CN102584920A - Culture medium for fermenting and producing tylosin with streptomyces fradiae, and fermentation method - Google Patents
Culture medium for fermenting and producing tylosin with streptomyces fradiae, and fermentation method Download PDFInfo
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Abstract
The invention relates to a compound menstruum for extracting tylosin and an extraction method. According to the invention, the compound menstruum formed by mixing butyl acetate, isobutyl acetate and butanol according to the volume ratio of 6:3 to 3.2 to 0.8-1 is used for extracting tylosin in fermentation filtrate through a secondary counter-current extraction method. The method has the advantages of low consumption of organic menstruum, low loss of tylosin, short extraction time, high extraction yield and the like.
Description
Technical field
The invention belongs to biological medicine extractive technique field, particularly relate to a kind of tylosin extraction solvent and process for extracting.
Background technology
Tylosin is claimed Desmycosin again, is a kind of macrolide antibiotics that is obtained through fermented extracted by the actinomyces streptomyces fradiae, and tylosin alkali, phosphoric acid salt and three kinds of forms of tartrate are arranged.Tylosin is a stud bird, poultry special-purpose efficient, the antibiotic growth-promoting agent of noresidue.Diseases such as chicken septicemia, the popular pneumonia of pig there is unique curative effect, and the growth of fowl, poultry is had obvious facilitation.Tylosin has avoided the shared microbiotic of people and animals to be prone to produce the problem of cross resistance as the animal specific microbiotic, is used to prevent and treat pig, fowl mycoplasmosis.
At present, domestic tylosin extraction process mainly is with the at first pre-treatment of tylosin fermented liquid, through solid-liquid separation, obtains ferment filtrate; Secondly ferment filtrate is extracted with organic solvent, tylosin gets into ester phase liquid, and ester phase liquid is taked the reextraction method, and through acidification, tylosin gets into water; Last tylosin water liquid obtains Webel Tylan Premix or tylosin tartrate through processes such as neutralization, decolouring, filtration and spraying dryings.
Usually adopt ETHYLE ACETATE or butylacetate (hereinafter to be referred as BA) in the said extracted method as extraction agent.ETHYLE ACETATE is a kind of typical extraction solvent commonly used, has excellent dissolving power.Tylosin alkali is water insoluble, is soluble in ETHYLE ACETATE.But there is very big deficiency in ETHYLE ACETATE: the solubleness under the normal temperature in water is 8.08% of massfraction, and standing storage or use are prone to decompose, and hydrolysate is acetate and ethanol.Be applied to tylosin and extract that loss reaches 20～40% in the industry.At present, the enterprise of domestic production tylosin has stopped using ETHYLE ACETATE.
Butylacetate (BA) possesses the dissolving power same with ETHYLE ACETATE, but it is water insoluble, is a kind of good extraction solvent difficult the decomposition.At present, most of enterprise of domestic production tylosin all selects BA as the organic solvent that extracts tylosin.But from fermented liquid, extract tylosin with BA, its weak point is: first: the BA price is high, consumption is big.One ton of tylosin filtrating needs 0.3～0.6 ton of BA.Because BA has volatile character, loss through volatilization accounts for 1～1.5% of BA sum in every batch of use; The BA recovery generally is controlled at 80～90%.Calculate the enterprise that produces 1000 tons of tylosins per year by this, the loss of 1 year BA is more than at least 1,300 ten thousand yuan.Second: the extracting power of BA is limited.Tylosin was filtrated into behind the secondary counter-current extraction, total twice extraction yield is controlled at 85～95%, tiring generally at 500～1000u/ml of aqueous phase tylosin is discharged with waste water in addition.Calculate by this, produce the enterprise of 1000 tons of tylosins per year, annual tylosin with discharge of wastewater loses up to more than 1,000 ten thousand yuan.
Summary of the invention
The object of the invention just is to overcome that tylosin filtrating extraction yield is low, the organic solvent consumption is many, the tylosin loss big and the extraction process time such as grows at technological deficiency; Provide a kind of tylosin to extract double solvent; Utilize this compound molten magnesium can effectively improve the extraction yield; Shorten the extraction time, reduce the loss of organic solvent and tylosin simultaneously to greatest extent, realize that tylosin is stable, produce efficiently.
