CN106173271A - A kind of tylosin phosphonate pre-mixing agent preparation method - Google Patents
A kind of tylosin phosphonate pre-mixing agent preparation method Download PDFInfo
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- CN106173271A CN106173271A CN201610694201.5A CN201610694201A CN106173271A CN 106173271 A CN106173271 A CN 106173271A CN 201610694201 A CN201610694201 A CN 201610694201A CN 106173271 A CN106173271 A CN 106173271A
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- tylosin
- phosphonate
- mixing agent
- tylosin phosphonate
- mixing
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P60/00—Technologies relating to agriculture, livestock or agroalimentary industries
- Y02P60/80—Food processing, e.g. use of renewable energies or variable speed drives in handling, conveying or stacking
- Y02P60/87—Re-use of by-products of food processing for fodder production
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Abstract
The present invention relates to antibiotic medicine preparation field, disclose a kind of tylosin phosphonate pre-mixing agent preparation method, pass through optimization order, directly with tylosin phosphonate fermentation liquid as initial feed, after extraction concentrates, prepare tylosin phosphonate pre-mixing agent, during decrease decolouring and wait the technique not affecting end product quality, simplify conventional production process, shorten the production cycle, reduce the loss of tylosin active unit, reduce production cost；Preparation method through appropriate design, tylosin phosphonate pre-mixing agent is directly prepared with tylosin phosphonate concentrated solution, being spray-dried or crystallize refinement in minimizing common process and prepare tylosin phosphonate, then re-dissolved tylosin phosphonate finished product goes to prepare the step of pre-mixing agent.Not only operate simplification, and decrease unnecessary energy consumption waste.
Description
Technical field
The present invention relates to antibiotic medicine preparation field, particularly a kind of tylosin phosphonate pre-mixing agent preparation method.
Background technology
Tylosin (Tylosin, TYL), has another name called safe Lip river mycin, tylosin, mainly by Tylosin A (tylosin),
Desmycosin B(desmycosin), Macrocin C (macrocin) and thunder Lip river rhzomorph D(relomycin) composition.Its
In, only component A has the highest antibacterial activity in vivo, so component A content its antibacterial effect the highest is the best.Tylosin energy
Effectively prevent mycoplasma disease, bacterial disease, spirillum class disease and coccidiosis, also poultry are had somatotrophic work simultaneously
With, the utilization in cultivation of this antibiotic is more and more universal.Major product has tylosin alkali, tylosin phosphate and Tai Le
Rhzomorph tartrate.Tylosin phosphonate typically adds in the middle of animal feed with the form of pre-mixing agent, prevents Animal diseases.
But, tylosin phosphonate is a kind of extremely unstable antibiotic, after tylosin phosphonate production, also can
Experience a considerably long period and just can be made into pre-mixing agent.But the most not only effective ingredient reduce and also quality also can not get protect
Card.Therefore, it is necessary to improve and improve the preparation method of tylosin phosphonate pre-mixing agent.
Summary of the invention
The purpose of invention is to provide a kind of tylosin phosphonate pre-mixing agent preparation method, optimization technological process, reduces anti-
Answer step, decrease Tylosin A loss in preparation process, it is ensured that product quality and active constituent content simultaneously.
For realizing above-mentioned technical purpose, reach above-mentioned technique effect, the invention discloses a kind of tylosin phosphonate premix
The preparation method of agent, comprises the steps that
Pretreatment: add flocculant or filter aid in the tylosin broth obtained by fermentation, stir 30-60 minute；
Filter: the tylosin broth after pre-treatment step is carried out filter pressing or squeezing, control filter pressing or squeeze pressure is
1.0-5.0MPa, obtains filtrate and is tylosin filtrate；
Purification: use ultrafiltration membrance filter tylosin filtrate, removes the soluble impurity of macromole in filtrate；
Concentrate: use NF membrane that the filtrate after ultrafiltration is concentrated, remove micromolecular compound；
Extraction and back extraction: with butyl acetate, filtrate is sent into static mixer and mixes, send into centrifuge after mixing,
Add phosphoric acid standing separation, collect lower floor's aqueous phase；
Reconcentration: use NF membrane that aqueous phase is concentrated, remove moisture removal, it is thus achieved that tylosin phosphonate concentrated solution；
Mixing: be sprayed at uniformly on adjuvant by tylosin phosphonate concentrated solution, is stirred for after adding adhesive, highly basic regulation pH
Uniformly, prepared moisture weight is than the tylosin phosphonate pre-mixing agent wet product at 30%-60%, standby；
Pelletize: by wet method extruding granulator or oscillating granulator pelletize；
It is dried: tylosin phosphonate pre-mixing agent wet product granule is through fluid bed airpillow-dry, and wherein wet feed airpillow-dry condition is temperature
Spend≤100 DEG C, time≤2.0 hour.
