CN104621156B - A kind of preparation method of polyoxin pre-mixing agent - Google Patents
A kind of preparation method of polyoxin pre-mixing agent Download PDFInfo
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- CN104621156B CN104621156B CN201510044283.4A CN201510044283A CN104621156B CN 104621156 B CN104621156 B CN 104621156B CN 201510044283 A CN201510044283 A CN 201510044283A CN 104621156 B CN104621156 B CN 104621156B
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/12—Powders or granules
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
- A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
- A01N47/10—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof
- A01N47/12—Carbamic acid derivatives, i.e. containing the group —O—CO—N<; Thio analogues thereof containing a —O—CO—N< group, or a thio analogue thereof, neither directly attached to a ring nor the nitrogen atom being a member of a heterocyclic ring
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Abstract
The invention discloses a kind of preparation method of many antibiotic pre-mixing agents, step is：The many antibiotic zymotic fluids for fermenting are heated to into 60～70 DEG C, maintain 5～10min, cooling, and with acid for adjusting pH to 2.5～5.0, add stabilizer, auxiliary agent, zymotic fluid is carried out into plate-frame filtering after being sufficiently stirred for, obtain many antibiotic wet cakes, then filter cake is carried out expansion drying, is crushed, addition auxiliary material dilution is obtained many antibiotic pre-mixing agents.Simple, low cost of the invention, much stability of the antibiotic pre-mixing agent finished product during storage is significantly improved for institute so as to convenient in storage, transport and application process, stably.
Description
Technical field：
The present invention relates to a kind of preparation method of polyoxin pre-mixing agent, more particularly to a kind of system of polyoxin pre-mixing agent
Preparation Method.
Background technology：
Polyoxin (Polyoxins) also known as Polyoxin, multi-effect mycin, are that one kind is produced with modern biotechnology
Peptide pyridimine nucleosides broad spectrum agricultural antibiotic.There are polyoxin absorbability and therapeutic action and the target organismses of height to select
Property, which can exclusively act on the Common mycotic disease of various crop.It is to mastigomycetes, ascus that polyoxin is most prominent
25 kinds of fungal diseases such as bacterium, half bacterium have stronger inhibitory action.Research shows, the total A to N of multi-effect mycin this 14
Plant into and be grouped into, since 1967, multi-effect mycin is widely used for treating rice sheath blight disease, tomato as disinfectant use in agriculture
The fungal diseases of plants such as gray mold and Pear black spot.
Polyoxin for fungi and insect cell wall it is chitinous synthesis have good inhibiting effect, in view of crops and
There is no chitin in vivo in mammal etc., so multi-effect mycin has non-target organism safety to vertebrate and mammal
Property, while the pathogenic cell Candida albicans also to causing mucous membrane and systemic infection has good inhibiting effect.Polyoxin
With natural adaptability and compatibility preferably, degraded after administration quickly, it is noresidue, pollution-free, there is no cross resistance and steady
Qualitative strong the advantages of, it has also become one of first-line drug of domestic biological pesticide.
In China's pesticide market, multi-effect mycin preparation formulation is varied, wherein have 1.5%, 2%, 3%, 10% it is wettable
Property pulvis, 1%, 3% aqua and 32% active compound etc., but this kind of formulation all exist storage during stability reduce and transport
Inconvenient the shortcomings of.
The content of the invention：
The present invention is for the not strong problem of polyoxin finished product stability, there is provided a kind of simple, low cost, gained
The preparation method of the polyoxin pre-mixing agent that product stability is significantly improved.
The technical scheme is that：A kind of preparation method of polyoxin pre-mixing agent, which comprises the following steps that：
(1) pre-process：The polyoxin zymotic fluid for fermenting is heated to into 60～70 DEG C, maintains 5～10min, cooling to use
Acid for adjusting pH adds stabilizer and auxiliary agent to 2.5～5.0；
(2) press filtration：Step (1) pretreated polyoxin zymotic fluid is carried out into plate compression, polyoxin is obtained wet
Filter cake；
(3) expansion drying is crushed：The wet cake that step (2) is obtained is carried out into expansion drying, control EAT for 110～
130 DEG C, 60～70 DEG C of leaving air temp, 80～100 DEG C of temperature of charge obtain polyoxin mycelium dry product after being dried；
(4) prepared by pre-mixing agent：Content is required according to polyoxin mycelium dry product purity and finished product, addition powdery is carried
Body, is well mixed, and obtains powdery polyoxin pre-mixing agent；
(5) granulate：Powdery polyoxin pre-mixing agent obtained by step (4) is carried out dry granulation and sieved, is obtained
Granular polyoxin pre-mixing agent.
The fermentation titer of the polyoxin zymotic fluid for fermenting described in preferred steps (1) is 2000～2500 μ g/mL.
