermentation liquor is carried out acidifying, the hydrochloric acid soln of 18% regulates pH to 1.3, secondly, adopts the ammonia soln of 19% to be adjusted to pH to 2.4 and 4.4 respectively; Leave standstill 28min, finally add tap water, the near 3325cps of fermentation broth viscosity.
Membrane filtration
Fermentation liquor pretreatment terminates, and filtrate is warming up to 68 DEG C, enters membrane filter plant, and use inorganic metal micropore microfiltration membrane, material is zirconium dioxide, and the support material of membrane filtration system is 316SS stainless steel.Filter type adopts high speed cross-current flow, membrane pore size 0.4um.In filtration procedure, pressure-controlling is at 2.5-3.5bar, and flow rate control is at 0.3 ~ 0.5m
3/ m
2.h.
Membrane filtration terminates, and filtrate volume is 52.3m
3, tire 26570u/ml, and yield is 108%.
Nanofiltration
Filtrate temperature controls at 38 DEG C, and in nanofiltration process, pressure-controlling is at 2-2.5MPa.The concentrated volume multiple of nanofiltration is 4.5 times.Nanofiltration terminates, and volume is 11.6m
3, tire 118117u/ml, and yield is 98.6%.
Crystallization
Filtrate temperature controls at 18 DEG C, and filtrate pH is adjusted to 6.4 by the ammoniacal liquor with 18%, adds 8.7m
3acetone, separates out solid-state duomycin crystal, and solid-liquid separation obtains solid-state duomycin 1264.6kg, and yield is 92.3%.
Washing
Add 3540L purified water in solid duomycin, stir duomycin mixing solutions 8min, then solid-liquid separation.Obtain solid duomycin 1198.8kg
Salify
Start crystallizer whipping device, rotating speed controls at 28r/min, adds 14% technical hydrochloric acid, solution warms to 49 DEG C, regulates pH to 3, and insulation 58min, then solid-liquid separation, obtain Isphamycin 1236kg, yield is 95.8%.
Drip washing and drying
With purified water drip washing Isphamycin 2min, then use ethanol rinse 2min.Enable bipyramid and mix powder machine, regulate inlet temperature to 90 ~ 130 DEG C, temperature of outgoing air to 50 ~ 80 DEG C, add wet-milling in charging opening, after 8 ~ 12 order stainless steel meshs, with air-flow to cyclonic separator, arrive powder shifter (machine having filled 60 order stainless steel meshs) and obtain Isphamycin 1215kg through sieving, its yield is 98.3%.
It is 87.7% that Isphamycin always extracts total recovery.
embodiment 5
Pre-treatment
Ferment of DM 50m
3, initially tire 24486u/ml.
First Aureomycin fermentation liquor is carried out acidifying, the sulphuric acid soln of 20% regulates pH to 1.5, secondly, adopts the sodium hydroxide solution of 20% to be adjusted to pH to 2.5 and 4.5 respectively; Leave standstill 30min, finally add tap water, the near 3073cps of fermentation broth viscosity.
Membrane filtration
Fermentation liquor pretreatment terminates, and filtrate is warming up to 70 DEG C, enters membrane filter plant, and use inorganic metal micropore microfiltration membrane, material is zirconium dioxide, and the support material of membrane filtration system is 316SS stainless steel.Filter type adopts high speed cross-current flow, membrane pore size 0.5um.In filtration procedure, pressure-controlling is at 2.5-3.5bar, and flow rate control is at 0.3 ~ 0.5m
3/ m
2.h.
Membrane filtration terminates, and filtrate volume is 56.7m
3, tire 23428u/ml, and yield is 108.5%.
Nanofiltration
Filtrate temperature controls at 40 DEG C, and in nanofiltration process, pressure-controlling is at 2-2.5MPa.The concentrated volume multiple of nanofiltration is 5 times.Nanofiltration terminates, and volume is 11.3m
3, tire 115674u/ml, and yield is 98.4%.
Crystallization
Filtrate temperature controls at 20 DEG C, and filtrate pH is adjusted to 6.5 by the sodium hydroxide with 20%, adds 9m
3acetone, separates out solid-state duomycin crystal, and solid-liquid separation obtains solid-state duomycin 1213kg, and yield is 92.8%.
