CN103636632B - A kind of Pesticidal combination containing chlorine chlorfenapyr and Aphox - Google Patents
A kind of Pesticidal combination containing chlorine chlorfenapyr and Aphox Download PDFInfo
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- CN103636632B CN103636632B CN201310629395.7A CN201310629395A CN103636632B CN 103636632 B CN103636632 B CN 103636632B CN 201310629395 A CN201310629395 A CN 201310629395A CN 103636632 B CN103636632 B CN 103636632B
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Abstract
The invention discloses a kind of agricultural insecticide composition containing active ingredient chlorine chlorfenapyr and Aphox, wherein the weight ratio of active ingredient chlorine chlorfenapyr and active ingredient Aphox is 1 ~ 30 ︰ 1 ~ 30, and the gross weight of active ingredient accounts for 1% ~ 60% of composition total weight.Present composition formulation comprises wetting powder, water dispersible granules, suspending agent, aqueous emulsion, micro-capsule suspension.The present invention possesses chlorine chlorfenapyr and Aphox two kinds of insecticide double action mechanism, overcomes and delay the drug-fast generation of insect.Synergy is obvious, and dosage reduces, and cost reduces, and insecticidal spectrum increases.The various pests such as control diamond-back moth, prodenia litura, rice fulgorid, cotton bollworm, rice leaf roller can not only be used for, the aphid etc. on vegetables, tobacco, cereal crops can also be prevented and treated.Scope of using increases, and is applicable to the control of the multiple Lepidoptera of fruit tree, vegetables, grain, tobacco etc., Homoptera and Diptera pest.
Description
Technical field
The present invention relates to chlorine chlorfenapyr and Aphox is the Pesticidal combination of active ingredient.
Background technology
Chlorine chlorfenapyr, chemical name is the bromo-2-of 4-(4-chlorphenyl)-1-[(2-chloroethoxy) methyl]-5-trifluoromethyl pyrpole-3-formonitrile HCN, is the new pyrrole heterocycle compound with obvious insecticidal activity that Hunan Chemical Research Institute designs and synthesizes.
Its structural formula is:
Chlorine chlorfenapyr is the analog of novel pesticide chlorfenapyr.Its mechanism of action is by disturbing Intramitochondrial electrochemical gradient thus blocking oxide Phosphorylation events, have excellent to tag, stomach poison activity and comprehensive toxic action, its toxicity is low, and safety is good, without cross resistance.The various pests such as main control diamond-back moth, prodenia litura, rice fulgorid, cotton bollworm, rice leaf roller.But without stifling, systemic action, as eaten into carpophagous aphid, control is difficult to some crop pests.
Aphox (Pirimicarb) is the carbamates selectivity aphicide that the U.S. foretells the development of inside door company.This medicine sterling is colourless. the solid of odorless, can be dissolved in most of organic solvent.Under general condition deposit more stable, but meet strong acid, highly basic or easily decompose under ultraviolet illumination.Aphox have tag, fumigate, systemic action, permeability is woven with to vane group, can effectively prevents and treats aphid organic phosphor being had to resistance.Impose in soil and can be absorbed by crop root, to crop safety, there is quick-acting.This medicine can be used for cereal, fruit tree, vegetables, cigarette, beans and flowers etc.Also effective to Diptera pest.To crop safety, quick-acting is good, but persistence is not long.
The defect of existence is used alone in order to overcome chlorine chlorfenapyr, and expand insecticidal spectrum and the controlling object of chlorine chlorfenapyr, chlorine chlorfenapyr and Aphox are carried out compounded combination by spy, play chlorine chlorfenapyr and Aphox two kinds of insecticidal properties better, improve drug effect, expand insecticidal spectrum and use scope, reduce agriculture this and resistance generation.Have not yet to see the relevant report about chlorine chlorfenapyr and Aphox compounded combination.