" a kind of streptomycete and many antibiotic metabolic regulations fermentation work that fermentation used medium and condition of culture are submitted in this seminar
Skill " (ZL201210056364.2) in disclosed.Concrete scheme is：1.5～5.5g/L of dusty yeast, 10～25g/ of corn flour
L, 15～30g/L of soybean cake powder, 15～35g/L of glucose, 5～10g/L of sodium chloride, 10～15g/L of calcium carbonate, dipotassium hydrogen phosphate
2～4g/L, 5～15g/L of soya-bean oil, 0.2～0.8g/L of inorganic salts, pH value are maintained at 6.0～7.2, control tank pressure and temperature, fermentation
After carrying out 55～65 hours, fed-batch fermentation is carried out using the method for stream plus glucose, concentration of glucose in sweat is made
80～120g/L is maintained at, 90～120h of fermented and cultured obtains zymotic fluid, and zymotic fluid fermentation titer is 2000～2500 μ g/mL.Send out
Bacterial classification used by ferment is the golden streptomyces chromogenes (Streptomyces aureochromogenes) of autonomous screening
NJYHWG66382CGMCC No.5756, in Patent No. ZL201210056364.2, it is entitled " a kind of streptomycete and
Preservation is carried out in the patent of invention of many antibiotic metabolic regulation techniques ", depositary institution is managed for Chinese microorganism strain preservation
Committee's common micro-organisms center, preservation date are on 2 14th, 2012, and the patent has carried out public affairs on 22nd in August in 2012
Open, CGMCC No.5756 bacterial classifications used are disclosed.
It is hydrochloric acid, sulfuric acid, phosphoric acid, citric acid, oxalic acid or glycine that the acid used by pH value is adjusted in preferred steps (1)；Institute
The stabilizer stated is copper sulphate, aluminium chloride, aluminum sulfate or iron chloride；The addition of stabilizer be zymotic fluid quality 1.5～
2.5%；Described auxiliary agent is Toween80, sorbester p18 or polysorbate 60；The addition of auxiliary agent be zymotic fluid quality 0.2～
0.4%.
The pressure of the plate compression described in preferred steps (2) is 1.0～5.0MPa, and time of filter pressing is 1～2h.It is preferred that walking
Suddenly the polyoxin wet cake described in (2) is 30～40% containing water quality.
Powder carrier described in preferred steps (4) is powdered rice hulls, calcium carbonate, perlite, any one in zeolite powder；Powdery
The granularity of carrier is 80～100 mesh；The addition of powder carrier for powdery polyoxin pre-mixing agent quality 55%～81%.It is excellent
20～100 mesh sieves are crossed after selecting step (5) dry granulation.
Beneficial effect：
1. the present invention is pre-processed to the zymotic fluid of polyoxin, so as to change the quality of polyoxin pre-mixing agent finished product
Significantly reduce polyoxin palliating degradation degree, greatly improve the stability of polyoxin pre-mixing agent finished product.
2. the present invention adopts the methods such as plate-frame filtering, expansion drying, granulation to prepare the new technology of polyoxin pre-mixing agent, many
The granulating rate and yield of antimycin pre-mixing agent is greatly improved, and cost is reduced, and makes the product better adapt to the market demand.
3. gained polyoxin pre-mixing agent titer plateaus improve so as to transport, storage and application process in more
It is convenient, stable.
Specific embodiment：
With reference to embodiment, the present invention will be further elaborated, the description below merely to explain the present invention, and
Its content is not defined.
In following embodiments, zymotic fluid used is with golden streptomyces chromogenes (Streptomyces
Aureochromogenes) as a example by the zymotic fluid of NJYHWG66382CGMCC No.5756 fermentations gained, after the completion of fermentation, stop
Stirring and temperature control, zymotic fluid fermentation titer are 2000～2500 μ g/mL.Concrete fermentation used medium and condition of culture are according to this
Seminar submit to " a kind of streptomycete and many antibiotic metabolic regulation zymotechniques " (ZL201210056364.2) in carry out.
Embodiment 1：
(1) pre-process：Take the polyoxin zymotic fluid 1000L zymotic fluids (fermentation titer is 2140 μ g/mL) for fermenting to add
Heat maintains 5min, cooling with salt acid for adjusting pH to 2.5, to add the copper sulphate for accounting for zymotic fluid quality 1.5% as steady to 60 DEG C
Agent, zymotic fluid quality 0.2%Toween80 are determined as auxiliary agent.
(2) press filtration：Step (1) pretreated polyoxin zymotic fluid is carried out into plate compression, controlling press filtration pressure is
1.0MPa, time of filter pressing are 2h, obtain the polyoxin wet cake 174kg containing water quality 30%.
