CN103004866B - Insecticidal composition containing sufluoxime ether and pirimiphos-methyl - Google Patents
Insecticidal composition containing sufluoxime ether and pirimiphos-methyl Download PDFInfo
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- CN103004866B CN103004866B CN201210572646.8A CN201210572646A CN103004866B CN 103004866 B CN103004866 B CN 103004866B CN 201210572646 A CN201210572646 A CN 201210572646A CN 103004866 B CN103004866 B CN 103004866B
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Abstract
The invention discloses an insecticidal composition containing active ingredients, namely sufluoxime ether and pirimiphos-methyl. The mass ratio of the sufluoxime ether to the pirimiphos-methyl is (1-20) to (1-10); and the total weight of the active ingredients accounts for 0.2%-68% of the total weight of the composition. The composition provided by the invention can be prepared into water dispersible granules, granules, wettable powder, suspending agent, suspoemulsion, microcapsule suspension for agriculture according to a method known by technicians in the field. The insecticidal composition provided by the invention has remarkable synergism, can delay insecticide resistance to an extent, has a good fast-acting property and persistence, has a good pesticide effect for grain storage beetles, snout beetles, rice weevils, saw toothed grain beetles, tribolium castaneum, grain moths, ephestia cautella, phalaenae and mites, and can be used for preventing stored grain insects, household and public health insects (such as mosquitso and flies). Meanwhile, the dosage of the insecticidal composition is saved.
Description
Technical field
The present invention relates to a kind of Pesticidal combination containing sufluoxime and pirimiphos-methyl.
Technical background
Pirimiphos-methyl is a kind of efficient, low toxicity, quick-acting organic phosphates insecticidal/acaricidal agent, can be widely used in the control of domestic hygiene, public health and crop pests, have and knock down the advantages such as fast, effective, the effective substitute species that simultaneously can be used as phosphine carries out the control of storage pest, consumption is low, human body is had no adverse reaction substantially, not only cost saving, and high-efficiency low-toxicity.
But pirimiphos-methyl is not remarkable to preventive effects such as Lepidoptera storage pest meal moth, India snout moth, Mediterranean snout moth, the black worm of rice, gelechiid, cacac moths.
Sufluoxime chemical name is the fluoro-4-chlorphenyl of 1-(3-)-2-methylmercaptan ethyl ketoxime-O-(2-methyl biphenyl-3-methyl) ether, its chemical structural formula is as follows.
Sufluoxime has obvious stomach toxicity, action of contace poison, and toxicity is low, insecticidal spectrum is wide, can be used for preventing and treating various insects on the crops such as tealeaves, citrus, vegetables, when using dosage is 3～6g a.i./mu, lepidoptera pest is shown to good control efficiency as diamond-back moth, cabbage caterpillar, beet armyworm, euproctis pseudoconspersa, tea geometrid, tea lesser leafhopper, oranges and tangerines swallowtail butterfly etc.Sufluoxime there is no report for the control of storage pest.
Sufluoxime is pyrethroid insecticides, and pirimiphos-methyl is organophosphorus insecticide, and the farm chemical ingredients of different mechanism of action carries out composite, there is notable synergistic effect if composite, effective pest control, lowers agricultural chemicals usage amount, overcomes pesticide resistance or delays the growth of pest resistance to insecticide.
Summary of the invention
The invention provides the Pesticidal combination that a kind of active ingredient is made up of sufluoxime and pirimiphos-methyl.The mass ratio of active ingredient sufluoxime and pirimiphos-methyl is 1～20 ︰ 1～10, and the ratio that the gross weight of active ingredient accounts for composition total weight is 0.2%～68%.The present composition can be mixed with the water dispersible granules, granule, wetting powder, suspending agent, suspension emulsion, the micro-capsule suspension that are applicable to agricultural use according to method known in those skilled in the art.
When the agent of said composition granulation, each constituent content is:
The concrete procedure of processing of this Pesticidal combination granule is: by above-mentioned formula, sufluoxime, pirimiphos-methyl and filler are mixed, then add binding agent, dispersant even, after being dried, sieving, through sample analysis, make the granule that contains sufluoxime and pirimiphos-methyl Pesticidal combination of the present invention.
When said composition is made water dispersible granules, each constituent content is:
The concrete procedure of processing of this Pesticidal combination water dispersible granules is: by above-mentioned formula, sufluoxime, pirimiphos-methyl and dispersant, wetting agent, disintegrant and filler are mixed, pulverize with micro jet, through mediating, then add and in fluidized bed prilling dryer, carry out after granulation, dry, screening, through sample analysis, making the water dispersible granules that contains sufluoxime and pirimiphos-methyl Pesticidal combination of the present invention.
