CN103975936A - Effect-increased bactericide composition, preparation method and application thereof - Google Patents

Effect-increased bactericide composition, preparation method and application thereof Download PDF

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Publication number
CN103975936A
CN103975936A CN201410202862.2A CN201410202862A CN103975936A CN 103975936 A CN103975936 A CN 103975936A CN 201410202862 A CN201410202862 A CN 201410202862A CN 103975936 A CN103975936 A CN 103975936A
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Prior art keywords
humic acid
synergist
tmtd
metconazole
parts
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CN201410202862.2A
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CN103975936B (en
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周明国
孙琴
张兵
贾晓静
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Nanjing Nannong Pesticide Science & Technology Development Co Ltd
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Nanjing Nannong Pesticide Science & Technology Development Co Ltd
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Abstract

The invention aims to disclose an effect-increased bactericide composition. Raw materials of the bactericide composition comprise, by weight, 1-7 parts of metconazole, 1-7 parts of thiram and 0.5-2 parts of an effect-increasing agent. The effect-increasing agent is one or more of humic acid, magnesium humate, zinc humate and potassium humate. A preparation method includes following steps: adding conventional auxiliary materials to the raw materials and preparing a powdery agent, which is acceptable in use, according to conventional processes. The invention also discloses applications of the bactericide composition in prevention and cure of wheat scab pathogens, powdery mildew or rust, and particularly discloses an application of the bactericide composition in prevention and cure of wheat scab pathogens which has drug resistance to a benzimidazole bactericide. With addition of the effect-increasing agent, the bactericide composition not only achieves maximum effect in bactericidal activity but also has obvious and remarkable growth-stimulating and production-increasing effects.