Washing
Add 3630L purified water in solid duomycin, stir duomycin mixing solutions 10min, then solid-liquid separation.Obtain solid duomycin 1135kg.
Salify
Start crystallizer whipping device, rotating speed controls at 30r/min, adds 18% technical hydrochloric acid, solution warms to 50 DEG C, regulates pH to 3.3, and insulation 60min, then solid-liquid separation, obtain Isphamycin 1165kg, yield is 95.4%.
Drip washing and drying
With purified water drip washing Isphamycin 2min, then use ethanol rinse 3min.Enable bipyramid and mix powder machine, regulate inlet temperature to 90 ~ 130 DEG C, temperature of outgoing air to 50 ~ 80 DEG C, add wet-milling in charging opening, after 8 ~ 12 order stainless steel meshs, with air-flow to cyclonic separator, arrive powder shifter (machine having filled 60 order stainless steel meshs) and obtain Isphamycin 1147kg through sieving, its yield is 98.5%.
It is 87% that Isphamycin always extracts total recovery.
comparative example
Ferment of DM 50m
3, initially tire 25793u/ml.
The acidifying of 1 fermented liquid and filtration
Add appropriate oxalic acid, stir 10 minutes, then add concentrated hydrochloric acid, pH to 1.1, continue and stir 20 minutes.After acidifying, add by yellow prussiate of soda 125kg, zinc sulfate 100kg successively, stir 20 minutes.Plate-and-frame filter press press filtration, filtrate is back to filtrate tank, and controls filtrate temperature at 20 ~ 21 DEG C.Filtrate volume is 41m
3, tire 33562u/ml, for this operation yield answers 106.7%.
2 alkalization precipitations
Add magnesium chloride 110kg and calcium carbonate 120kg in filtrate successively, add continuous stirring and add 20% sodium hydroxide solution, regulate pH to 8.0, then stir 10 minutes, enter plate-and-frame filter press press filtration, charging is complete, to wash filter cake 20 minutes, then discharging.Filtrate volume is 43.8m
3, tire 28652u/ml, for this operation yield answers 91.2%.
3 coarse crystallization (abbreviation coarse-grain)
Add 1500L ethanol, then add the 200L concentrated hydrochloric acid of charging total hundred million, and be warming up to 50 DEG C of insulations 60 minutes.Insulation terminates, and material is thrown into plate-and-frame filter press press filtration, then uses 600L aqueous ethanolic solution (46 ~ 50 DEG C) top to wash, and end is washed on top, and obtain Isphamycin 1215kg, crystallization yield is 90%
4 are separated and drip washing
With purified water drip washing 5 minutes, with ethanol rinse 3 minutes.
5 dry mixed:
Starting outfit, carries out dry mixed, obtains Isphamycin 1085kg.
It is 78.2% that Isphamycin always extracts total recovery.
Claims (10)
1. the preparation method of an Isphamycin, it is characterized in that its processing step is: standing after first Aureomycin fermentation liquor being carried out acidifying, readjustment pH to 2 ~ 2.5, continuation leaves standstill and adds water after adjusting back pH to 4 ~ 4.5 and makes the pre-treatment of its viscosity drop to 3000 ~ 4000cps, obtains Isphamycin powder after then carrying out membrane filtration, nanofiltration, crystallization, washing, salify and drip washing and drying successively;
Described membrane filtration refers under 60 ~ 70 DEG C of conditions, and adopt high speed cross-current flow to carry out membrane filtration to pretreated duomycin filtrate, in filtration procedure, pressure-controlling is at 2.5-3.5bar, and flow rate control is at 0.3 ~ 0.5m
3/ m
2.h;
Described nanofiltration refers under 30 ~ 40 DEG C of conditions, carries out nanofiltration to the first filtrate after membrane filtration, and in nanofiltration process, pressure-controlling is at 2 ~ 2.5MPa, and the concentrated volume multiple of nanofiltration is 3 ~ 5 times;
Described crystallization refers at the temperature of 10 ~ 20 DEG C, with alkali lye, the pH of nanofiltration filtrate is adjusted to 6 ~ 6.5, then the acetone of 60 ~ 80% of filtrate volume is added, separate out solid-state duomycin crystal, leave standstill 10 ~ 20min, then solid-liquid separation obtains solid-state duomycin, and wherein said alkali lye is ammoniacal liquor or sodium hydroxide;
Described salify refers to and starts crystallizer whipping device, and rotating speed controls at 20 ~ 30r/min, adds 8 ~ 16% technical hydrochloric acids, solution warms to 45 ~ 50 DEG C, regulates pH to 2.3 ~ 3.3, and insulation 50 ~ 60min, then solid-liquid separation obtains Isphamycin.