When said composition is made wetting powder, each constituent content is:
The concrete procedure of processing of this Pesticidal combination wetting powder is: by above-mentioned formula, sufluoxime and pirimiphos-methyl and dispersant, wetting agent and filler are mixed, uniform stirring in stirred tank, after airslide disintegrating mill, mix, can make the wetting powder of the present composition.
When said composition is processed into suspending agent, each constituent content is:
The production stage of this Pesticidal combination suspending agent is for first mixing auxiliary agent, mix through high speed shear, add the former medicine of sufluoxime and pirimiphos-methyl, ball milling 2～3 hours in ball mill, make diameter of particle all below 5 μ m, make the suspending agent preparation of the Pesticidal combination that contains sufluoxime and pirimiphos-methyl of the present invention.
When said composition is processed into suspension emulsion, each constituent content is:
The production stage of this Pesticidal combination suspension emulsion is for mixing dispersant, defoamer, thickener, antifreezing agent through high speed shear, add sufluoxime, in sand mill, grind 2～3 hours, make diameter of particle all below 5 μ m, make the former medicine suspending agent of sufluoxime, then by pirimiphos-methyl, emulsifier and various auxiliary agent with the direct emulsification of high speed agitator in suspending agent, make the suspension emulsion of the Pesticidal combination that contains sufluoxime and pirimiphos-methyl of the present invention.
When said composition is processed into micro-capsule suspension, each constituent content is:
The preparation method of this Pesticidal combination microcapsule suspending agent has two kinds:
Method one: the preparation of (1) urea resin prepolymer: by urea and 37% formalin (mol ratio=1 ︰ 1.5～2) mix and blend, with triethylamine adjusting pH to 8.5, be warming up to 70 ℃, with 450 revs/min of stirring reactions 1 hour, obtain the urea resin prepolymer aqueous solution; (2) micro-capsule suspension preparation: under normal temperature, sufluoxime, pirimiphos-methyl are dissolved in solvent, under stirring condition, add dispersant, urea-formaldehyde resin aqueous solution, emulsifier, high speed homogenizing 5 minutes, after forming oil-in-water emulsion, reduce rotating speed to 450 rev/min, regulate pH, under acid catalysis, react 1 hour, to reaction end, adjust pH to neutral; Add adjuvant, thickener, stir and make microcapsule suspending agent.
Method two: (1) is dissolved in sufluoxime, pirimiphos-methyl in solvent, adds capsule leather material to stir and obtains oil phase; (2) in water, add emulsifier, adjuvant to stir and obtain water; (3) water joins in oil phase, and high speed homogenizing forms stabilized oil-in-water emulsion; (4) under 450 revs/min, add polyamine to participate in interface polymerization reaction, reaction temperature rises to 25 ℃～70 ℃, keeps 2～24 hours curing encystation; (5) add dispersant, thickener, stir and make microcapsule suspending agent.
Emulsifier of the present invention 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.
Dispersant of the present invention 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.
Wetting agent of the present invention 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, spaonin powder.
Binding agent of the present invention is one or more in carboxymethyl cellulose, polyvinyl alcohol, gelatin, gum Arabic.
Disintegrant of the present invention is selected from: one or more in bentonite, urea, ammonium sulfate, aluminium chloride, citric acid, succinic acid, sodium bicarbonate.
Filler of the present invention is selected from: one or more in kaolin, diatomite, bentonite, attapulgite, white carbon, starch, precipitated calcium carbonate.
Thickener of the present invention is a kind of or several in aluminium-magnesium silicate, xanthans, CMC, gum Arabic, polyvinylpyrrolidone.
Antifreezing agent of the present invention is selected from: one or more in ethylene glycol, propane diols, glycerine, polyethylene glycol.
Defoamer of the present invention is selected from: silicone oil, silicone compound, C
10-20saturated fat acid compounds, C
8-10one or more in aliphatic alcohols compound, polyoxyethylene glycerol ether.
Capsule leather material of the present invention is one or more in tolyl isocyanates, the many toluene diisocyanates of polymethylene, methyl diphenylene diisocyanate, Lauxite.
Solvent of the present invention is one or more in toluene, dimethylbenzene, ethanol, DMF, chloroform, cyclohexanone, acetone.
PH adjusting agent of the present invention mainly contains the one in hydrochloric acid, glacial acetic acid, citric acid, sodium hydroxide, ammoniacal liquor, ethylenediamine, triethanolamine, triethylamine.