(3) expansion drying is crushed：The wet cake that step (2) is obtained is carried out into expansion drying, EAT is controlled for 110
DEG C, 65 DEG C of leaving air temp, 85 DEG C of temperature of charge obtain polyoxin mycelium dry product 52.2kg after being dried.After testing much
In antimycin mycelium dry product, the weight percentage of polyoxin is 4.1%.
(4) prepared by pre-mixing agent：Add the powdered rice hulls of 215.3kg in the dry product obtained in step (3), be well mixed,
Obtain the powdery polyoxin pre-mixing agent that 267.5kg polyoxin mass contents are 0.8%.
(5) granulate：Powdery polyoxin pre-mixing agent obtained by step (4) is carried out into dry granulation, 60 mesh sieves are finally crossed,
Granularity is obtained for 60 mesh sieve polyoxin pre-mixing agent granules.
0.8% obtained polyoxin pre-mixing agent is than the granulating rate and output increased obtained by conventional method about after testing
15%, stability improves about 9%.
Embodiment 2：
(1) pre-process：Take polyoxin zymotic fluid 1000L (fermentation titer is 2340 μ g/mL) the temperature heating for fermenting
To 65 DEG C, 7min, cooling is maintained with phosphorus acid for adjusting pH to 3.0, to add the aluminum sulfate for accounting for zymotic fluid quality 2.0% as stable
Agent, 0.25% sorbester p18 of zymotic fluid quality are used as auxiliary agent.
(2) press filtration：Step (1) pretreated polyoxin zymotic fluid is carried out into plate compression, controlling press filtration pressure is
2.0MPa, time of filter pressing are 1.5h, are obtained containing 34% polyoxin wet cake 156kg of water quality.
(3) expansion drying is crushed：The wet cake that step (2) is obtained is carried out into expansion drying, EAT is controlled for 120
DEG C, 70 DEG C of leaving air temp, 95 DEG C of temperature of charge obtain polyoxin mycelium dry product 52kg after being dried.Much resist after testing
In mycin mycelium dry product, the weight percentage of polyoxin is 4.5%.
(4) prepared by pre-mixing agent：Add the calcium carbonate of 104kg in the dry product obtained in step (3), be well mixed, obtain
To the powdery polyoxin pre-mixing agent that 156kg polyoxin mass contents are 1.5%.
(5) granulate：Powdery polyoxin pre-mixing agent obtained by step (4) is carried out into dry granulation, 80 mesh sieves are finally crossed,
Granularity is obtained for 80 mesh sieve polyoxin pre-mixing agent granules.
1.5% obtained polyoxin pre-mixing agent is than the granulating rate and output increased obtained by conventional method about after testing
10%, stability improves about 15%.
Embodiment 3：
(1) pre-process：Take polyoxin zymotic fluid 1000L (fermentation titer is 2250 μ g/mL) the temperature heating for fermenting
To 70 DEG C, 10min, cooling is maintained with lemon acid for adjusting pH to 4.0, to add the aluminium chloride of zymotic fluid quality 3.0% as stable
Agent, 0.3% polysorbate 60 of zymotic fluid quality are used as auxiliary agent.
(2) press filtration：Step (1) pretreated polyoxin zymotic fluid is carried out into plate compression, controlling press filtration pressure is
4.5MPa, time of filter pressing are 2h, are obtained containing 40% polyoxin wet cake 125kg of water quality.
(3) expansion drying is crushed：The wet cake that step (2) is obtained is carried out into expansion drying, EAT is controlled for 130
DEG C, 60 DEG C of leaving air temp, 100 DEG C of temperature of charge obtain polyoxin mycelium dry product 50kg after being dried.Much resist after testing
In mycin mycelium dry product, the weight percentage of polyoxin is 4.5%.
(4) prepared by pre-mixing agent：Add the perlite of 62.5kg in the dry product obtained in step (3), be well mixed, obtain
To the powdery polyoxin pre-mixing agent that 112.5kg polyoxin mass contents are 2.0%.
(5) granulate：Powdery polyoxin pre-mixing agent obtained by step (4) is carried out into dry granulation, 100 mesh are finally crossed
Sieve, obtains granularity for 100 mesh sieve polyoxin pre-mixing agent granules.
2.0% obtained polyoxin pre-mixing agent is than the granulating rate and output increased obtained by conventional method about after testing
20%, stability improves about 10%.