Description

A kind of synergy fungicide composite and its preparation method and application
Technical field
The present invention relates to belong to the processing technique field of agricultural chemicals, specifically, relate to a kind of synergy fungicide composite and its preparation method and application.
Background technology
Wheat scab is the most important disease that affects China's Wheat Production, the yield and quality of wheat is all caused to significant damage. and China is used benzimidazole and triazole bactericidal agent to prevent and treat head blight for a long time, monitor at present the bacterial strain that above-mentioned medicament is produced to high resistance, and seed DON toxin increases, and the grain security of China's wheat and food security are faced a severe challenge.
Metconazole and tmtd built agent have certain control efficiency to wheat scab, but in the market this series products mainly with common can wet-milling and suspending agent be main, in wetting powder production and use procedure, dust has larger harm to operator, and because its particle diameter is difficult to more greatly reach desirable preventive effect, and easy layering and precipitating in suspending agent storage process, severe patient cannot be poured out from container, and these are all seriously restricting the promotion and application of metconazole tmtd preparation.
Lack at present effect remarkable, concise production process, environmental protection, and pesticidal preparations easy to use.
Summary of the invention
In order to meet the control needs of wheat scab powdery mildew etc., improve the drawback of current conventional pesticide formulation, the object of the invention is to open a kind of synergy fungicide composite, the present invention also aims to the preparation method of open said composition, the present invention also aims to the purposes of open said composition.
The present invention seeks to be achieved through the following technical solutions:
Raw material of the present invention consists of: 0.5-2 parts of 1-7 parts of metconazoles, 1-7 parts of tmtd and synergist, described synergist is humic acid, humic acid magnesium, zinc humic acid, one or more of humic acid potassium.
The preferred raw material of the present invention composition is preferably: 1 part of 1 part of metconazole, 5 parts of tmtd and synergist, described synergist is humic acid, humic acid magnesium, zinc humic acid, one or more of humic acid potassium.
The preferred raw material of the present invention consists of: 1.2 parts of 1 part of metconazole, 2 parts of tmtd and synergist, described synergist is humic acid, humic acid magnesium, zinc humic acid, one or more of humic acid potassium.
Get above-mentioned raw materials, add conventional auxiliary material, according to common process, make acceptable pulvis, wetting powder, suspending agent, granule, water dispersible granules while use. microemulsion, sustained release agent.
Above-mentioned pulvis is preferably ultra-fine pulvis.
The ultra-fine pulvis of the composition of synergy fungicide of the present invention, has also added wetting agent, dispersant, disintegrant and auxiliary material
Described wetting agent is preferably sldium lauryl sulfate.
Described dispersant is preferably polymerization contracting hydrochlorate.
Described disintegrant is preferably ammonium sulfate.
Described Optimization of Adjuvant is that pH value is the kaolin of micro-acid of 5-7.
Above-mentioned wetting agent, dispersant, their mass ratio of disintegrant and auxiliary agent is 1.5:3:1:5.
The preparation method of pharmaceutical composition of the present invention comprises the steps:
A is wetting agent, dispersant, and disintegrant, metconazole and tmtd and water mix and blend, high speed shear obtains suspension;
B by grinding, reaches 2-3 micron to its particle diameter by the suspension of A step, obtains mother liquor to be sprayed;
C adds synergist in the mother liquor that B step obtains, and stirs;
D adopts spray drying process, and the mother liquor in C step is dry, obtains finished product.
The preparation method of pharmaceutical composition of the present invention preferably includes following steps:
A is wetting agent, dispersant, and disintegrant, metconazole and tmtd and water are pressed the weight ratio mix and blend of 1:0.8, and high speed shear obtains the suspension of pre-sand milling;
B grinds the suspension of A step by two series connection sand mills, reach 2-3 micron to its particle diameter, obtains mother liquor to be sprayed;
C adds synergist in the mother liquor in B step and stirs;
D adopts spray drying process, by the mother liquor in C step at EAT 110-120, sample introduction speed 50-80Kg/h, atomizing pressure 0.1-0.3MPa, dry under the environment of hot air flow 25-35m3/h, obtain the superfine powder of metconazole tmtd.
Composition of the present invention is being prevented and treated the application of wheat scab germ and/or powdery mildew and/or rust.
beneficial effect of the present invention:
1, technological break-through: compared with existing product and technology of preparing thereof, the present invention has the following advantages: inventor, through a large amount of creationary experimental studies and groping, surprisingly obtains technological break-through, finds to adopt wet grinding, sprays into the preparation processing method of powder.This is compared with Traditional Agricultural medicament preparation, avoided all deficiencies of solid pharmaceutical preparation and liquid preparation: in (1) production process without dust from flying, reduce the harm to environment and operator, be easy to realize cleaning production, solved common wetting powder and added the problems such as dust pollution in man-hour; (2) in water, be cloud diffusion, have good dispersiveness and suspension, suspensibility, up to more than 98%, precipitates thereby solved metconazole tmtd suspending agent storage layered; (3) particle diameter ultra micro, D90 reaches 3 microns, and the medicament of unit mass, at the broad covered area of crop surface, far ahead of other regular dosage form, is more conducive to the performance of bactericidal activity; (4) adding of synergist its biologically active is significantly improved, and crop is had to obvious stimulating growth and production-increasing function; (5) this processing method easily makes the product of high-load, will lead the development of world pesticide formulation.
2, the present invention passes through a large amount of creative research of inventor and gropes, and unexpected discovery, because synergist adds, not only makes its bactericidal activity farthest be brought into play, and crop is had to obvious stimulating growth and production-increasing function, and effect is remarkable
Embodiment
The beneficial effect of further setting forth below pharmaceutical composition of the present invention by test example, following examples are used for illustrating the present invention, limit the scope of the invention but be not used in.
experimental example 1, with conventional products performance comparison test
Reagent agent is selected the prepared Synergistic type 60% metconazole tmtd superfine powder agent of embodiment 1 embodiment 2 embodiment 3 embodiment 4, conventional 60% metconazole thiram wettable powder, conventional 60% metconazole tmtd suspending agent.
Table 1 performance comparison test
As can be seen from Table 1, the superfine powder particle diameter D90 making by the inventive method is all less than 3 microns, and its particle diameter is not only less than conventional suspending agent, is significantly less than especially 15.6 microns of conventional wetting powders; Show intuitively on suspensibility, embodiment of the present invention suspensibility, all higher than more than 98%, is not only better than suspending agent product, especially apparently higher than other several formula wetting powders.And adding of synergist humic acid and salt thereof makes its contact angle be starkly lower than conventional formulation, be slightly better than the fast T of the generally acknowledged synergist of existing market and azone, be more conducive to the adhesion on wheat leaf blade, expansion, but cost of the present invention is starkly lower than fast T and azone.
experimental example 2, field control effectiveness test
Reagent agent is selected the prepared Synergistic type 60% metconazole tmtd superfine powder agent of embodiment 1 embodiment 2 embodiment 3 embodiment 4, conventional 60% metconazole thiram wettable powder, conventional 60% metconazole tmtd suspending agent.
Result of the test is as follows
The flowering initial stage dispenser of table 2 wheat prevents and treats wheat scab.
experimental example 3, above medicament are in wheat powdery mildew initial stage of origination dispenser medication.
Reagent agent is selected the prepared Synergistic type 60% metconazole tmtd superfine powder agent of embodiment 1 embodiment 2 embodiment 3 embodiment 4, conventional 60% metconazole thiram wettable powder, conventional 60% metconazole tmtd suspending agent.
Result of the test is as table 3:
Can find out by table 2 and table 3, the Synergistic type 60% metconazole tmtd Ultramicro-powder consumption making by the embodiment of the present invention is at 40 grams, 60 grams to head blight, powdery mildew all has stable control efficiency, obviously be better than conventional pulvis and the suspending agent of this product, also be obviously better than adding the preparation of fast T and azone, what especially table 2 reflected can extend its lasting period, the disease resistance of wheat that may be synergist humic acid or its salt activator, the growth potential of performance wheat, effect of increasing production is very obvious, amplification can reach 15%--20%, this point has huge advantage preventing and treating in wheat scab.
 