The present composition has significant synergies, can delay to a certain extent drug-fast generation, quick-acting and lasting effect are good, all have good drug effect for grain storage beetle, weevil, rice weevil, saw-toothed grain beetle, red flour beetle, lesser grain borer, meal moth, moth class and mite class; Also can prevent and treat stored grain insects, family and public health insect (mosquito, fly) etc., save dosage simultaneously.
Embodiment
Below in conjunction with embodiment, content of the present invention is described further.
Toxicity Determination:
This experimental example 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 is antagonism, 80≤CTC≤120 are summation action, CTC >=120 are synergistic effect, on this basis, then carry out field trial.
Table 1 sufluoxime and the pirimiphos-methyl toxicity test to meal moth
As seen from Table 1, when sufluoxime and pirimiphos-methyl proportioning are 1 ︰ 20～10 ︰ 1, the co-toxicity coefficient of mixture is more than 140, showing has synergistic effect, especially when sufluoxime and pirimiphos-methyl proportioning are between 1 ︰ 15～5 ︰ 1, synergistic effect is more remarkable, and co-toxicity coefficient is more than 200.
In embodiment, all by weight, the various preparation processing technique of the present composition is prior art, can change to some extent according to different situations for each component percentage composition or proportioning.
Embodiment 1 40% sufluoxime and pirimiphos-methyl wetting powder
Add to 100g by sufluoxime 30g, pirimiphos-methyl 10g, Nekal BX 6g, alkylphenol polyoxyethylene 3g, bentonite 30g, afrodite, make 40% sufluoxime and pirimiphos-methyl wetting powder according to conventional production process.Said preparation is by 1000 times of dilution sprayings, after medicine 7 days to lesser grain borer and rice weevil control efficiency be respectively 94% and 89%; 10% sufluoxime suspending agent and 25% pirimiphos-methyl missible oil, according to same method, dilute respectively 750 times and 1500 times and use afterwards, and after medicine, 7 days preventive effects are respectively 76%, 74% and 64%, 76%.
Embodiment 2 48% sufluoximes and pirimiphos-methyl wetting powder
Add to 100g by sufluoxime 40g, pirimiphos-methyl 8g, lauryl sodium sulfate 6g, lignosulfonates 3g, White Carbon black 20g, kaolin, make 48% sufluoxime and pirimiphos-methyl wetting powder according to conventional production process.Said preparation is by 1000 times of dilution sprayings, after medicine 7 days to lesser grain borer and rice weevil control efficiency be respectively 96% and 94%; 10% sufluoxime suspending agent and 25% pirimiphos-methyl missible oil, according to same method, dilute respectively 750 times and 1500 times and use afterwards, and after medicine, 7 days preventive effects are respectively 76%, 84% and 64%, 76%.
Embodiment 3 2% sufluoximes and pirimiphos-methyl granule
Add to 100g by sufluoxime 1g, pirimiphos-methyl 1g, fatty acid amide N methyl taurine sodium salt 2g, polyvinyl alcohol 2g, bentonite, production technology makes 2% sufluoxime and pirimiphos-methyl granule routinely.Said preparation applies by 5g active ingredient/ton-grain food, the control efficiency of lesser grain borer and rice weevil is respectively to 93% and 91% in after medicine 7 days; 10% sufluoxime suspending agent and 25% pirimiphos-methyl missible oil, according to same method, dilute respectively 750 times and 1500 times and use afterwards, and after medicine, 7 days preventive effects are respectively 67%, 64% and 64%, 66%.
Embodiment 4 10% sufluoximes and pirimiphos-methyl granule
Add to 100g by sufluoxime 9g, pirimiphos-methyl 1g, fatty alcohol-polyoxyethylene ether 3g, gum Arabic 1g, bentonite, production technology makes 10% sufluoxime and pirimiphos-methyl granule routinely.This proportioning applies by 5g active ingredient/ton-grain food, the control efficiency of lesser grain borer and rice weevil is respectively to 84% and 80% in after medicine 7 days; 10% sufluoxime suspending agent and 25% pirimiphos-methyl missible oil, according to same method, dilute respectively 750 times and 1500 times and use afterwards, and after medicine, 7 days preventive effects are respectively 68%, 60% and 64%, 62%.
