CN102232388A - Flusilazole water dispersible granule and preparation process thereof - Google Patents

Flusilazole water dispersible granule and preparation process thereof Download PDF

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CN102232388A
CN102232388A CN2011101147315A CN201110114731A CN102232388A CN 102232388 A CN102232388 A CN 102232388A CN 2011101147315 A CN2011101147315 A CN 2011101147315A CN 201110114731 A CN201110114731 A CN 201110114731A CN 102232388 A CN102232388 A CN 102232388A
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flusilazole
water dispersible
dispersible granules
water
weight ratio
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CN102232388B (en
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许鑫
戴宝江
杭建胜
吴明
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Jiangshan Pesticides & Chemical Co Ltd Nantong
NANTONG NANCHEN ZHIBAO TECHNOLOGY DEVELOPMENT CO LTD
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Jiangshan Pesticides & Chemical Co Ltd Nantong
NANTONG NANCHEN ZHIBAO TECHNOLOGY DEVELOPMENT CO LTD
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Abstract

The invention provides a flusilazole water dispersible granule which contains 5% to 40% of flusilazole, 0% to 5% of solvent, 5% to 20% of surface active agent, 10% to 20% of absorbant, inert fillers and the like. A preparation process of the flusilazole water dispersible granule comprises the steps of: dissolving crude drugs of flusilazole by using the solvent and the surface active agent under heating and stirring conditions to form a uniform organic liquid phase; then, absorbing the organic liquid phase into a solid wet material by using the absorbant; mixing solid dry materials such as inert fillers and the like into the solid wet material; and after pinching in a pinching machine, extruding, granulating, drying and sieving to obtain the water dispersible granule. The water dispersible granule has high content of effective components and better water dispersity and suspension, is capable of sufficiently playing the medical effect of the flusilazole, is safe and convenient in storage, transportation, measurement and utilization and meets the development requirement of an environmental friendly insecticide.

