CN103004769A - Acaricidal composition containing chlorine chlorfenapyr and spirodiclofen - Google Patents
Acaricidal composition containing chlorine chlorfenapyr and spirodiclofen Download PDFInfo
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- CN103004769A CN103004769A CN2012105720692A CN201210572069A CN103004769A CN 103004769 A CN103004769 A CN 103004769A CN 2012105720692 A CN2012105720692 A CN 2012105720692A CN 201210572069 A CN201210572069 A CN 201210572069A CN 103004769 A CN103004769 A CN 103004769A
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- chlorine chlorfenapyr
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Abstract
The invention discloses an acaricidal composition containing active ingredients, namely chlorine chlorfenapyr and spirodiclofen. The weight ratio of the chlorine chlorfenapyr to the spirodiclofen is (1-30) to (1-30), and the total weight of the active ingredients accounts for 1%-60% of that of the composition. The acaricidal composition provided by the invention is prepared into wettable powder, water dispersible granules, suspending agent, suspoemulsion and microcapsule suspension according to a universal technology in the field. The acaricidal composition is used for preventing red spiders, polyphagotarsonemus latus, tetranychus cinabarinus boisdu and tetranychus urticae koch, and further can be used for preventing mites on fruit trees, vegetables and cotton. The acaricidal composition has the advantages that firstly, the synergism is remarkable, wherein the chlorine chlorfenapyr and the spirodiclofen are blended with each other without conflict, so that the synergism can be adjusted, the dosage of the composition can be reduced, and the cost can be reduced; secondly, by virtue of double action mechanisms of the compounded two acaricide, the insecticide resistance of the mites is delayed; and thirdly, an insecticidal spectrum is expanded, wherein the application range of the composition is enlarged, and the composition is suitable for a plurality of mites on the fruit trees, the vegetables and the cotton.
Description
Technical field
The present invention relates to the chlorine chlorfenapyr and spiral shell mite ester is the miticide composition of active ingredient.
Background technology
The chlorine chlorfenapyr, chemical name is 4-bromo-2-(4-chlorphenyl)-1-[(2-chloroethoxy) methyl]-5-trifluoromethyl pyrpole-3-formonitrile HCN, be the new pyrrole heterocycle compound with obvious pesticide and miticide actility that Hunan Chemical Research Institute designs and synthesizes.
Its structural formula is:
The chlorine chlorfenapyr is the analog of new type disinsection miticide chlorfenapyr.Thereby its mechanism of action is by disturbing Intramitochondrial electrochemical gradient blocking oxide phosphorylation process.Through result of the test show noval chemical compound chlorine chlorfenapyr have excellent tag, stomach poison activity and comprehensive toxic action, its toxicity is low, safety is good, without cross resistance.
Spiral shell mite ester (Spirodiclofen) chemical name be 3-(2,4-dichlorophenyl)-2-oxo-1-oxaspiro [4,5]-last of the ten Heavenly stems-3-alkene-4-base-2,2-dimethyl butyrate acid esters.Its structural formula is for being:
The mechanism of action is the Fatty synthesis that suppresses in the pest mite body.Spiral shell mite ester has tags and stomach toxicity, without interior absorption.It is wide that it kills mite spectrum, the ovum children holds concurrently and kills, lasting period length, low toxicity, low-residual, safety are good, and other miticides without cross resistance.Shortcoming is that its quick-acting is poor, to becoming the mite effect undesirable.Use with existing miticide, both can improve its quick-acting, be conducive to again the resistance management of mite evil.
Have not yet to see about the composite relevant report of chlorine chlorfenapyr and spiral shell mite ester.
Summary of the invention
The invention provides a kind of agricultural chemicals miticide composition that contains effective composition chlorine chlorfenapyr and spiral shell mite ester, wherein the weight ratio of chlorine chlorfenapyr and spiral shell mite ester is 1~30 ︰ 1~30, and the gross weight of active ingredient accounts for 1%~60% of composition total weight.
Miticide composition of the present invention is processed into wetting powder, water dispersible granules, suspending agent, aqueous emulsion, micro-capsule suspension etc. by this area current techique.