Sub-sieve: the tylosin phosphonate pre-mixing agent upper strata obtained be No. two sieve lower floors be No. seven sieve vibration sub-sieves, obtain
The granule between 24-120 mesh, be tylosin phosphonate pre-mixing agent finished product.
Wherein, in pre-treatment step, flocculant is aluminum sulfate, polyaluminium sulfate or aluminum chloride, aluminium polychlorid, addition
Account for the 0.4-1.5% of tylosin phosphonate fermentating liquid volume；Filter aid is kieselguhr, and addition accounts for tylosin phosphonate fermentation liquid
The 0-10% of volume total amount.
Preferably, extraction and back extraction are embodied as step for by filtrate: the flow of butyl acetate volume ratio=1:1-4, logical
Crossing liquid caustic soda regulation pH is 9.0-12.0, enters static mixer mixing, and temperature controls at 35-45 DEG C；Send into after mixing from
Scheming is centrifuged, and retains organic facies, removes aqueous phase；Organic facies adds concentration 2.0-10% phosphoric acid solution and adjusts pH to 2.0-5.0, stir
Mix 5-30 minute, stand layering in 10-60 minute, collect lower floor's aqueous phase；
Wherein, in blend step, adjuvant is plant amylum, peanut cake powder, analysis for soybean powder, soybean cake powder, maize cob meal, zeolite, Margarita
The mixture of one or more in rock, calcium carbonate or rice chaff powder, fineness requirement is 80 mesh；Adhesive is PVP, dextrin, methylol
In sodium cellulosate, sodium carboxymethyl cellulose, carboxymethylstach sodium or hydroxypropylcellulose, the mixture of one or more, accounts for pre-mixing agent total
Part by weight is 0.5-5%；Highly basic be potassium hydroxide, sodium hydroxide, disodium hydrogen phosphate, dipotassium hydrogen phosphate, sodium phosphate, potassium phosphate,
The mixture of one or more in sodium carbonate or potassium carbonate, the pH of regulation is between 6.5-7.5.
The method have the advantages that
1. the present invention passes through optimization order, directly with tylosin phosphonate fermentation liquid as initial feed, prepares after extraction concentrates
Tylosin phosphonate pre-mixing agent, during decrease decolouring and wait and do not affect the technique of end product quality, simplify conventional production
Technique, shortens the production cycle, reduces the loss of tylosin active unit, reduces production cost.
2., through the preparation side of appropriate design, directly prepare tylosin phosphonate premix with tylosin phosphonate concentrated solution
Agent, is spray-dried or crystallizes refinement in minimizing common process and prepare tylosin phosphonate, and then re-dissolved tylosin phosphonate becomes
Product go to prepare the step of pre-mixing agent.Not only operate simplification, and decrease unnecessary energy consumption waste.
3. in the application as a example by the 1000kg tylosin phosphonate pre-mixing agent that preparation specification is 10%, if using common process
Production need to consume tylosin phosphonate 110-130kg, needs tylosin broth 9.5-11m3, and the present invention directly uses and sends out
The concentrated solution that ferment liquid is purified, concentration etc. is made substitutes initiation material, it is only necessary to equal potency unit tylosin 8.5-10m3,
Cost declines more than 5%.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the present invention.
Detailed description of the invention
In order to make the purpose of the present invention, technical scheme and advantage clearer, below in conjunction with drawings and Examples, right
The present invention is further elaborated.
Embodiment 1
As it is shown in figure 1, the invention discloses a kind of tylosin phosphonate pre-mixing agent preparation method:
Tylosin broth volume 10m3, titer 12386U/mL, total hundred million is 123.9.Add the 20-22% prepared and be polymerized chlorine
Changing aluminum solutions, final addition is by the 0.6%(w/v with fermentating liquid volume), stir 50 minutes.With flame filter press to fermentation liquid
Filtering, controlling filter pressing/squeeze pressure is 3.0MPa, obtains filtrate, be tylosin filtrate after filter pressing, and volume is 8m3,
Titer is 14432U/mL.