Summary of the invention
The object of the invention is the defect being used alone existence in order to overcome chlorine chlorfenapyr, expand insecticidal spectrum and the controlling object of chlorine chlorfenapyr, the invention provides a kind of Pesticidal combination containing insecticidal active ingredient chlorine chlorfenapyr and insecticidal active ingredient Aphox, wherein the weight ratio of insecticidal active ingredient chlorine chlorfenapyr and insecticidal active ingredient Aphox is 1 ~ 30 ︰ 1 ~ 30, and the gross weight of insecticidal active ingredient accounts for 1% ~ 60% of composition total weight.
Pesticidal combination of the present invention, has into wetting powder, water dispersible granules, suspending agent, aqueous emulsion, micro-capsule suspension by the formulation of this area current techique processing.
When the present composition is wetting powder, each constituent content is:
The concrete procedure of processing of said composition wetting powder is: by above-mentioned formula by chlorine chlorfenapyr and Aphox and the mixing of dispersant, wetting agent and filler, uniform stirring in stirred tank, mix after airslide disintegrating mill, the wetting powder of the present composition can be obtained.
When the present composition is for becoming water dispersible granules, each constituent content is:
The concrete procedure of processing of said composition water dispersible granules is: chlorine chlorfenapyr, Aphox and dispersant, wetting agent, disintegrant and filler are mixed by above-mentioned formula, pulverize with micro jet, through mediating, then add in fluidized-bed granulation dryer and carry out through sample analysis after granulation, drying, screening, the water dispersible granules containing chlorine chlorfenapyr and Aphox Pesticidal combination obtained of the present invention.
When the present composition is suspending agent, each constituent content is:
The concrete procedure of processing of said composition suspending agent is first mixed by auxiliary agent, mix through high speed shear, add chlorine chlorfenapyr and the former medicine of Aphox, ball milling 2-3 hour in ball mill, make diameter of particle all below 5 μm, the aqueous suspension formulations containing the Pesticidal combination of chlorine chlorfenapyr and Aphox obtained of the present invention.
When the present composition is aqueous emulsion, each constituent content is:
The concrete procedure of processing of this Pesticidal combination aqueous emulsion is for be added together former medicine chlorine chlorfenapyr and Aphox, solvent and emulsifier, it is made to be dissolved into uniform oil phase, other insecticides adjuvants such as part water, antifreezing agent are mixed into uniform aqueous phase, in a kettle. while high-speed stirred, oil phase is added in aqueous phase, slowly add water until arrive phase inversion point, open clipper and carry out high speed shear, and add remaining water, shear 30min.The i.e. aqueous emulsion preparation containing the Pesticidal combination of chlorine chlorfenapyr and Aphox obtained of the present invention.
When the present composition is micro-capsule suspension, constituent content is:
The processing method of this Pesticidal combination micro-capsule suspension has two kinds:
Method one: the preparation of (1) urea resin prepolymer: by formalin (mol ratio=1:1.5-2 of urea and the formaldehyde) mix and blend of urea and 37% mass percentage concentration, pH to 8.5 is regulated with triethylamine, be warming up to 70 DEG C, with 450 revs/min of stirring reactions 1 hour, obtain the urea resin prepolymer aqueous solution; (2) micro-capsule suspension preparation: under normal temperature, chlorine chlorfenapyr, Aphox are dissolved in solvent, dispersant, urea-formaldehyde resin aqueous solution, emulsifier is added under stirring condition, high speed homogenizing 5 minutes, reduce rotating speed to 450 rev/min after forming oil-in-water emulsion, regulate pH, react 1 hour under acid catalysis, to reaction end, adjust pH to neutral; Add thickener, stir and namely make micro-capsule suspension.
Method two: chlorine chlorfenapyr, Aphox are dissolved in solvent by (1), adds capsule leather material and stirs and obtain oil phase; (2) in water, add emulsifier for mixing and evenly obtain aqueous phase; (3) aqueous phase joins in oil phase, high speed homogenizing formation stabilized oil-in-water emulsion; (4) under 450 revs/min, add pH adjusting agent and participate in interface polymerization reaction, reaction temperature rises to 25 DEG C-70 DEG C, keeps solidifying encystation in 2-24 hour; (5) add dispersant, thickener, stir and namely make micro-capsule suspension.