When said composition was made wetting powder, each constituent content was:
The concrete procedure of processing of this miticide composition wetting powder is: press above-mentioned prescription with chlorine chlorfenapyr and spiral shell mite ester and dispersant, wetting agent and filler mixing, uniform stirring in stirred tank, behind airslide disintegrating mill, mix, can make the wetting powder of the present composition.
When said composition was made water dispersible granules, each constituent content was:
The concrete procedure of processing of this miticide composition water dispersible granules is: by above-mentioned prescription chlorine chlorfenapyr, spiral shell mite ester and dispersant, wetting agent, disintegrant and filler are mixed, pulverize with micro jet, through mediating, then add and carry out granulation, drying, screening in the fluidized bed prilling dryer by sample analysis, make the water dispersible granules that contains chlorine chlorfenapyr and spiral shell mite ester miticide composition of the present invention.
When said composition was processed into suspending agent, each constituent content was:
The concrete procedure of processing of this miticide composition suspending agent is for mixing auxiliary agent first, mix through high speed shear, add chlorine chlorfenapyr and the former medicine of spiral shell mite ester, in ball mill ball milling 2-3 hour, make diameter of particle all below 5 μ m, make the suspending agent preparation that contains the miticide composition of chlorine chlorfenapyr and spiral shell mite ester of the present invention.
When said composition was processed into aqueous emulsion, each constituent content was:
The concrete procedure of processing of this miticide composition aqueous emulsion is for former medicine chlorine chlorfenapyr and spiral shell mite ester, solvent and emulsifier are added together, make it be dissolved into uniform oil phase, other insecticides adjuvants such as part water, antifreezing agent are mixed into uniform water, when the reactor high speed stirs, oil phase is added aqueous phase, slowly add water until arrive the phase inversion point, open clipper and carry out high speed shear, and add remaining water, shear 30min.Namely make the aqueous emulsion preparation that contains the miticide composition of chlorine chlorfenapyr and spiral shell mite ester of the present invention.
When said composition was processed into micro-capsule suspension, constituent content was:
The processing method of this miticide composition microcapsule suspending agent has two kinds:
Method one: the preparation of (1) urea resin prepolymer: with urea and the 37% formalin (mix and blend of mol ratio=1:1.5-2), regulate pH to 8.5 with triethylamine, be warming up to 70 ℃, with 450 rev/mins of stirring reactions 1 hour, obtain the urea resin prepolymer aqueous solution; (2) micro-capsule suspension preparation: under the normal temperature, chlorine chlorfenapyr, spiral shell mite ester are dissolved in the solvent, add dispersant, urea-formaldehyde resin aqueous solution, emulsifier under the stirring condition, high speed homogenizing 5 minutes, form and reduce rotating speed to 450 rev/min after the oil-in-water emulsion, regulate pH, reaction is 1 hour under acid catalysis, to reaction end, transfer pH to neutral; Add adjuvant, thickener, stir and namely make microcapsule suspending agent.
Method two: (1) is dissolved in chlorine chlorfenapyr, spiral shell mite ester in the solvent, and adding capsule leather material stirs and obtains oil phase; (2) in water, add emulsifier, adjuvant stirs and obtains water; (3) water joins in the oil phase, and the high speed homogenizing forms the stabilized oil-in-water emulsion; (4) under 450 rev/mins, add polyamine and participate in interface polymerization reaction, reaction temperature rises to 25 ℃-70 ℃, keeps solidifying in 2-24 hour encystation; (5) add dispersant, thickener, stir and namely make microcapsule suspending agent.
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, farming breast 500, farming breast 600, Tween-80, the 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, the fatty alcohol-polyoxyethylene ether.
Described wetting agent is selected from one or more in lauryl sodium sulfate, calcium dodecyl benzene sulfonate, Nekal BX, sodium alkyl benzene sulfonate, polyoxyethylene triphenylethylene phosphenylic acid salt, the spaonin powder.
Described disintegrant is selected from one or more in bentonite, urea, ammonium sulfate, aluminium chloride, citric acid, succinic acid, the sodium bicarbonate.
Described filler is selected from one or more in kaolin, diatomite, bentonite, attapulgite, white carbon, starch, the precipitated calcium carbonate.
Described thickener is a kind of or several in aluminium-magnesium silicate, xanthans, CMC, gum Arabic, the polyvinylpyrrolidone.