Description

Flusilazole water dispersible granules and preparation technology thereof
Technical field
The present invention relates to the Flusilazole bactericide in the agricultural chemicals, water dispersible granules and preparation technology thereof that to refer in particular to a kind of main active ingredient be Flusilazole.
Background technology
Flusilazole, molecular formula: C16H15F2N3Si, chemical name: two (4-fluorophenyls)-(1H-1,2,4-triazol-1-yl methyl) monosilane, chemical structural formula:
Figure BSA00000489170800011
Flusilazole can be used as disinfectant use in agriculture; At present, the formulation of Flusilazole bactericide is mainly missible oil (57%), aqueous emulsion (16%) and microemulsion (18%), owing to contain a large amount of organic solvents in the product of these formulations, active ingredient is on the low side, can cause negative effect to environment; Also having the fraction formulation is pulvis, dust pollution atmosphere during use, and crop absorption is bad, and drug effect reduces.
The number of applying for a patent is that the aqueous emulsion of 200810101142.1 the disclosed a kind of fluorine silicon azoles of specification and the number of applying for a patent are the microemulsion of 200410033766.6 the disclosed a kind of fluorine silicon azoles of specification, and the active ingredient accounting is little, stores and transportation inconvenience.The number of applying for a patent is 03109575.5 the disclosed a kind of Flusilazole aerosol of specification, and except the active ingredient accounting was little, smog had certain harm to operating personnel.The number of applying for a patent is that 200610013029.9 the disclosed a kind of Flusilazole of specification and the bactericidal composition of kresoxim-methyl can be made into multiple formulation, the constituent of water dispersion granule wherein is too complicated, and configuration technology is too simple, allocation ratio is too fuzzy, lack theory and experimental basis, do not reach the drug effect of two kinds of predetermined medicines, even can bring unpredictalbe side effect.
Summary of the invention
Goal of the invention: overcome the shortcoming of traditional Flusilazole bactericide, provide that a kind of comprehensive function is strong, the Flusilazole water dispersible granules of environmental protection, broad-spectrum high efficacy.
Technical scheme: Flusilazole water dispersible granules of the present invention as effective sterilization component, is the water dispersible granular formulation with Flusilazole, adopts water as binding agent in this water dispersible granules preparation process.Include multiple constituent: weight ratio is that 5%~40% Flusilazole, weight ratio are that 0~5% solvent, weight ratio are that 5%~20% surfactant, weight ratio are that 10%~20% adsorbent, weight ratio are 0.01%~3% water, and other contains the part inert filler.
Described solvent is a kind of in toluene, dimethylbenzene, the heavy aromatic solvent or several.
Described surfactant is one or more the mixture in anion, cation, the nonionic surface active agent.Mainly comprise alkyl naphthalene sulfonic acid condensation polymer sodium salt, enhancement mode naphthalenesulfonate, lignosulfonates, carboxylate, sodium isopropyl xanthate, sodium alklyarylsulfonate mixture, block copolymer etc.
Described adsorbent is silica gel, white carbon, activated alumina, corn starch, lactose or dextrin etc.
Described filler is diatomite, kaolin, bentonite or attapulgite etc.
Among the present invention, Flusilazole is preferably 10%~25%, and this moment, the bacteria-eliminating efficacy of bactericide was better.When solvent preferably used No. 150 heavy aromatic solvents or No. 200 heavy aromatic solvents, solute effect was better.
Among the present invention, can also contain weight ratio and be 3%~10% dispersant and weight ratio is 0~7% wetting agent; The trade mark of described dispersant or model are T2020, D425 or YUS-WG4; The trade mark of described wetting agent or model are TERWET1004, SD200 or YUS-SXC.
The particle diameter of water dispersion granule of the present invention can be 500 μ m~5mm.
Another object of the present invention: the preparation technology that the large-scale production of a kind of Flusilazole water dispersible granules is provided.
For realizing this purpose of the present invention, adopt such technical scheme: comprise following preparation process:
One, former medicinal solvent of bactericide Flusilazole and surfactant are dissolved under water-bath heating and stirring condition, form the organic liquid phase of homogeneous, the temperature of water-bath heating may be selected to be 50 ℃~70 ℃ scope.
Two, with adsorbent organic liquid is adsorbed as mutually the solid-state wet feed of pasty state.
Three, dispersant, wetting agent, filler are fully mixed after, become the solid-state siccative of powdery through comminution by gas stream.
Four, in kneader, solid-state wet feed and solid-state siccative are mixed, add suitable quantity of water and make binding agent, fully mediate.
Five, material extruder grain, oven dry, the screening after will mediating obtains the Flusilazole water dispersible granules; The particle diameter of material extruder grain is 500 μ m~5mm.
Beneficial effect:
Flusilazole water dispersible granules of the present invention has water dispersible and suspension preferably, and disintegration rapidly after the entry disperses, and forms the higher suspension dispersion.Working concentration lower surface tension force is low, can give full play to drug effect.The liquid preparation solidification, the active constituent content height has better physical stability and chemical stability in storage period.Do not have dust from flying during use, avoid the harm that causes because of dust from flying.Than great, packaging volume is little, stores and transports convenient and safe.Good fluidity is easy to metering, can fully pour out from packaging bag.Reduce influence, meet the formulations of pesticide in the world and develop towards the water base property preparation and the non-dusting solid particulate preparation direction of high safety, environmental protection to environment.
Description of drawings
Accompanying drawing is preparation technology's flow chart of the present invention.
Embodiment
Below in conjunction with drawings and Examples the present invention is done more specifically explanation; Adopt technological process as shown in the drawing, prepare Flusilazole water dispersible granules respectively with following constituent:
Embodiment 1: choose the former medicine of 5 gram Flusilazoles, 2 gram xylene solvents, 5 gram alkyl naphthalene sulfonic acid condensation polymer sodium salt surface active agents mixing, be dissolved into homogeneous organic liquid phase under 55 ℃ of water-baths, adsorb into solid-state wet feed with 30 gram activated alumina adsorbents; Again 6 gram T2020 dispersants, 3 gram TERWET1004 wetting agents, 34 gram kaolin fillers are mixed, become solid-state siccative through comminution by gas stream; Solid-state wet feed and solid-state siccative are mediated processing, add suitable quantity of water and make binding agent; Carry out extruder grain, drying, screening at last, obtaining particle diameter is 500 μ m~5mm, and active ingredient is about 6% Flusilazole water dispersible granules.It is 81% that experiment records sample physics suspensibility, and chemical suspensibility is 92%.
The former medicine of embodiment 2:25 gram Flusilazole, No. 200 heavy aromatic solvents of 3 grams, 5 gram enhancement mode naphthalenesulfonate surfactants mix, and are dissolved into homogeneous organic liquid phase under 60 ℃ of water-baths, adsorb into solid-state wet feed with 30 gram corn starchs; Again 7 gram YUS-WG4 dispersants, 2 gram YUS-SXC wetting agents and 18 gram tripolite filling materials are mixed, become solid-state siccative through comminution by gas stream; Solid-state wet feed and solid-state siccative are mediated processing, add suitable quantity of water and make binding agent; Carry out extruder grain, drying, screening at last, drawing and obtaining particle diameter is 500 μ m~5mm, and active ingredient is about 28% Flusilazole water dispersible granules.It is 83% that experiment records sample physics suspensibility, and chemical suspensibility is 95%.
The former medicine of embodiment 3:40 gram Flusilazole, No. 150 heavy aromatic solvents of 3 grams, 5 gram nonionic block copolymer surfactants mix, under 70 ℃ of water-baths, be dissolved into homogeneous organic liquid phase, become solid-state wet feed with 20 gram white carbon adsorbents adsorb with 8 gram corn starchs; Again 5 gram D425 dispersants, 4 gram SD200 wetting agents and 15 gram attapulgite fillers are mixed, become solid-state siccative through comminution by gas stream; Solid-state wet feed and solid-state siccative are mediated processing, add suitable quantity of water and make binding agent; Carry out extruder grain, drying, screening at last, drawing and obtaining particle diameter is 500 μ m~5mm, and active ingredient is about 40% Flusilazole water dispersible granules.It is 80% that experiment records sample physics suspensibility, and chemical suspensibility is 91%.