Another object of the present invention provides a kind of extraction tylosin process for extracting.
For realizing that the technical scheme that above-mentioned purpose is taked is:
A kind of tylosin extracts double solvent, it is characterized in that it being to be mixed by butylacetate, isobutyl acetate and the butanols volume ratio according to 6:3～3.2:0.8～1;
A kind of tylosin process for extracting is characterized in that adopting double solvent and tylosin filtrating under 40～50 ℃, to carry out the secondary counter-current extraction, filtrating: double solvent=10 ︰ 2.5～2.8 (V/V); In extraction process, take a sample to check double solvent mutually and the aqueous phase separation situation, tire and aqueous pH values; Strict control extraction liquid one-level pH 7.0～10.0, secondary pH is 8.0～11.0; The control raffinate is tired at 300 μ/below the ml, collects the double solvent extraction liquid; Emulsion possibly appear in extraction process, can suitably add to be no more than 4L/m
3Emulsion splitter (X 2073), can reduce emulsification.
Tylosin after the extraction carries out acidifying under pH2～5 conditions strips, after neutralization, decolouring, filtration and spraying drying obtain Webel Tylan Premix or tylosin tartrate.
Discover that isobutyl acetate and BA are similar, and be water insoluble, also difficult the decomposition, and can dissolve each other with the BA arbitrary proportion.Add suitable propyl alcohol and help to strengthen the solvability of isopropyl acetate and BA, improve its extracting power.
The present invention processes the tylosin in the double solvent extractive fermentation filtrating with butylacetate, isobutyl acetate and butanols according to certain proportion compatibility, has the effect that consumption is little, extraction efficiency is high.Specifically, its advantage is mainly reflected in the following aspects:
1 reduces the organic solvent consumption: extract 60m
3Tylosin filtrating needs butylacetate 19.2m at least
3Use double solvent, need 16.8m at most
3, reduce more than 15.6% with the contrast of the consumption of butylacetate; Reduce the influence of organic solvent to environment.
2 reduce the loss of tylosins: after using BA extraction tylosin, and the tiring generally of water at 500～1000u/ml, behind double solvent extraction tylosin, tiring＜300u/ml of water reduces the tylosin loss more than 20%.
3 reduce the extraction time: extract 80m with BA
3Tylosin filtrating, consuming time generally at 6h; Consuming time with double solvent generally at 3～4 hours, reduce the time spent more than 30%.
4 extraction yields are high: adopt the secondary counter-current extraction, the average yield of BA extraction tylosin is 90%; The average yield of double solvent extraction tylosin is 96%; The extraction average yield improves more than 6%.
Embodiment
With instance the present invention is described below, it should be understood that instance is to be used to explain the present invention rather than limitation of the present invention.Scope of the present invention and core content are confirmed according to claims.
Embodiment 1 usefulness butylacetate extracts tylosin from ferment filtrate
Secondary counter-current extraction: tylosin ferment filtrate 60m
3, tiring is 13523u/ml.Organic solvent acetic acid butyl ester 18m
3Open whizzer, treat that rotating speed and electric current are normal after, open each material pipe valve, opening conduits well heater steam valve heats material simultaneously, the fermented liquid temperature that makes the entering whizzer is at 44 ℃.In extraction process, take a sample to check double solvent mutually and the aqueous phase separation situation, tire and aqueous pH values, extraction liquid one-level pH 7.0～10.0, secondary pH is 8.0～11.0.After extraction finished, the water volume was 58m
3, tiring is 748u/ml.The butylacetate volume is 17.1m
3, tiring is 41898u/ml.Time spent 4.1h.The extraction yield is 88.3%.