Described antifreezing agent is selected from one or more in ethylene glycol, propane diols, glycerine, the polyethylene glycol.
Described defoamer is selected from silicone oil, silicone compound, C
10-20Saturated fat acid compounds, C
8-10In aliphatic alcohols compound and the polyoxyethylene glycerol ether one or more.
Described capsule leather material is one or more in tolyl isocyanates, the many toluene diisocyanates of polymethylene, methyl diphenylene diisocyanate, the Lauxite.
Described solvent is one or more in toluene, dimethylbenzene, ethanol, DMF, chloroform, cyclohexanone, the acetone.
Described pH adjusting agent mainly contains a kind of in hydrochloric acid, glacial acetic acid, citric acid, sodium hydroxide, ammoniacal liquor, ethylenediamine, triethanolamine, the triethylamine.
The present invention is used for preventing two spotted spider mite, yellow tea mite, Tetranychus cinnabarinus and Tetranychus urticae, also can be used for the mite class etc. on fruit tree, vegetables and the cotton.Have the following advantages:
(1) synergy is obvious: chlorine chlorfenapyr and spiral shell mite ester mutually are mixed and can produce conflict, and tunable synergy reduces dose, reduces cost.
(2) delaying drug resistance: two kinds of composite miticide double action mechanism delay the drug-fast generation of acarid.
(3) enlarge insecticidal spectrum: this composition is used scope to be increased, and is applicable to the multiple mite class of fruit tree, vegetables, cotton etc.
Embodiment
Below by embodiment the present invention is elaborated, the percentage among the embodiment is weight percentage, but the present invention is not limited thereto.
Embodiment 1:21% spiral shell mite ester chlorine chlorfenapyr wetting powder
Spiral shell mite ester 1%, chlorine chlorfenapyr 20%, polyoxyethylene carboxylate 5%, lauryl sodium sulfate 5%, kaolin complement to 100%, mix laggard promoting the circulation of qi stream and pulverize, and make 21% spiral shell mite ester chlorine chlorfenapyr wetting powder.
Embodiment 2:60% spiral shell mite ester chlorine chlorfenapyr wetting powder
Spiral shell mite ester 30%, chlorine chlorfenapyr 30%, lignosulfonates 7%, spaonin powder 5%, bentonite complement to 100%, mix laggard promoting the circulation of qi stream and pulverize, and make 60% spiral shell mite ester chlorine chlorfenapyr wetting powder.
Embodiment 3:2% spiral shell mite ester chlorine chlorfenapyr wetting powder
Spiral shell mite ester 1%, chlorine chlorfenapyr 1%, alkylsulfonate 4%, Nekal BX 3%, diatomite complement to 100%, mix laggard promoting the circulation of qi stream and pulverize, and make 2% spiral shell mite ester chlorine chlorfenapyr wetting powder.
Embodiment 4:40% spiral shell mite ester chlorine chlorfenapyr water dispersible granules
Spiral shell mite ester 10%, chlorine chlorfenapyr 30%, alkylphenol polyoxyethylene 6%, lauryl sodium sulfate 4%, urea 5%, kaolin supply 100%, and mixing granulation makes 40% spiral shell mite ester chlorine chlorfenapyr water dispersible granules.
Embodiment 5:60% spiral shell mite ester chlorine chlorfenapyr water dispersible granules
Spiral shell mite ester 30%, chlorine chlorfenapyr 30%, fatty alcohol-polyoxyethylene ether 9%, sodium alkyl benzene sulfonate 5%, ammonium sulfate 2%, diatomite supply 100%, and mixing granulation makes 60% spiral shell mite ester chlorine chlorfenapyr water dispersible granules.
Embodiment 6:2% spiral shell mite ester chlorine chlorfenapyr water dispersible granules
Spiral shell mite ester 1%, chlorine chlorfenapyr 1%, fatty acid amide N methyl taurine sodium salt 3%, polyoxyethylene triphenylethylene phosphenylic acid salt 3%, bentonite supply 100%, the 2% spiral shell mite ester chlorine chlorfenapyr water dispersible granules that mixing granulation makes.