Described emulsifier is one or more in alkylbenzene naphthalene sulfonate, alkylphenol polyoxyethylene phosphate, diphenyl phenol polyethenoxy polyethenoxy ether, styrenated phenol APEO, alkylphenol polyoxyethylene formaldehyde condensation products, diphenyl phenol polyethenoxy polyformaldehyde condensation product, castor oil ethylene oxide adduct, NNO, NP, agriculture breast 500, agriculture breast 600, Tween-80, polyvinyl alcohol.
Described dispersant is one or more in lignosulfonates, fatty acid amide N methyl taurine sodium salt, alkylphenol polyoxyethylene sulphate, polyoxyethylene polyoxypropylene block copolymer, alkylphenol polyoxyethylene, fatty alcohol-polyoxyethylene ether.
Described wetting agent be selected from lauryl sodium sulfate, calcium dodecyl benzene sulfonate, Nekal BX, sodium alkyl benzene sulfonate, polyoxyethylene tri-styryl phosphenylic acid salt, spaonin powder one or more.
Described disintegrant be selected from bentonite, urea, ammonium sulfate, aluminium chloride, citric acid, succinic acid, sodium bicarbonate one or more.
Described filler be selected from kaolin, diatomite, bentonite, attapulgite, white carbon, starch, precipitated calcium carbonate one or more.
Described thickener is one in aluminium-magnesium silicate, xanthans, CMC, gum Arabic, polyvinylpyrrolidone or several.
Described antifreezing agent is selected from one or more in ethylene glycol, propane diols, glycerine, polyethylene glycol.
Described defoamer is selected from silicone oil, aluminium-magnesium silicate, silicone compound, C
10-20saturated fat acid compounds, C
8-10one or more in aliphatic alcohols compound and polyoxyethylene glycerol ether.
Described capsule leather material is one or more in tolyl isocyanate, the many toluene diisocyanates of polymethylene, methyl diphenylene diisocyanate, Lauxite.
Described solvent is one or more in toluene, dimethylbenzene, ethanol, DMF, chloroform, cyclohexanone, acetone.
Described pH adjusting agent mainly contains one or more in hydrochloric acid, glacial acetic acid, citric acid, sodium hydroxide, ammoniacal liquor, ethylenediamine, triethanolamine, triethylamine.
The present invention has the following advantages:
(1) synergy is obvious: chlorine chlorfenapyr and the mutual mixture of Aphox do not produce conflict, and coordinate synergy, reduces dose, reduces costs.
(2) delaying drug resistance: possess two kinds of insecticide double action mechanism, overcome and delay the drug-fast generation of insect.
(3) insecticidal spectrum is expanded: the various pests such as control diamond-back moth, prodenia litura, rice fulgorid, cotton bollworm, rice leaf roller can not only be used for, the aphid etc. on vegetables, tobacco, cereal crops can also be prevented and treated.
(4) scope of using increases: the control being applicable to the multiple Lepidoptera of fruit tree, vegetables, grain, tobacco etc., Homoptera and Diptera pest.
Embodiment
Be elaborated the present invention below by embodiment, the percentage in embodiment is weight percentage, but the present invention is not limited thereto.
Embodiment 1:21% Aphox chlorine chlorfenapyr wetting powder
Aphox 1%, chlorine chlorfenapyr 20%, polyoxyethylene carboxylate 5%, lauryl sodium sulfate 5%, kaolin complement to 100%, mix laggard row air-flow crushing, obtained 21% Aphox chlorine chlorfenapyr wetting powder.
Embodiment 2:60% Aphox chlorine chlorfenapyr wetting powder
Aphox 30%, chlorine chlorfenapyr 30%, lignosulfonates 7%, spaonin powder 5%, bentonite complement to 100%, mix laggard row air-flow crushing, obtained 60% Aphox chlorine chlorfenapyr wetting powder.