Strip: extraction liquid is squeezed in the jar of stripping, be cooled to 8 ℃, adding concentration is 3.2% phosphoric acid solution.Control phosphoric acid solution flow is so that aqueous pH values reaches 4.5, and stirs 15min, standing demix, tell anti-stripping agent after, the one-level anti-stripping agent is transferred to neutralization tank further neutralizes.Add concentration and be 6.5% phosphoric acid solution, control phosphoric acid solution flow is so that aqueous pH values to 2.3, and stirs 15min, standing demix, tell anti-stripping agent after, the secondary anti-stripping agent is transferred to neutralization tank merges the one-level anti-stripping agent and further neutralize.Strip after the end, the detection double solvent is tired and is 412u/ml.
Neutralization, decolouring, filtration and spraying drying: with the calcium hydroxide suspension of purified water preparation 21%.Under agitation slowly add the calcium hydroxide suspension, the each 40min at interval of hydro-oxidation calcium time, the pH value transfers to and added gac 42kg at 6.5 o'clock, stirs 15min, adds super-cell 40kg again, continues to stir 15min.Advance flame filter press and begin to filter, collect filtrating.Refined liquid behind the Plate Filtration contains some small-particle impurity, uses earlier Plate Filtration, carries out the smart filtration of secondary with microfiltration membrane again, and filtration medium is 5um, 0.3um filter membrane.Refined liquid after the smart filter is carried out next step spraying drying.Spraying drying is to utilize high pressure reciprocating pump will concentrate feed liquid to be sprayed into fine mist, and the dry-heat air that blasts at the drying tower top is with the droplet wink-dry, and the waste gas body is discharged outside the tower body, and dry back powder is deposited to the bottom and collects, and obtains the tylosin phosphate powder.
Embodiment 2 usefulness double solvents extract tylosin from ferment filtrate
Secondary counter-current extraction: tylosin ferment filtrate 60m
3, tiring is 13416u/ml.Double solvent 15m
3(butylacetate 9.1 m
3, isobutyl acetate 4.65m
3, butanols 1.2m
3).Open whizzer, treat that rotating speed and electric current are normal after, open each material pipe valve, opening conduits well heater steam valve heats material simultaneously, the fermented liquid temperature that makes the entering whizzer is at 40 ℃.In extraction process, take a sample to check double solvent mutually and the aqueous phase separation situation, tire and aqueous pH values, extraction liquid one-level pH 7.0～10.0, secondary pH is 8.0～11.0.After extraction finished, the water volume was 57m
3, tiring is 286u/ml.Double solvent is long-pending to be 14.6m
3, tiring is 52542u/ml.Extraction time spent 3.1h.The extraction yield is 95.3%.
Strip: extraction liquid is squeezed in the jar of stripping, be cooled to 7 ℃, adding concentration is 3.8% phosphoric acid solution.Control phosphoric acid solution flow is so that aqueous pH values reaches 4.2, and stirs 14min, standing demix, tell anti-stripping agent after, the one-level anti-stripping agent is transferred to neutralization tank further neutralizes.Add concentration and be 6.2% phosphoric acid solution, control phosphoric acid solution flow is so that aqueous pH values to 2.1, and stirs 13min, standing demix, tell anti-stripping agent after, the secondary anti-stripping agent is transferred to neutralization tank merges the one-level anti-stripping agent and further neutralize.Strip after the end, the detection double solvent is tired and is 407u/ml.
Neutralization, decolouring, filtration and spraying drying: with the calcium hydroxide suspension of purified water preparation 24%.Under agitation slowly add the calcium hydroxide suspension, the each 45min at interval of hydro-oxidation calcium time, the pH value transfers to and added gac 41.3kg at 6.2 o'clock, stirs 12min, adds super-cell 40.5kg again, continues to stir 15min.Advance flame filter press and begin to filter, collect filtrating.Refined liquid behind the Plate Filtration contains some small-particle impurity, uses earlier Plate Filtration, carries out the smart filtration of secondary with microfiltration membrane again, and filtration medium is 5um, 0.3um filter membrane.Refined liquid after the smart filter is carried out next step spraying drying.Spraying drying is to utilize high pressure reciprocating pump will concentrate feed liquid to be sprayed into fine mist, and the dry-heat air that blasts at the drying tower top is with the droplet wink-dry, and the waste gas body is discharged outside the tower body, and dry back powder is deposited to the bottom and collects, and obtains the tylosin phosphate powder.