embodiment 1
A is 15Kg wetting agent, 30Kg dispersant, and 50Kg disintegrant, 100Kg metconazole, 500Kg tmtd and 255Kg kaolin and water are pressed the weight ratio mix and blend of 1:0.8, and high speed shear obtains the suspension of pre-sand milling.Wetting agent is sldium lauryl sulfate, and dispersant is polymerization contracting hydrochlorate, and disintegrant is ammonium sulfate, and auxiliary material is that pH value is the kaolin of micro-acid of 5-7.
B grinds the suspension of A step by two series connection sand mills, reach 2-3 micron (controlling its discharging speed is 2-3Kg/min, obtains mother liquor to be sprayed) to its particle diameter.
C adds 100Kg natural source synergist humic acid in the mother liquor in B step and stirs
D adopts spray drying process, by the mother liquor in C step at EAT 110, sample introduction speed 50Kg/h, atomizing pressure 0.1-0.3MPa, dry under the environment of hot air flow 25-35m3/h, obtain the ultrafine preparation containing 60% metconazole tmtd of 10% natural source synergist humic acid
embodiment 2
A is 15Kg wetting agent, 30Kg dispersant, and 50Kg disintegrant, 100Kg metconazole, 500Kg tmtd and 205Kg kaolin and water are pressed the weight ratio mix and blend of 1:0.8, and high speed shear obtains the suspension of pre-sand milling.Wetting agent is sldium lauryl sulfate, and dispersant is polymerization contracting hydrochlorate, and disintegrant is ammonium sulfate, and auxiliary material is that pH value is the kaolin of micro-acid of 5-7.
B grinds the suspension of A step by two series connection sand mills, (controlling its discharging speed is 2-3Kg/min, obtains mother liquor to be sprayed to reach 2-3 micron to its particle diameter.
C adds 100Kg natural source synergist humic acid potassium in the mother liquor in B step and stirs
D adopts spray drying process, by the mother liquor in C step at EAT 120, sample introduction speed 60Kg/h, atomizing pressure 0.1-0.3MPa, dry under the environment of hot air flow 25-35m3/h, obtain the ultrafine preparation containing 60% metconazole tmtd of 10% natural source synergist humic acid potassium.
embodiment 3
A is 15Kg wetting agent, 30Kg dispersant, and 50Kg disintegrant, 100Kg metconazole, 500Kg tmtd and 225Kg kaolin and water are pressed the weight ratio mix and blend of 1:0.8, and high speed shear obtains the suspension of pre-sand milling.Wetting agent is sldium lauryl sulfate, and dispersant is polymerization contracting hydrochlorate, and disintegrant is ammonium sulfate, and auxiliary material is that pH value is the kaolin of micro-acid of 5-7.
B grinds the suspension of A step by two series connection sand mills, reach 2-3 micron (controlling its discharging speed is 2-3Kg/min, obtains mother liquor to be sprayed) to its particle diameter.
C adds 100Kg natural source synergist humic acid magnesium in the mother liquor in B step and stirs
D adopts spray drying process, by the mother liquor in C step at EAT 110, sample introduction speed 50Kg/h, atomizing pressure 0.1-0.3MPa, dry under the environment of hot air flow 25-35m3/h, obtain the ultrafine preparation containing 60% metconazole tmtd of 10% natural source synergist humic acid magnesium
embodiment 4
A is 15Kg wetting agent, 30Kg dispersant, and 50Kg disintegrant, 100Kg metconazole, 500Kg tmtd and 300Kg kaolin and water are pressed the weight ratio mix and blend of 1:0.8, and high speed shear obtains the suspension of pre-sand milling.Wetting agent is sldium lauryl sulfate, and dispersant is polymerization contracting hydrochlorate, and disintegrant is ammonium sulfate, and auxiliary material is that pH value is the kaolin of micro-acid of 5-7.
B grinds the suspension of A step by two series connection sand mills, reach 2-3 micron (controlling its discharging speed is 2-3Kg/min, obtains mother liquor to be sprayed) to its particle diameter.
C adds 100Kg natural source synergist zinc humic acid in the mother liquor in B step and stirs
D adopts spray drying process, by the mother liquor in C step at EAT 110, sample introduction speed 50Kg/h, atomizing pressure 0.1-0.3MPa, dry under the environment of hot air flow 25-35m3/h, obtain the ultrafine preparation containing 60% metconazole tmtd of 10% natural source synergist zinc humic acid.