Embodiment 3:2% Aphox chlorine chlorfenapyr wetting powder
Aphox 1%, chlorine chlorfenapyr 1%, alkylsulfonate 4%, Nekal BX 3%, diatomite complement to 100%, mix laggard row air-flow crushing, obtained 2% Aphox chlorine chlorfenapyr wetting powder.
Embodiment 4:40% Aphox chlorine chlorfenapyr water dispersible granules
Aphox 10%, chlorine chlorfenapyr 30%, alkylphenol polyoxyethylene 6%, lauryl sodium sulfate 4%, urea 5%, kaolin supply 100%, and mixing granulation obtains 40% Aphox chlorine chlorfenapyr water-dispersible granules.
Embodiment 5:60% Aphox chlorine chlorfenapyr water dispersible granules
Aphox 30%, chlorine chlorfenapyr 30%, fatty alcohol-polyoxyethylene ether 9%, sodium alkyl benzene sulfonate 5%, ammonium sulfate 2%, diatomite supply 100%, and mixing granulation obtains 60% Aphox chlorine chlorfenapyr water-dispersible granules.
Embodiment 6:2% Aphox chlorine chlorfenapyr water dispersible granules
Aphox 1%, chlorine chlorfenapyr 1%, fatty acid amide N methyl taurine sodium salt 3%, polyoxyethylene tri-styryl phosphenylic acid salt 3%, bentonite supply 100%, the 2% Aphox chlorine chlorfenapyr water-dispersible granules that mixing granulation is obtained.
Embodiment 7:25% Aphox chlorine chlorfenapyr suspending agent
Aphox 20%, chlorine chlorfenapyr 5%, alkylphenol polyoxyethylene 6%, aluminium-magnesium silicate 4%, ethylene glycol 1%, polyoxyethylene glycerol ether 0.5%, water supply 100%, obtained 25% Aphox chlorine chlorfenapyr suspending agent after mixing
Embodiment 8:60% Aphox chlorine chlorfenapyr suspending agent
Aphox 30%, chlorine chlorfenapyr 30%, lignosulfonates 10%, xanthans 3%, polyethylene glycol 2%, silicone oil 1%, water supply 100%, obtained 60% Aphox chlorine chlorfenapyr suspending agent after mixing.
Embodiment 9:2% Aphox chlorine chlorfenapyr suspending agent
Aphox 1%, chlorine chlorfenapyr 1%, fatty alcohol-polyoxyethylene ether 10%, polyvinylpyrrolidone 5%, propane diols 2%, C
8-10aliphatic alcohols compound 0.1%, water supply 100%, obtained 2% Aphox chlorine chlorfenapyr suspending agent after mixing
Embodiment 10:41% Aphox chlorine chlorfenapyr aqueous emulsion
Aphox 30%, chlorine chlorfenapyr 11%, agriculture breast 5008%, dimethylbenzene 6%, aluminium-magnesium silicate 4%, ethylene glycol 1%, polyoxyethylene glycerol ether 0.5%, water supply 100%, obtained 41% Aphox chlorine chlorfenapyr aqueous emulsion after mixing.
Embodiment 11:60% Aphox chlorine chlorfenapyr aqueous emulsion
Aphox 30%, chlorine chlorfenapyr 30%, styrenated phenol APEO 10%, toluene 10%, xanthans 3%, polyethylene glycol 2%, silicone oil 1%, water supply 100%, 60% Aphox chlorine chlorfenapyr aqueous emulsion obtained after mixing.
Embodiment 12:2% Aphox chlorine chlorfenapyr aqueous emulsion
Aphox 1%, chlorine chlorfenapyr 1%, Tween-80 1%, DMF 10%, polyvinylpyrrolidone 5%, propane diols 2%, C
8-10aliphatic alcohols compound 0.1%, water supply 100%, obtained 2% Aphox chlorine chlorfenapyr water after mixing
Emulsion.