Embodiment 3 usefulness double solvents extract tylosin from ferment filtrate
Tylosin ferment filtrate 60m
3, tiring is 13462u/ml.Emulsion appears in fermented liquid, adds emulsion splitter X 2073 204L.Add double solvent 15.6m
3(butylacetate 9.4 m
3, isobutyl acetate 4.8m
3, butanols 1.4m
3).Open whizzer, treat that rotating speed and electric current are normal after, open each material pipe valve, opening conduits well heater steam valve heats material simultaneously, the fermented liquid temperature that makes the entering whizzer is at 45 ℃.In extraction process, take a sample to check double solvent mutually and the aqueous phase separation situation, tire and aqueous pH values, extraction liquid one-level pH 7.0～10.0, secondary pH is 8.0～11.0.After extraction finished, the water volume was 57m
3, tiring is 272u/ml.Double solvent is long-pending to be 15.2m
3, tiring is 50748u/ml.Extraction time spent 3h.The extraction yield is 95.5%.Extraction liquid is squeezed in the jar of stripping, be cooled to 8 ℃, adding concentration is 3.2% phosphoric acid solution.Control phosphoric acid solution flow is so that aqueous pH values reaches 4.5, and stirs 15min, standing demix, tell anti-stripping agent after, the one-level anti-stripping agent is transferred to neutralization tank further neutralizes.Add concentration and be 6.5% phosphoric acid solution, control phosphoric acid solution flow is so that aqueous pH values to 2.3, and stirs 15min, standing demix, tell anti-stripping agent after, the secondary anti-stripping agent is transferred to neutralization tank merges the one-level anti-stripping agent and further neutralize.Strip after the end, the detection double solvent is tired and is 412u/ml.Calcium hydroxide suspension with purified water preparation 21%.Under agitation slowly add the calcium hydroxide suspension, the each 40min at interval of hydro-oxidation calcium time, the pH value transfers to and added gac 42kg at 6.5 o'clock, stirs 15min, adds super-cell 40kg again, continues to stir 15min.Advance flame filter press and begin to filter, collect filtrating.Refined liquid behind the Plate Filtration contains some small-particle impurity, uses earlier Plate Filtration, carries out the smart filtration of secondary with microfiltration membrane again, and filtration medium is 5um, 0.3um filter membrane.Refined liquid after the smart filter is carried out next step spraying drying.Spraying drying is to utilize high pressure reciprocating pump will concentrate feed liquid to be sprayed into fine mist, and the dry-heat air that blasts at the drying tower top is with the droplet wink-dry, and the waste gas body is discharged outside the tower body, and dry back powder is deposited to the bottom and collects, and obtains the tylosin phosphate powder.
Embodiment 4 usefulness double solvents extract tylosin from ferment filtrate
Secondary counter-current extraction: tylosin ferment filtrate 60m
3, tiring is 13417u/ml.Double solvent 16.2m
3(butylacetate 9.5 m
3, isobutyl acetate 4.9m
3, butanols 1.6m
3).Open whizzer, treat that rotating speed and electric current are normal after, open each material pipe valve, opening conduits well heater steam valve heats material simultaneously, the fermented liquid temperature that makes the entering whizzer is at 46 ℃.In extraction process, take a sample to check double solvent mutually and the aqueous phase separation situation, tire and aqueous pH values, extraction liquid one-level pH 7.0～10.0, secondary pH is 8.0～11.0.After extraction finished, the water volume was 57m
3, tiring is 254u/ml.Double solvent is long-pending to be 16m
3, tiring is 48402u/ml.Extraction time spent 2.9h.The extraction yield is 96.2%.