Use ultrafiltration membrance filter tylosin filtrate, remove the soluble impurity that filtrate middle-molecular-weihydroxyethyl is bigger, enter back into and receive
Filter membrane concentrates, and concentrated solution volume is 4m3.By filtrate: the flow of butyl acetate volume ratio=1:1, liquid adjusting PH with base is 9.0-
11.0, enter static mixer, temperature controls at 40-42 DEG C.Subsequently into centrifuge, retain organic facies, remove aqueous phase；
Organic facies adds concentration 6% phosphoric acid solution and adjusts pH to 3.0, stir 10 minutes, stand layering in 40 minutes, collect lower floor's aqueous phase, body
Amass as 2m3, titer is 56728U/mL.Use NF membrane that lower floor's aqueous phase is concentrated, mainly remove moisture removal etc., it is thus achieved that phosphorus
Acid tylosin concentrated solution, volume is 0.5m3, concentrated solution titer is 225964U/mL.
Intend producing 1000kg according to tylosin phosphonate pre-mixing agent product specification (%).Happy to prepare the phosphoric acid Thailand of 10% specification
As a example by rhzomorph pre-mixing agent.Above-mentioned tylosin phosphonate concentrated solution is sprayed at corn starch uniformly, and adjuvant fineness requirement is 80
Mesh, the gross weight of adjuvant is 1000kg.Adding dextrin, accounting for pre-mixing agent gross weight ratio is 1.0%.Again with 30% (W/V) phosphoric acid hydrogen
Two sodium solution 30L, the pH of regulation tylosin phosphonate pre-mixing agent, recording tylosin phosphonate pre-mixing agent wet product pH is 7.2.Stirring
Uniform tylosin phosphonate pre-mixing agent wet product moisture content is 47%.By this wet product after extruding granulator is pelletized, through boiling
Rising dry, wet feed airpillow-dry condition is temperature 80 DEG C, 2.0 hours time, obtains tylosin phosphonate pre-mixing agent semi-finished product.With
Upper strata be No. two sieve lower floors be No. seven sieve vibration sub-sieve tylosin phosphonate pre-mixing agent semi-finished product, obtain between 24-120 mesh it
Between granule, be tylosin phosphonate pre-mixing agent finished product, granulating rate is 91%.
Embodiment 2
As it is shown in figure 1, the invention discloses a kind of tylosin phosphonate pre-mixing agent preparation method:
Tylosin broth volume 9.5m3, titer 13194U/mL, total hundred million is 126.9.Add the 20-22% polymerization prepared
Liquor alumini chloridi, final addition is by the 0.6%(w/v with fermentating liquid volume), stir 40 minutes.With flame filter press to fermentation
Liquid filters, and controlling filter pressing/squeeze pressure is 4.0MPa, obtains filtrate, be tylosin filtrate after filter pressing, and volume is
8m3, titer is 14895 U/mL.
Use ultrafiltration membrance filter tylosin filtrate, remove the soluble impurity that filtrate middle-molecular-weihydroxyethyl is bigger, enter back into and receive
Filter membrane concentrates, and concentrated solution volume is 3.5m3.By filtrate: the flow of butyl acetate volume ratio=1:2, liquid adjusting PH with base is 9.0-
11.0, enter static mixer, temperature controls at 40-42 DEG C.Subsequently into centrifuge, retain organic facies, remove aqueous phase；
Organic facies adds concentration 5% phosphoric acid solution and adjusts pH to 3.5, stir 20 minutes, stand layering in 50 minutes, collect lower floor's aqueous phase, body
Amass as 2m3, titer is 58316U/mL.Use NF membrane that lower floor's aqueous phase is concentrated mutually, mainly remove moisture removal etc., it is thus achieved that
Tylosin phosphonate concentrated solution, volume is 0.5m3, concentrated solution titer is 232478U/mL.
According to tylosin phosphonate pre-mixing agent product specification (%), intend producing 1000kg.Safe to prepare the phosphoric acid of 10% specification
As a example by happy rhzomorph pre-mixing agent.Above-mentioned tylosin phosphonate concentrated solution is sprayed at soybean cake powder uniformly, and adjuvant fineness requirement is
80 mesh, the gross weight of adjuvant is 1000kg.Adding Carboxymethyl cellulose sodium, accounting for pre-mixing agent gross weight ratio is 2%.Again with 15%
(W/V) potassium phosphate solution 30L, the pH of regulation tylosin phosphonate pre-mixing agent, recording tylosin phosphonate pre-mixing agent wet product pH is
7.4.The tylosin phosphonate pre-mixing agent wet product moisture content stirred is 46%.By this wet product through extruding granulator system
After Li, through airpillow-dry, wet feed airpillow-dry condition is temperature 85 DEG C, 1.5 hours time, obtains tylosin phosphonate pre-mixing agent
Semi-finished product.With upper strata be No. two sieve lower floors be No. seven sieve vibration sub-sieve tylosin phosphonate pre-mixing agent semi-finished product, obtain between
Granule between 24-120 mesh, is tylosin phosphonate pre-mixing agent finished product, and granulating rate is 92%.