2., according to the preparation method of Isphamycin according to claim 1, it is characterized in that described acidifying refers to that employing mass percent concentration is the acidic substance tune pH 0.5 ~ 1.5 of 15% ~ 20%, pH regulator speed is every 4 ~ 6min, and pH value changes 1 unit.
3., according to the preparation method of Isphamycin according to claim 2, it is characterized in that described acidic substance are hydrochloric acid, sulfuric acid or phosphoric acid.
4., according to the preparation method of Isphamycin according to claim 1, it is characterized in that described readjustment refers to that employing mass percent concentration is the alkaline matter tune pH of 15% ~ 20%, pH regulator speed is every 4 ~ 6min, and pH value changes 1 unit.
5., according to the preparation method of Isphamycin according to claim 1, it is characterized in that the described time left standstill for twice is 20 ~ 30min.
6. according to the preparation method of Isphamycin according to claim 1, it is characterized in that the filtering membrane that described membrane filtration adopts is inorganic metal micropore microfiltration membrane, membrane pore size 0.1 ~ 0.5 μm, material is zirconium dioxide, and the support material of membrane filtration system is 316SS stainless steel.
7., according to the preparation method of Isphamycin according to claim 1, it is characterized in that described nanofiltration membrane module used is can block molecular weight to be less than the hollow-fibre membrane that 1000 are greater than the material of 100, material is mixed type composite nanometer filtering film.
8. according to the preparation method of Isphamycin according to claim 1, it is characterized in that described washing adds purified water in the solid-state duomycin pointing to described crystallization gained, solid-liquid separation after abundant stirring 5 ~ 10min, wash 2 ~ 3 times, the ratio of adding water is 2 ~ 3L/kg.
9., according to the preparation method of Isphamycin according to claim 1, it is characterized in that described drip washing refers to and use ethanol rinse 2 ~ 3min again with after purified water drip washing 3 ~ 5min.
10. according to the preparation method of Isphamycin according to claim 1, it is characterized in that described drying refers to that enabling bipyramid mixes powder machine, regulate inlet temperature to 90 ~ 130 DEG C, temperature of outgoing air to 50 ~ 80 DEG C, add wet-milling in charging opening, after 8 ~ 12 order stainless steel meshs, with air-flow to cyclonic separator, arrive powder shifter and obtain Isphamycin through sieving.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1132124A (en) * | 1966-04-28 | 1968-10-30 | Krka Tovarna Zdravil | Process for the isolation of tetracycline antibiotics from impure solutions thereof |
| CN101863797A (en) * | 2010-07-07 | 2010-10-20 | 福建省福抗药业股份有限公司 | New process for preparing chlortetracycline hydrochloride |
| CN102898326A (en) * | 2012-10-31 | 2013-01-30 | 金河生物科技股份有限公司 | Preparation method of chlortetracycline hydrochloride |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1132124A (en) * | 1966-04-28 | 1968-10-30 | Krka Tovarna Zdravil | Process for the isolation of tetracycline antibiotics from impure solutions thereof |
| CN101863797A (en) * | 2010-07-07 | 2010-10-20 | 福建省福抗药业股份有限公司 | New process for preparing chlortetracycline hydrochloride |
| CN102898326A (en) * | 2012-10-31 | 2013-01-30 | 金河生物科技股份有限公司 | Preparation method of chlortetracycline hydrochloride |
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