Strip: extraction liquid is squeezed in the jar of stripping, be cooled to 6 ℃, adding concentration is 3.6% phosphoric acid solution.Control phosphoric acid solution flow is so that aqueous pH values reaches 4.4, and stirs 13min, standing demix, tell anti-stripping agent after, the one-level anti-stripping agent is transferred to neutralization tank further neutralizes.Add concentration and be 6.6% phosphoric acid solution, control phosphoric acid solution flow is so that aqueous pH values to 2.9, and stirs 15min, standing demix, tell anti-stripping agent after, the secondary anti-stripping agent is transferred to neutralization tank merges the one-level anti-stripping agent and further neutralize.Strip after the end, the detection double solvent is tired and is 389u/ml.
Neutralization, decolouring, filtration and spraying drying: with the calcium hydroxide suspension of purified water preparation 26%.Under agitation slowly add the calcium hydroxide suspension, the each 44min at interval of hydro-oxidation calcium time, the pH value transfers to and added gac 42.3kg at 6.0 o'clock, stirs 15min, adds super-cell 40.4kg again, continues to stir 15min.Advance flame filter press and begin to filter, collect filtrating.Refined liquid behind the Plate Filtration contains some small-particle impurity, uses earlier Plate Filtration, carries out the smart filtration of secondary with microfiltration membrane again, and filtration medium is 5um, 0.3um filter membrane.Refined liquid after the smart filter is carried out next step spraying drying.Spraying drying is to utilize high pressure reciprocating pump will concentrate feed liquid to be sprayed into fine mist, and the dry-heat air that blasts at the drying tower top is with the droplet wink-dry, and the waste gas body is discharged outside the tower body, and dry back powder is deposited to the bottom and collects, and obtains the tylosin phosphate powder.
Embodiment 5 usefulness double solvents extract tylosin from ferment filtrate
Secondary counter-current extraction: tylosin ferment filtrate 60m
3, tiring is 13504u/ml.Double solvent 16.8m
3(butylacetate 9.9m
3, isobutyl acetate 5.2m
3, butanols 1.7m
3).Open whizzer, treat that rotating speed and electric current are normal after, open each material pipe valve, opening conduits well heater steam valve heats material simultaneously, the fermented liquid temperature that makes the entering whizzer is at 45 ℃.In extraction process, take a sample to check double solvent mutually and the aqueous phase separation situation, tire and aqueous pH values, extraction liquid one-level pH 7.0～10.0, secondary pH is 8.0～11.0.After extraction finished, the water volume was 57m
3, tiring is 251u/ml.Double solvent is long-pending to be 16.4m
3, tiring is 47527u/ml.Extraction time spent 2.9h.The extraction yield is 96.2%.
Strip: extraction liquid is squeezed in the jar of stripping, be cooled to 7 ℃, adding concentration is 4.1% phosphoric acid solution.Control phosphoric acid solution flow is so that aqueous pH values reaches 4.5, and stirs 15min, standing demix, tell anti-stripping agent after, the one-level anti-stripping agent is transferred to neutralization tank further neutralizes.Add concentration and be 6.9% phosphoric acid solution, control phosphoric acid solution flow is so that aqueous pH values to 2.7, and stirs 15min, standing demix, tell anti-stripping agent after, the secondary anti-stripping agent is transferred to neutralization tank merges the one-level anti-stripping agent and further neutralize.Strip after the end, the detection double solvent is tired and is 392u/ml.
Neutralization, decolouring, filtration and spraying drying: with the calcium hydroxide suspension of purified water preparation 25%.Under agitation slowly add the calcium hydroxide suspension, the each 45min at interval of hydro-oxidation calcium time, the pH value transfers to and added gac 42.5kg at 6.2 o'clock, stirs 15min, adds super-cell 40.3kg again, continues to stir 15min.Advance flame filter press and begin to filter, collect filtrating.Refined liquid behind the Plate Filtration contains some small-particle impurity, uses earlier Plate Filtration, carries out the smart filtration of secondary with microfiltration membrane again, and filtration medium is 5um, 0.3um filter membrane.Refined liquid after the smart filter is carried out next step spraying drying.Spraying drying is to utilize high pressure reciprocating pump will concentrate feed liquid to be sprayed into fine mist, and the dry-heat air that blasts at the drying tower top is with the droplet wink-dry, and the waste gas body is discharged outside the tower body, and dry back powder is deposited to the bottom and collects, and obtains the tylosin phosphate powder.