Embodiment 13:22% Aphox chlorine chlorfenapyr micro-capsule suspension
Aphox 2%, chlorine chlorfenapyr 20%, toluene 5%, Lauxite 3%, NP5%, sodium lignin sulfonate 3%, hydrochloric acid 2%, sodium hydroxide 1%, xanthans 5%, suitable quantity of water, namely make 22% Aphox chlorine chlorfenapyr micro-capsule suspension according to preparation method one.
Embodiment 14:60% Aphox chlorine chlorfenapyr micro-capsule suspension
Aphox 30%, chlorine chlorfenapyr 30%, dimethylbenzene 5%, toluene di-isocyanate(TDI) 10%, Tween-80 8%, alkylphenol polyoxyethylene 5%, ethylenediamine 1%, aluminium-magnesium silicate 2%, suitable quantity of water, namely make 60% Aphox chlorine chlorfenapyr micro-capsule suspension according to preparation method two.
Embodiment 15:2% Aphox chlorine chlorfenapyr micro-capsule suspension
Aphox 1%, chlorine chlorfenapyr 1%, N; dinethylformamide 1%, methyl diphenylene diisocyanate 0.5%, polyvinyl alcohol 2%, fatty acid amide N methyl taurine sodium salt 1%, triethanolamine 1%, gum Arabic 5%, suitable quantity of water, namely make 2% Aphox chlorine chlorfenapyr micro-capsule suspension according to preparation method two.
This experiment is the method adopting Toxicity Determination and field trial to combine.First by Toxicity Determination, the co-toxicity coefficient (CTC) after clear and definite two kinds of medicaments are composite by a certain percentage, CTC<80 is antagonism, 80≤CTC≤120 are summation action, CTC >=120 are synergistic effect, on this basis, then carry out field trial.
Table 1. Aphox, chlorine chlorfenapyr are to the Toxicity Determination of rice fulgorid
As shown in Table 1, Aphox and the LC50 of chlorine chlorfenapyr to rice fulgorid are respectively 5.68mg/L and 2.78mg/L.Aphox and chlorine chlorfenapyr proportioning are when 30:1 to 1:30, and co-toxicity coefficient CTC is all greater than 120, illustrate that Aphox and chlorine chlorfenapyr mixture in 30:1 to 1:30 scope all shows synergistic effect, and especially both synergistic effects when 1:1 are the most obvious.
The test of pesticide effectiveness of table 2 Aphox, chlorine chlorfenapyr and composite control rice fulgorid thereof
As can be seen from Table 2, Aphox and chlorine chlorfenapyr composite after effectively can prevent and treat rice fulgorid, the lasting period is also long, and control efficiency is all better than the preventive effect of single dose.In test scope of medication, Target crops is had no adverse effects.
The test of pesticide effectiveness of table 3 Aphox, chlorine chlorfenapyr and composite control apple yellow aphid thereof
As can be seen from Table 3, Aphox and chlorine chlorfenapyr composite after not only have good preventive effect to rice fulgorid, also have significant preventive effect to apple yellow aphid, the lasting period might as well, control efficiency is better than the preventive effect of single dose, and expands insecticidal spectrum.
In sum, the present invention contains the Pesticidal combination of Aphox and chlorine chlorfenapyr, has good control efficiency to rice fulgorid and apple yellow aphid.Complex preparation not only increases preventive effect, and expands insecticidal spectrum, and in production reality, tool is of great significance.
Claims (3)
1. an agricultural insecticide composition, it is characterized in that containing active ingredient chlorine chlorfenapyr and active ingredient Aphox, the weight ratio of chlorine chlorfenapyr and Aphox is 1 ~ 30 ︰ 1 ~ 30, the gross weight of active ingredient accounts for 1% ~ 60% of composition total weight, and Pesticidal combination formulation comprises wetting powder, water dispersible granules, suspending agent, aqueous emulsion, micro-capsule suspension.