Embodiment 3
As it is shown in figure 1, the invention discloses a kind of tylosin phosphonate pre-mixing agent preparation method:
Tylosin broth volume 9.0m3, titer 13688U/mL, total hundred million is 126.9.Add the 20-22% polymerization prepared
Liquor alumini chloridi, final addition is by the 0.6%(w/v with fermentating liquid volume), stir 40 minutes.With flame filter press to fermentation
Liquid filters, and controlling filter pressing/squeeze pressure is 4.0MPa, obtains filtrate, be tylosin filtrate after filter pressing, and volume is
7.5m3, titer is 15793 U/mL.
Use ultrafiltration membrance filter tylosin filtrate, remove the soluble impurity that filtrate middle-molecular-weihydroxyethyl is bigger, enter back into and receive
Filter membrane concentrates, and concentrated solution volume is 3.5m3.By filtrate: the flow of butyl acetate volume ratio=1:3, liquid adjusting PH with base is 9.0-
11.0, enter static mixer, temperature controls at 40-42 DEG C.Subsequently into centrifuge, retain organic facies, remove aqueous phase；
Organic facies adds concentration 4% phosphoric acid solution and adjusts pH to 4.0, stir 30 minutes, stand layering in 60 minutes, collect lower floor's aqueous phase, body
Amass as 2m3, titer is 58464U/mL.Use NF membrane that lower floor's aqueous phase is concentrated mutually, mainly remove moisture removal etc., it is thus achieved that
Tylosin phosphonate concentrated solution, volume is 0.5m3, concentrated solution titer is 230368U/mL.
Intend producing 1000kg according to tylosin phosphonate pre-mixing agent product specification (%).Happy to prepare the phosphoric acid Thailand of 10% specification
As a example by rhzomorph pre-mixing agent.Above-mentioned tylosin phosphonate concentrated solution is sprayed on maize cob meal uniformly, and adjuvant fineness requirement is
80 mesh, the gross weight of adjuvant is 1000kg.Adding PVP, accounting for pre-mixing agent gross weight ratio is 0.5%.Again with 15% (W/V) potassium carbonate
Solution 35L, the pH of regulation tylosin phosphonate pre-mixing agent, recording tylosin phosphonate pre-mixing agent wet product pH is 7.5.Stir
Tylosin phosphonate pre-mixing agent wet product moisture content be 48%.By this wet product after extruding granulator is pelletized, dry through boiling
Dry, wet feed airpillow-dry condition is temperature 90 DEG C, 1 hour time, obtains tylosin phosphonate pre-mixing agent semi-finished product.With upper strata it is
No. two sieve lower floors be No. seven sieve vibration sub-sieve tylosin phosphonate pre-mixing agent semi-finished product, obtain between 24-120 mesh
Grain, is tylosin phosphonate pre-mixing agent finished product, and granulating rate is 93%.
The above, the only present invention preferably detailed description of the invention, but protection scope of the present invention is not limited thereto,
Any those familiar with the art in the technical scope that the invention discloses, the change that can readily occur in or replacement,
All should contain within protection scope of the present invention.