Embodiment 6 usefulness double solvents extract tylosin from ferment filtrate
Secondary counter-current extraction: tylosin ferment filtrate 60m
3, tiring is 13487u/ml.Emulsion appears in fermented liquid, adds emulsion splitter X 2073 186L, double solvent 16.2m
3(butylacetate 9.6m
3, isobutyl acetate 5m
3, butanols 1.6m
3).Open whizzer, treat that rotating speed and electric current are normal after, open each material pipe valve, opening conduits well heater steam valve heats material simultaneously, the fermented liquid temperature that makes the entering whizzer is at 45 ℃.In extraction process, take a sample to check double solvent mutually and the aqueous phase separation situation, tire and aqueous pH values, extraction liquid one-level pH 7.0～10.0, secondary pH is 8.0～11.0.After extraction finished, the water volume was 57m
3, tiring is 264u/ml.Double solvent is long-pending to be 15.9m
3, tiring is 48960u/ml.Extraction time spent 2.9h.The extraction yield is 96.2%.
Strip: extraction liquid is squeezed in the jar of stripping, be cooled to 7 ℃, adding concentration is 4.3% phosphoric acid solution.Control phosphoric acid solution flow is so that aqueous pH values reaches 4.6, and stirs 12min, standing demix, tell anti-stripping agent after, the one-level anti-stripping agent is transferred to neutralization tank further neutralizes.Add concentration and be 6.7% phosphoric acid solution, control phosphoric acid solution flow is so that aqueous pH values to 1.9, and stirs 15min, standing demix, tell anti-stripping agent after, the secondary anti-stripping agent is transferred to neutralization tank merges the one-level anti-stripping agent and further neutralize.Strip after the end, the detection double solvent is tired and is 396u/ml.
Neutralization, decolouring, filtration and spraying drying: with the calcium hydroxide suspension of purified water preparation 26%.Under agitation slowly add the calcium hydroxide suspension, the each 50min at interval of hydro-oxidation calcium time, the pH value transfers to and added gac 42.2kg at 6.1 o'clock, stirs 15min, adds super-cell 40.2kg again, continues to stir 15min.Advance flame filter press and begin to filter, collect filtrating.Refined liquid behind the Plate Filtration contains some small-particle impurity, uses earlier Plate Filtration, carries out the smart filtration of secondary with microfiltration membrane again, and filtration medium is 5um, 0.3um filter membrane.Refined liquid after the smart filter is carried out next step spraying drying.Spraying drying is to utilize high pressure reciprocating pump will concentrate feed liquid to be sprayed into fine mist, and the dry-heat air that blasts at the drying tower top is with the droplet wink-dry, and the waste gas body is discharged outside the tower body, and dry back powder is deposited to the bottom and collects, and obtains the tylosin phosphate powder.
Embodiment 7 usefulness double solvents extract tylosin from ferment filtrate
Secondary counter-current extraction: tylosin ferment filtrate 60m
3, tiring is 13461u/ml.Double solvent 16.2m
3(butylacetate 9.6m
3, isobutyl acetate 5m
3, butanols 1.6m
3).Open whizzer, treat that rotating speed and electric current are normal after, open each material pipe valve, opening conduits well heater steam valve heats material simultaneously, the fermented liquid temperature that makes the entering whizzer is at 47 ℃.In extraction process, take a sample to check double solvent mutually and the aqueous phase separation situation, tire and aqueous pH values, extraction liquid one-level pH 7.0～10.0, secondary pH is 8.0～11.0.After extraction finished, the water volume was 57m
3, tiring is 273u/ml.Double solvent is long-pending to be 15.8m
3, tiring is 49211u/ml.Extraction time spent 2.9h.The extraction yield is 96.3%.