Claims (8)
1. a kind of preparation method of polyoxin pre-mixing agent, which comprises the following steps that：
(1) pre-process：The polyoxin zymotic fluid for fermenting is heated to into 60～70 DEG C, 5～10min, cooling, with acid tune is maintained
Section pH to 2.5～5.0, adds stabilizer and auxiliary agent；
(2) press filtration：Step (1) pretreated many antibiotic zymotic fluids are carried out into plate compression, polyoxin wet cake is obtained；
(3) expansion drying is crushed：The wet cake that step (2) is obtained is carried out into expansion drying, EAT is controlled for 110～130
DEG C, 60～70 DEG C of leaving air temp, 80～100 DEG C of temperature of charge obtain polyoxin mycelium dry product after being dried；
(4) prepared by pre-mixing agent：Content is required according to finished product, is added powder carrier, is well mixed, obtain powdery polyoxin premix
Agent；
(5) granulate：The many antibiotic pre-mixing agents of powdery obtained by step (4) are carried out dry granulation and sieved, graininess is obtained
Polyoxin pre-mixing agent.
2. preparation method according to claim 1, it is characterised in that the polyoxin for fermenting described in step (1) is sent out
The fermentation titer of zymotic fluid is 2000～2500 μ g/mL.
3. preparation method according to claim 1, is characterized in that：It is hydrochloric acid, sulphur that the acid used by pH value is adjusted in step (1)
Acid, phosphoric acid, citric acid, oxalic acid or glycine.
4. preparation method according to claim 1, is characterized in that：Stabilizer described in step (1) is copper sulphate, chlorination
Aluminium, aluminum sulfate or iron chloride；The addition of stabilizer is zymotic fluid quality 1.5～2.5%；Described auxiliary agent be Toween80,
Sorbester p18 or polysorbate 60；The addition of auxiliary agent is zymotic fluid quality 0.2～0.4%.
5. preparation method according to claim 1, it is characterised in that the pressure of the plate compression described in step (2) is
1.0～5.0MPa, time of filter pressing are 1～2h.
6. preparation method according to claim 1, is characterized in that：Polyoxin wet cake described in step (2) contains
Water quality is 30～40%.
7. preparation method according to claim 1, is characterized in that：Powder carrier described in step (4) is powdered rice hulls, carbonic acid
Any one in calcium, perlite, zeolite powder；The granularity of powder carrier is 80～100 mesh；The addition of powder carrier is that powdery is more
The 55%～81% of antimycin pre-mixing agent quality.
8. preparation method according to claim 1, it is characterised in that 20～100 mesh sieves are crossed after step (5) dry granulation.
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| CN201510044283.4A CN104621156B (en) | 2015-01-28 | 2015-01-28 | A kind of preparation method of polyoxin pre-mixing agent |
| PCT/CN2015/092826 WO2016119491A1 (en) | 2015-01-28 | 2015-10-26 | Preparation method of multi-antibiotics premix |
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| CN201510044283.4A CN104621156B (en) | 2015-01-28 | 2015-01-28 | A kind of preparation method of polyoxin pre-mixing agent |
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| CN104621156B (en) * | 2015-01-28 | 2017-04-05 | 南京工业大学 | A kind of preparation method of polyoxin pre-mixing agent |
| CN110483617A (en) * | 2019-09-17 | 2019-11-22 | 陕西绿盾环境工程研究院有限公司 | A kind of preparation method of high-content polyoxin original powder |
| CN110592159B (en) * | 2019-09-23 | 2021-04-09 | 浙江拜克生物科技有限公司 | Preparation process and device of monensin premix |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102424636A (en) * | 2011-09-27 | 2012-04-25 | 陕西绿盾生物制品有限责任公司 | Method for producing organic fertilizer by polyoxin residue |
| CN102885056A (en) * | 2011-07-22 | 2013-01-23 | 湖北绿天地生物科技有限公司 | Natamycin preparation and preparation method thereof |
| CN103230582A (en) * | 2013-04-17 | 2013-08-07 | 南京工业大学 | Enramycin premix preparation method |
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| CN103145489B (en) * | 2013-02-20 | 2014-07-23 | 游彩霞 | Wettable polyoxin powder and its preparation method |
| CN104621156B (en) * | 2015-01-28 | 2017-04-05 | 南京工业大学 | A kind of preparation method of polyoxin pre-mixing agent |
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- 2015-01-28 CN CN201510044283.4A patent/CN104621156B/en active Active
- 2015-10-26 WO PCT/CN2015/092826 patent/WO2016119491A1/en active Application Filing
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102885056A (en) * | 2011-07-22 | 2013-01-23 | 湖北绿天地生物科技有限公司 | Natamycin preparation and preparation method thereof |
| CN102424636A (en) * | 2011-09-27 | 2012-04-25 | 陕西绿盾生物制品有限责任公司 | Method for producing organic fertilizer by polyoxin residue |
| CN103230582A (en) * | 2013-04-17 | 2013-08-07 | 南京工业大学 | Enramycin premix preparation method |
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