2. a kind of agricultural insecticide composition according to claim 1, when it is characterized in that said composition formulation is wetting powder, each constituent content is:
Chlorine chlorfenapyr 1-30%
Aphox 1-30%
Dispersant 3-10%
Wetting agent 3-10%
Filler polishing to 100%
When said composition is water dispersible granules, each constituent content is:
Chlorine chlorfenapyr 1-30%
Aphox 1-30%
Dispersant 3-10%
Wetting agent 3-10%
Disintegrant 2-5%
Filler polishing to 100%
When said composition is suspending agent, each constituent content is:
Chlorine chlorfenapyr 1-30%
Aphox 1-30%
Dispersant 3-10%
Antifreezing agent 0.5-4%
Thickener 0.1-2%
Defoamer 0.1-1%
Water polishing to 100%
When said composition is aqueous emulsion, each constituent content is:
Chlorine chlorfenapyr 1-30%
Aphox 1-30%
Emulsifier 2-10%
Solvent 3-10%
Thickener 0.1-5%
Antifreezing agent 0.5-2%
Defoamer 0.1-1%
Water polishing to 100%
When said composition is micro-capsule suspension, constituent content is:
Chlorine chlorfenapyr 1-30%
Aphox 1-30%
Capsule leather material 0.5-10%
Solvent 1-5%
Dispersant 1-8%
Emulsifier 2-8%
Thickener 2-5%
PH adjusting agent 0-3%
Water polishing to 100%.
3. a kind of agricultural insecticide composition according to claim 2, is characterized in that:
Described emulsifier is one or more in alkylbenzene naphthalene sulfonate, alkylphenol polyoxyethylene phosphate, diphenyl phenol polyethenoxy polyethenoxy ether, styrenated phenol APEO, alkylphenol polyoxyethylene formaldehyde condensation products, diphenyl phenol polyethenoxy polyformaldehyde condensation product, castor oil ethylene oxide adduct, NNO, NP, agriculture breast 500, agriculture breast 600, Tween-80, polyvinyl alcohol;
Described dispersant is one or more in lignosulfonates, fatty acid amide N methyl taurine sodium salt, alkylphenol polyoxyethylene sulphate, polyoxyethylene polyoxypropylene block copolymer, alkylphenol polyoxyethylene, fatty alcohol-polyoxyethylene ether;
Described wetting agent be selected from lauryl sodium sulfate, calcium dodecyl benzene sulfonate, Nekal BX, sodium alkyl benzene sulfonate, polyoxyethylene tri-styryl phosphenylic acid salt, spaonin powder one or more;
Described disintegrant be selected from bentonite, urea, ammonium sulfate, aluminium chloride, citric acid, succinic acid, sodium bicarbonate one or more;
Described filler be selected from kaolin, diatomite, bentonite, attapulgite, white carbon, starch, precipitated calcium carbonate one or more;
Described thickener is one in aluminium-magnesium silicate, xanthans, CMC, gum Arabic, polyvinylpyrrolidone or several;
Described antifreezing agent is selected from one or more in ethylene glycol, propane diols, glycerine, polyethylene glycol;
Described defoamer is selected from silicone oil, aluminium-magnesium silicate, silicone compound, C
10-20saturated fat acid compounds, C
8-10one or more in aliphatic alcohols compound and polyoxyethylene glycerol ether;
Described capsule leather material is one or more in tolyl isocyanate, the many toluene diisocyanates of polymethylene, methyl diphenylene diisocyanate, Lauxite;
Described solvent is one or more in toluene, dimethylbenzene, ethanol, DMF, chloroform, cyclohexanone, acetone;
Described pH adjusting agent mainly contains one or more in hydrochloric acid, glacial acetic acid, citric acid, sodium hydroxide, ammoniacal liquor, ethylenediamine, triethanolamine, triethylamine.
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| CN101323584B (en) * | 2005-04-05 | 2010-08-25 | 湖南化工研究院 | Oxime ether aryl pyrrole compounds having insecticidal, acaricidal and antifungal bioactivity |
| EP2320741A2 (en) * | 2008-08-28 | 2011-05-18 | Basf Se | Pesticidal mixtures comprising cyanosulfoximine compounds and spinetoram |
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