Strip: extraction liquid is squeezed in the jar of stripping, be cooled to 5 ℃, adding concentration is 3.9% phosphoric acid solution.Control phosphoric acid solution flow is so that aqueous pH values reaches 4.0, and stirs 15min, standing demix, tell anti-stripping agent after, the one-level anti-stripping agent is transferred to neutralization tank further neutralizes.Add concentration and be 6.7% phosphoric acid solution, control phosphoric acid solution flow is so that aqueous pH values to 2.6, and stirs 10min, standing demix, tell anti-stripping agent after, the secondary anti-stripping agent is transferred to neutralization tank merges the one-level anti-stripping agent and further neutralize.Strip after the end, the detection double solvent is tired and is 402u/ml.
Neutralization, decolouring, filtration and spraying drying: with the calcium hydroxide suspension of purified water preparation 26%.Under agitation slowly add the calcium hydroxide suspension, the each 43min at interval of hydro-oxidation calcium time, the pH value transfers to and added gac 42.1kg at 6.2 o'clock, stirs 13min, adds super-cell 40.1kg again, continues to stir 15min.Advance flame filter press and begin to filter, collect filtrating.Refined liquid behind the Plate Filtration contains some small-particle impurity, uses earlier Plate Filtration, carries out the smart filtration of secondary with microfiltration membrane again, and filtration medium is 5um, 0.3um filter membrane.Refined liquid after the smart filter is carried out next step spraying drying.Spraying drying is to utilize high pressure reciprocating pump will concentrate feed liquid to be sprayed into fine mist, and the dry-heat air that blasts at the drying tower top is with the droplet wink-dry, and the waste gas body is discharged outside the tower body, and dry back powder is deposited to the bottom and collects, and obtains the tylosin phosphate powder.
Embodiment 8 usefulness double solvents extract tylosin from ferment filtrate
Secondary counter-current extraction: tylosin ferment filtrate 60m
3, tiring is 13521u/ml.Double solvent 16.2m
3(butylacetate 9.6m
3, isobutyl acetate 5m
3, butanols 1.6m
3).Open whizzer, treat that rotating speed and electric current are normal after, open each material pipe valve, opening conduits well heater steam valve heats material simultaneously, the fermented liquid temperature that makes the entering whizzer is at 50 ℃.In extraction process, take a sample to check double solvent mutually and the aqueous phase separation situation, tire and aqueous pH values, extraction liquid one-level pH 7.0～10.0, secondary pH is 8.0～11.0.After extraction finished, the water volume was 57m
3, tiring is 237u/ml.Double solvent is long-pending to be 15.8m
3, tiring is 47854u/ml.Extraction time spent 3h.The extraction yield is 93.2%.
Strip: extraction liquid is squeezed in the jar of stripping, be cooled to 6 ℃, adding concentration is 4.2% phosphoric acid solution.Control phosphoric acid solution flow is so that aqueous pH values reaches 4.8, and stirs 12min, standing demix, tell anti-stripping agent after, the one-level anti-stripping agent is transferred to neutralization tank further neutralizes.Add concentration and be 6.6% phosphoric acid solution, control phosphoric acid solution flow is so that aqueous pH values to 2.3, and stirs 14min, standing demix, tell anti-stripping agent after, the secondary anti-stripping agent is transferred to neutralization tank merges the one-level anti-stripping agent and further neutralize.Strip after the end, the detection double solvent is tired and is 387u/ml.
Neutralization, decolouring, filtration and spraying drying: with the calcium hydroxide suspension of purified water preparation 22%.Under agitation slowly add the calcium hydroxide suspension, the each 45min at interval of hydro-oxidation calcium time, the pH value transfers to and added gac 43.1kg at 6.2 o'clock, stirs 15min, adds super-cell 41.3kg again, continues to stir 13min.Advance flame filter press and begin to filter, collect filtrating.Refined liquid behind the Plate Filtration contains some small-particle impurity, uses earlier Plate Filtration, carries out the smart filtration of secondary with microfiltration membrane again, and filtration medium is 5um, 0.3um filter membrane.Refined liquid after the smart filter is carried out next step spraying drying.Spraying drying is to utilize high pressure reciprocating pump will concentrate feed liquid to be sprayed into fine mist, and the dry-heat air that blasts at the drying tower top is with the droplet wink-dry, and the waste gas body is discharged outside the tower body, and dry back powder is deposited to the bottom and collects, and obtains the tylosin phosphate powder.