Embodiment 7:25% spiral shell mite ester chlorine chlorfenapyr suspending agent
Spiral shell mite ester 20%, chlorine chlorfenapyr 5%, alkylphenol polyoxyethylene 6%, aluminium-magnesium silicate 4%, ethylene glycol 1%, polyoxyethylene glycerol ether 0.5%, water supply 100%, make 25% spiral shell mite ester chlorine chlorfenapyr suspending agent after the mixing.
Embodiment 8:60% spiral shell mite ester chlorine chlorfenapyr suspending agent
Spiral shell mite ester 30%, chlorine chlorfenapyr 30%, lignosulfonates 10%, xanthans 3%, polyethylene glycol 2%, silicone oil 1%, water supply 100%, make 60% spiral shell mite ester chlorine chlorfenapyr suspending agent after the mixing.
Embodiment 9:2% spiral shell mite ester chlorine chlorfenapyr suspending agent
Spiral shell mite ester 1%, chlorine chlorfenapyr 1%, fatty alcohol-polyoxyethylene ether 10%, polyvinylpyrrolidone 5%, propane diols 2%, C8-10 aliphatic alcohols compound 0.1%, water supply 100%, make 2% spiral shell mite ester chlorine chlorfenapyr suspending agent after the mixing.
Embodiment 10:41% spiral shell mite ester chlorine chlorfenapyr aqueous emulsion
Spiral shell mite ester 30%, chlorine chlorfenapyr 11%, farming breast 5008%, dimethylbenzene 6%, aluminium-magnesium silicate 4%, ethylene glycol 1%, polyoxyethylene glycerol ether 0.5%, water supply 100%, make 41% spiral shell mite ester chlorine chlorfenapyr aqueous emulsion after the mixing.
Embodiment 11:60% spiral shell mite ester chlorine chlorfenapyr aqueous emulsion
Spiral shell mite ester 30%, chlorine chlorfenapyr 30%, styrenated phenol APEO 10%, toluene 10%, xanthans 3%, polyethylene glycol 2%, silicone oil 1%, water supply 100%, the 60% spiral shell mite ester chlorine chlorfenapyr aqueous emulsion that makes after the mixing.
Embodiment 12:2% spiral shell mite ester chlorine chlorfenapyr aqueous emulsion
Spiral shell mite ester 1%, chlorine chlorfenapyr 1%, Tween-80 1%, DMF 10%, polyvinylpyrrolidone 5%, propane diols 2%, C
8-10Aliphatic alcohols compound 0.1%, water supply 100%, make 2% spiral shell mite ester chlorine chlorfenapyr aqueous emulsion after the mixing.
Embodiment 13:22% spiral shell mite ester chlorine chlorfenapyr micro-capsule suspension
Spiral shell mite ester 2%, chlorine chlorfenapyr 20%, toluene 5%, Lauxite 3%, NP 5%, sodium lignin sulfonate 3%, hydrochloric acid 2%, sodium hydroxide 1%, xanthans 5%, suitable quantity of water are namely made 22% spiral shell mite ester chlorine chlorfenapyr micro-capsule suspension according to preparation method one.
Embodiment 14:60% spiral shell mite ester chlorine chlorfenapyr micro-capsule suspension
Spiral shell mite ester 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 are namely made 60% spiral shell mite ester (chlorine chlorfenapyr micro-capsule suspension according to preparation method two.
Embodiment 15:2% spiral shell mite ester chlorine chlorfenapyr micro-capsule suspension
Spiral shell mite ester 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 are namely made 2% spiral shell mite ester chlorine chlorfenapyr micro-capsule suspension according to preparation method two.
This experiment is the method that adopts 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 are antagonism, and 80≤CTC≤120 are summation action, and CTC 〉=120 are synergistic effect, on this basis, carry out field trial again.
Table 1. spiral shell mite ester, chlorine chlorfenapyr are to the Toxicity Determination of two-spotted spider mite
As shown in Table 1, spiral shell mite ester and chlorine chlorfenapyr are respectively 2.09mg/L and 2.63mg/L to the LC50 of two spotted spider mite.Spiral shell mite ester and chlorine chlorfenapyr proportioning are when 30:1 to 1:30, and co-toxicity coefficient CTC is all greater than 120, illustrate that spiral shell mite ester and chlorine chlorfenapyr are mixed all to show synergistic effect in 30:1 to 1:30 scope, and especially both synergistic effects when 10:1 are the most obvious.