Claims (4)
1. a tylosin phosphonate pre-mixing agent preparation method, it is characterised in that comprise the steps that
Pretreatment: add flocculant or filter aid in the tylosin broth obtained by fermentation, stir 30-60 minute；
Filter: the tylosin broth after pre-treatment step is carried out filter pressing or squeezing, control filter pressing or squeeze pressure is
1.0-5.0MPa, obtains filtrate and is tylosin filtrate；
Purification: use ultrafiltration membrance filter tylosin filtrate, removes the soluble impurity of macromole in filtrate；
Concentrate: use NF membrane that the filtrate after ultrafiltration is concentrated, remove micromolecular compound；
Extraction and back extraction: with butyl acetate, filtrate is sent into static mixer and mixes, send into centrifuge after mixing,
Add phosphoric acid standing separation, collect lower floor's aqueous phase；
Reconcentration: use NF membrane that aqueous phase is concentrated, remove moisture removal, it is thus achieved that tylosin phosphonate concentrated solution；
Mixing: be sprayed at uniformly on adjuvant by tylosin phosphonate concentrated solution, is stirred for after adding adhesive, highly basic regulation pH
Uniformly, prepared moisture weight is than the tylosin phosphonate pre-mixing agent wet product at 30%-60%, standby；
Pelletize: by wet method extruding granulator or oscillating granulator pelletize；
It is dried: tylosin phosphonate pre-mixing agent wet product granule is through fluid bed airpillow-dry, and wherein wet feed airpillow-dry condition is temperature
Spend≤100 DEG C, time≤2.0 hour；
Sub-sieve: the tylosin phosphonate pre-mixing agent upper strata obtained be No. two sieve lower floors be No. seven sieve vibration sub-sieves, Jie obtained
Granule between 24-120 mesh, is tylosin phosphonate pre-mixing agent finished product.
2. a kind of tylosin phosphonate pre-mixing agent preparation method as claimed in claim 1, it is characterised in that: described pretreatment
In step, flocculant is aluminum sulfate, polyaluminium sulfate or aluminum chloride, aluminium polychlorid, and addition accounts for tylosin phosphonate fermentation liquid
The 0.4-1.5% of volume；Filter aid is kieselguhr, and addition accounts for the 0-10% of tylosin phosphonate fermentating liquid volume total amount.
3. tylosin phosphonate pre-mixing agent preparation method as claimed in claim 1 a kind of, it is characterised in that: described extraction and
Back extraction is embodied as step for by filtrate: the flow of butyl acetate volume ratio=1:1-4, is 9.0-by liquid caustic soda regulation pH
12.0, enter static mixer mixing, temperature controls at 35-45 DEG C；Send into centrifuge after mixing, retain organic
Phase, removes aqueous phase；Organic facies adds concentration 2.0-10% phosphoric acid solution and adjusts pH to 2.0-5.0, stir 5-30 minute, stand 10-
Layering in 60 minutes, collects lower floor's aqueous phase.
4. a kind of tylosin phosphonate pre-mixing agent preparation method as claimed in claim 3, it is characterised in that: described mixing step
In rapid, adjuvant is plant amylum, peanut cake powder, analysis for soybean powder, soybean cake powder, maize cob meal, zeolite, perlite, calcium carbonate or rice chaff
The mixture of one or more in powder, fineness requirement is 80 mesh；Described adhesive is PVP, dextrin, Carboxymethyl cellulose sodium,
The mixture of one or more in sodium carboxymethyl cellulose, carboxymethylstach sodium or hydroxypropylcellulose, accounts for pre-mixing agent gross weight ratio
For 0.5-5%；Described highly basic is potassium hydroxide, sodium hydroxide, disodium hydrogen phosphate, dipotassium hydrogen phosphate, sodium phosphate, potassium phosphate, carbon
The mixture of one or more in acid sodium or potassium carbonate, the pH of regulation is between 6.5-7.5.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106800593A (en) * | 2017-01-09 | 2017-06-06 | 博瑞生物医药泰兴市有限公司 | A kind of method for purifying anidulafungin precursor compound |
| CN107441050A (en) * | 2017-08-29 | 2017-12-08 | 湖北龙翔药业科技股份有限公司 | A kind of preparation method of valnemulin hydrochloride premix |
| CN108329370A (en) * | 2018-04-19 | 2018-07-27 | 齐鲁制药（内蒙古）有限公司 | A kind of preparation method of tartaric acid/Tylosin phosphate |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106800593A (en) * | 2017-01-09 | 2017-06-06 | 博瑞生物医药泰兴市有限公司 | A kind of method for purifying anidulafungin precursor compound |
| CN106800593B (en) * | 2017-01-09 | 2021-04-27 | 博瑞生物医药泰兴市有限公司 | Method for purifying anidulafungin precursor compound |
| CN107441050A (en) * | 2017-08-29 | 2017-12-08 | 湖北龙翔药业科技股份有限公司 | A kind of preparation method of valnemulin hydrochloride premix |
| CN108329370A (en) * | 2018-04-19 | 2018-07-27 | 齐鲁制药（内蒙古）有限公司 | A kind of preparation method of tartaric acid/Tylosin phosphate |
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Application publication date: 20161207 |