Claims (10)

1. a synergy fungicide composite, the raw material composition and the weight portion that it is characterized in that making said composition are: 0.5-2 parts of 1-7 parts of metconazoles, 1-7 parts of tmtd and synergist, described synergist is humic acid, humic acid magnesium, zinc humic acid, one or more of humic acid potassium.
2. a kind of synergy fungicide composite as claimed in claim 1, the raw material composition and the weight portion that it is characterized in that making said composition are: 1 part of 1 part of metconazole, 5 parts of tmtd and synergist, described synergist is humic acid, humic acid magnesium, zinc humic acid, one or more of humic acid potassium.
3. a kind of synergy fungicide composite as claimed in claim 1, the raw material composition and the weight portion that it is characterized in that making said composition are: 1.2 parts of 1 part of metconazole, 2 parts of tmtd and synergist, described synergist is humic acid, humic acid magnesium, zinc humic acid, one or more of humic acid potassium.
4. a kind of synergy fungicide composite as described in as arbitrary in claim 1-3, it is characterized in that getting raw material, add conventional auxiliary material, according to common process, make acceptable pulvis, wetting powder, suspending agent, granule, water dispersible granules while use. microemulsion, sustained release agent.
5. a kind of synergy fungicide composite as claimed in claim 4, it is characterized in that making pulvis is ultra-fine pulvis, has also added wetting agent, dispersant, disintegrant and auxiliary material.
6. the ultra-fine pulvis of a kind of synergy fungicide composite as claimed in claim 5, it is characterized in that: described wetting agent is sldium lauryl sulfate, described dispersant is polymerization contracting hydrochlorate, and described disintegrant is ammonium sulfate, and described auxiliary material is that pH value is the kaolin of micro-acid of 5-7.
7. the ultra-fine pulvis of a kind of synergy fungicide composite as described in as arbitrary in claim 5-6, is characterized in that: described wetting agent, and dispersant, their mass ratio of disintegrant and auxiliary material is 1.5:3:5:20-50.
8. the preparation method of the ultra-fine pulvis of a kind of synergy fungicide composite as described in claim 1-3,5-6, is characterized in that: the method comprises the steps:
A is wetting agent, dispersant, and disintegrant, metconazole and tmtd and water mix and blend, high speed shear obtains suspension;
B by grinding, reaches 2-3 micron to its particle diameter by the suspension of A step, obtains mother liquor to be sprayed;
C adds synergist in the mother liquor that B step obtains, and stirs;
D adopts spray drying process, and the mother liquor in C step is dry, obtains finished product.
9. the preparation method of the ultra-fine pulvis of a kind of synergy fungicide composite as claimed in claim 8, is characterized in that: the method comprises the steps:
A is wetting agent, dispersant, and disintegrant, metconazole and tmtd and water are pressed the weight ratio mix and blend of 1:0.8, and high speed shear obtains the suspension of pre-sand milling;
B grinds the suspension of A step by two series connection sand mills, reach 2-3 micron to its particle diameter, obtains mother liquor to be sprayed;
C adds synergist in the mother liquor in B step and stirs;
D adopts spray drying process, by the mother liquor in C step at EAT 110-120, sample introduction speed 50-80Kg/h, atomizing pressure 0.1-0.3MPa, dry under the environment of hot air flow 25-35m3/h, obtain the superfine powder of metconazole tmtd.
10. if a kind of synergy fungicide composite of claim 1-3,5-6 as described in arbitrary is in the application that prevents and treats wheat scab germ and/or powdery mildew and/or rust.
CN201410202862.2A 2014-05-15 2014-05-15 A kind of synergy fungicide composite and its preparation method and application Active CN103975936B (en)

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CN105724393A (en) * 2016-04-07 2016-07-06 陕西上格之路生物科学有限公司 Application of bactericidal compound containing metconazole to preventing wheat scab
CN107258775A (en) * 2017-07-07 2017-10-20 无锡华格新材料有限公司 A kind of pesticide wettable cleanly production technique

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CN105724393A (en) * 2016-04-07 2016-07-06 陕西上格之路生物科学有限公司 Application of bactericidal compound containing metconazole to preventing wheat scab
CN105724393B (en) * 2016-04-07 2018-06-05 陕西上格之路生物科学有限公司 Application of the bactericidal composition containing metconazole in prevention wheat scab
CN107258775A (en) * 2017-07-07 2017-10-20 无锡华格新材料有限公司 A kind of pesticide wettable cleanly production technique

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