Claims (5)
1. a tylosin extracts double solvent, it is characterized in that it being to be mixed by butylacetate, isobutyl acetate and the butanols volume ratio according to 6:3～3.2:0.8～1.
2. tylosin process for extracting; It is characterized in that adopting double solvent and tylosin filtrating under 40～50 ℃, to carry out the secondary counter-current extraction; Control one-level pH7.0～10.0; Secondary pH8.0～11.0, wherein tylosin filtrating and double solvent are according to the volume ratio compatibility of 10:2.5～2.8.
3. according to the described tylosin process for extracting of claim 2, it is characterized in that: in secondary counter-current extraction process, add emulsion splitter, add-on is no more than 4L/m
3
4. according to the described tylosin process for extracting of claim 3, it is characterized in that: said emulsion splitter is an X 2073.
5. according to the described tylosin process for extracting of claim 2, it is characterized in that: the tylosin after the extraction carries out acidifying under pH2～5 conditions strips, after neutralization, decolouring, filtration and spraying drying obtain Webel Tylan Premix or tylosin tartrate.
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| CN2012100183357A CN102584920A (en) | 2012-01-20 | 2012-01-20 | Culture medium for fermenting and producing tylosin with streptomyces fradiae, and fermentation method |
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| CN (1) | CN102584920A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102899374A (en) * | 2012-11-14 | 2013-01-30 | 宁夏泰瑞制药股份有限公司 | Cleaner production method of tylosin |
| CN103074402A (en) * | 2013-02-05 | 2013-05-01 | 宁夏泰瑞制药股份有限公司 | Culture medium for producing tylosin through fermentation of streptomyces fradiae and fermentation method |
| CN106148229A (en) * | 2016-07-08 | 2016-11-23 | 金正大生态工程集团股份有限公司 | A kind of streptomyces fradiae solid medium, cultural method and the preparation method of agricultural microbial agent |
| CN115403643A (en) * | 2021-05-28 | 2022-11-29 | 宁夏泰益欣生物科技有限公司 | Purification method of tylosin |
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| CN1224021A (en) * | 1998-01-22 | 1999-07-28 | 清华大学 | Extracting and purifying of antibiotics using naphthenic acid extractive system |
| CN101565439A (en) * | 2008-04-21 | 2009-10-28 | 王玉万 | Improved extraction method for tylosin |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN87102137A (en) * | 1986-03-21 | 1987-11-04 | 伊莱利利公司 | The improvement relating to antibiotic-producing microorganisms |
| CN1224021A (en) * | 1998-01-22 | 1999-07-28 | 清华大学 | Extracting and purifying of antibiotics using naphthenic acid extractive system |
| CN101565439A (en) * | 2008-04-21 | 2009-10-28 | 王玉万 | Improved extraction method for tylosin |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102899374A (en) * | 2012-11-14 | 2013-01-30 | 宁夏泰瑞制药股份有限公司 | Cleaner production method of tylosin |
| CN103074402A (en) * | 2013-02-05 | 2013-05-01 | 宁夏泰瑞制药股份有限公司 | Culture medium for producing tylosin through fermentation of streptomyces fradiae and fermentation method |
| CN103074402B (en) * | 2013-02-05 | 2014-12-10 | 宁夏泰瑞制药股份有限公司 | Culture medium for producing tylosin through fermentation of streptomyces fradiae and fermentation method |
| CN106148229A (en) * | 2016-07-08 | 2016-11-23 | 金正大生态工程集团股份有限公司 | A kind of streptomyces fradiae solid medium, cultural method and the preparation method of agricultural microbial agent |
| CN106148229B (en) * | 2016-07-08 | 2020-01-10 | 金正大生态工程集团股份有限公司 | Streptomyces fradiae solid culture medium, culture method and preparation method of agricultural microbial agent |
| CN115403643A (en) * | 2021-05-28 | 2022-11-29 | 宁夏泰益欣生物科技有限公司 | Purification method of tylosin |
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Application publication date: 20120718 |