The test of pesticide effectiveness of table 2 spiral shell mite ester, chlorine chlorfenapyr and composite control two spotted spider mite thereof
As can be seen from Table 2, can effectively prevent and treat two spotted spider mite after spiral shell mite ester and chlorine chlorfenapyr are composite, control efficiency all is better than the preventive effect of single dose.In the test scope of medication, the target crop is had no adverse effects.
The test of pesticide effectiveness of table 3 spiral shell mite ester, chlorine chlorfenapyr and composite control oranges and tangerines Tetranychus urticae thereof
As can be seen from Table 3, not only two spotted spider mite is had good preventive effect after spiral shell mite ester and chlorine chlorfenapyr are composite, the oranges and tangerines Tetranychus urticae is also had significant preventive effect, control efficiency is better than the preventive effect of single dose, and has enlarged insecticidal spectrum.
Claims (2)
1. agricultural chemicals miticide composition that contains effective composition chlorine chlorfenapyr and spiral shell mite ester, the weight ratio that it is characterized in that chlorine chlorfenapyr and spiral shell mite ester is 1~30 ︰ 1~30, the gross weight of active ingredient accounts for 1%~60% of composition total weight, and the miticide composition formulation comprises wetting powder, water dispersible granules, suspending agent, aqueous emulsion, micro-capsule suspension.
2. described a kind of agricultural chemicals miticide composition that contains effective composition chlorine chlorfenapyr and spiral shell mite ester according to claim 1 is characterized in that
When said composition was wetting powder, each constituent content was:
When said composition was water dispersible granules, each constituent content was:
When said composition was suspending agent, each constituent content was:
When said composition was aqueous emulsion, each constituent content was:
When said composition was micro-capsule suspension, constituent content was:
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, farming breast 500, farming breast 600, Tween-80, the 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, the fatty alcohol-polyoxyethylene ether;
Described wetting agent is selected from one or more in lauryl sodium sulfate, calcium dodecyl benzene sulfonate, Nekal BX, sodium alkyl benzene sulfonate, polyoxyethylene triphenylethylene phosphenylic acid salt, the spaonin powder;
Described disintegrant is selected from one or more in bentonite, urea, ammonium sulfate, aluminium chloride, citric acid, succinic acid, the sodium bicarbonate;
Described filler is selected from one or more in kaolin, diatomite, bentonite, attapulgite, white carbon, starch, the precipitated calcium carbonate;
Described thickener is a kind of or several in aluminium-magnesium silicate, xanthans, CMC, gum Arabic, the polyvinylpyrrolidone;
Described antifreezing agent is selected from one or more in ethylene glycol, propane diols, glycerine, the polyethylene glycol;
Described defoamer is selected from silicone oil, silicone compound, C
10-20Saturated fat acid compounds, C
8-10In aliphatic alcohols compound and the polyoxyethylene glycerol ether one or more;
Described capsule leather material is one or more in tolyl isocyanates, the many toluene diisocyanates of polymethylene, methyl diphenylene diisocyanate, the Lauxite;
Described solvent is one or more in toluene, dimethylbenzene, ethanol, DMF, chloroform, cyclohexanone, the acetone;
Described pH adjusting agent mainly contains a kind of in hydrochloric acid, glacial acetic acid, citric acid, sodium hydroxide, ammoniacal liquor, ethylenediamine, triethanolamine, the triethylamine.
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Cited By (2)
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CN104186474A (en) * | 2014-08-11 | 2014-12-10 | 广东中迅农科股份有限公司 | Insecticidal composition containing chlorine chlorfenapyr and methoxyfenozide |
US20220279790A1 (en) * | 2016-12-09 | 2022-09-08 | Adama Makhteshim Ltd. | High-concentration fluensulfone formulations, their uses and processes of preparation |
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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US20220279790A1 (en) * | 2016-12-09 | 2022-09-08 | Adama Makhteshim Ltd. | High-concentration fluensulfone formulations, their uses and processes of preparation |
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Application publication date: 20130403 |