Claims (8)

1. Flusilazole water dispersible granules, with Flusilazole as effective sterilization component, it is characterized in that: this Flusilazole bactericide is the water dispersible granular formulation, adopt water as binding agent in this water dispersible granules preparation process, include multiple constituent: weight ratio is that 5%~40% Flusilazole, weight ratio are that 0~5% solvent, weight ratio are that 5%~20% surfactant, weight ratio are that 10%~20% adsorbent, weight ratio are 0.01%~3% water, and other has the part inert filler;
Described solvent is a kind of in toluene, dimethylbenzene, the heavy aromatic solvent or several, described surfactant is a kind of in alkyl naphthalene sulfonic acid condensation polymer sodium salt, enhancement mode naphthalene sulfonate, lignosulfonates, carboxylate, the sodium isopropyl xanthate sodium alklyarylsulfonate or several, described adsorbent is a kind of in silica gel, white carbon, activated alumina, corn starch, lactose, the dextrin or several, and described filler is a kind of in diatomite, kaolin, bentonite, the attapulgite or several.
2. Flusilazole water dispersible granules according to claim 1 is characterized in that: the weight ratio of described Flusilazole is 10%~25%.
3. Flusilazole water dispersible granules according to claim 1 is characterized in that: described solvent is No. 150 heavy aromatic solvents or No. 200 heavy aromatic solvents.
4. Flusilazole water dispersible granules according to claim 1 is characterized in that: also contain weight ratio and be 3%~10% dispersant and weight ratio and be 0~7% wetting agent; Described dispersant is T2020, D425 or YUS-WG4; Described wetting agent is TERWET1004, SD200 or YUS-SXC.
5. according to claim 1,2,3 or 4 described Flusilazole water dispersible granules, it is characterized in that: the particle diameter of described water dispersion granule is 500 μ m~5mm.
6. the preparation technology of the described a kind of Flusilazole water dispersible granules of claim 1 is characterized in that: mainly comprise following technical process:
One, former medicinal solvent of bactericide Flusilazole and surfactant are dissolved under water-bath heating and stirring condition, form the organic liquid phase of homogeneous;
Two, with adsorbent organic liquid is adsorbed as mutually the solid-state wet feed of pasty state;
Three, dispersant, wetting agent, filler are fully mixed after, become the solid-state siccative of powdery through comminution by gas stream;
Four, in kneader, solid-state wet feed and solid-state siccative are mixed, add suitable quantity of water and make binding agent, fully mediate;
Five, material extruder grain, oven dry, the screening after will mediating obtains the Flusilazole water dispersible granules.
7. the preparation technology of Flusilazole water dispersible granules according to claim 6 is characterized in that: the temperature of the water-bath heating of described technical process one is 50 ℃~70 ℃.
8. according to the preparation technology of claim 6 or 7 described Flusilazole water dispersible granules, it is characterized in that: the particle diameter of the material extruder grain of described technical process five is 500 μ m~5mm.
CN201110114731.5A 2010-07-28 2011-04-19 Flusilazole water dispersible granule and preparation technology thereof Active CN102232388B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102696584A (en) * 2012-05-09 2012-10-03 安徽华星化工股份有限公司 Method for preparing pesticide granules
CN105410035A (en) * 2015-12-08 2016-03-23 济南舜昊生物科技有限公司 Compounded preparation containing flusilazole

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5837651A (en) * 1993-08-05 1998-11-17 American Cyanamid Company Solid formulation
CN101632355A (en) * 2009-08-31 2010-01-27 桂林集琦生化有限公司 Pesticide water dispersible granule containing organic silicon surface active agent and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5837651A (en) * 1993-08-05 1998-11-17 American Cyanamid Company Solid formulation
CN101632355A (en) * 2009-08-31 2010-01-27 桂林集琦生化有限公司 Pesticide water dispersible granule containing organic silicon surface active agent and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102696584A (en) * 2012-05-09 2012-10-03 安徽华星化工股份有限公司 Method for preparing pesticide granules
CN105410035A (en) * 2015-12-08 2016-03-23 济南舜昊生物科技有限公司 Compounded preparation containing flusilazole

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