Embodiment 5 46.2% sufluoximes and pirimiphos-methyl water dispersible granules
Add to 100g by sufluoxime 2.2g, pirimiphos-methyl 44g, alkylphenol polyoxyethylene sulphate 3g, sodium alkyl benzene sulfonate 2g, urea 2g, kaolin, production technology makes 46.2% sufluoxime and pirimiphos-methyl water dispersible granules routinely.This proportioning, by 1000 times of dilution sprayings, is respectively 80% and 82% to the control efficiency of lesser grain borer and rice weevil in after medicine 7 days; 10% sufluoxime suspending agent and 25% pirimiphos-methyl missible oil, according to same method, dilute respectively 750 times and 1500 times and use afterwards, and after medicine, 7 days preventive effects are respectively 67%, 69% and 74%, 73%.
Embodiment 6 60% sufluoximes and pirimiphos-methyl water dispersible granules
Add to 100g by sufluoxime 46g, pirimiphos-methyl 14g, polyoxyethylene polyoxypropylene block copolymer 3g, spaonin powder 5g, ammonium sulfate 3g, bentonite, production technology makes 60% sufluoxime and pirimiphos-methyl water dispersible granules routinely.This proportioning, by 1200 times of dilution sprayings, is respectively 80% and 82% to the control efficiency of lesser grain borer and rice weevil in after medicine 7 days; 10% sufluoxime suspending agent and 25% pirimiphos-methyl missible oil, according to same method, dilute respectively 750 times and 1500 times and use afterwards, and after medicine, 7 days preventive effects are respectively 78%, 72% and 73%, 68%.
Embodiment 7 16% sufluoximes and pirimiphos-methyl suspending agent
Add to 100g by sufluoxime 1g, pirimiphos-methyl 15g, lignosulfonates 2g, xanthans 3g, silicone oil 0.1g, ethylene glycol 3g, water, production technology makes 16% sufluoxime and pirimiphos-methyl suspending agent routinely.This proportioning, by 1500 times of dilution sprayings, is respectively 95% and 96% to the control efficiency of lesser grain borer and rice weevil in after medicine 7 days; 10% sufluoxime suspending agent and 25% pirimiphos-methyl missible oil, according to same method, dilute respectively 750 times and 1500 times and use afterwards, and after medicine, 7 days preventive effects are respectively 70%, 73% and 70%, 75%.
Embodiment 8 42% sufluoximes and pirimiphos-methyl suspending agent
Press sufluoxime 3g, pirimiphos-methyl 39g, fatty acid amide N methyl taurine sodium salt 2g, NP-100.5g, aluminium-magnesium silicate 0.35g, xanthans 0.05g, C
10-20saturated fat acid compounds 0.25g, polyethylene glycol 2g, water add to 100g, and production technology makes 42% sufluoxime and pirimiphos-methyl suspending agent routinely.This proportioning, by 1500 times of dilution sprayings, is respectively 88% and 89% to the control efficiency of lesser grain borer and rice weevil in after medicine 7 days; 10% sufluoxime suspending agent and 25% pirimiphos-methyl missible oil, according to same method, dilute respectively 750 times and 1500 times and use afterwards, and after medicine, 7 days preventive effects are respectively 74%, 78% and 62%, 75%.
Embodiment 9 20% sufluoximes and pirimiphos-methyl suspension emulsion
Press sufluoxime 4g, pirimiphos-methyl 16g, fatty alcohol-polyoxyethylene ether 4g, 500
#3g, aluminium-magnesium silicate 0.4g, xanthans 0.1g, silicone oil 0.1g, propane diols 2g, water add to 100g, and production technology makes 20% sufluoxime and pirimiphos-methyl suspension emulsion routinely.This proportioning, by 1500 times of dilution sprayings, is respectively 90% and 89% to the control efficiency of lesser grain borer and rice weevil in after medicine 7 days; 10% sufluoxime suspending agent and 25% pirimiphos-methyl missible oil, according to same method, dilute respectively 750 times and 1500 times and use afterwards, and after medicine, 7 days preventive effects are respectively 70%, 78% and 62%, 75%.
Embodiment 10 68% sufluoximes and pirimiphos-methyl suspension emulsion
Add to 100g by sufluoxime 10g, pirimiphos-methyl 58g, alkylphenol polyoxyethylene 4g, Tween-80 4g, NP-10 0.5g, aluminium-magnesium silicate 3g, polyoxyethylene glycerol ether 0.13g, ethylene glycol 2g, water, production technology makes 68% sufluoxime and pirimiphos-methyl suspension emulsion routinely.This proportioning, by 1500 times of dilution sprayings, is respectively 90% and 93% to the control efficiency of lesser grain borer and rice weevil in after medicine 7 days; 10% sufluoxime suspending agent and 25% pirimiphos-methyl missible oil, according to same method, dilute respectively 750 times and 1500 times and use afterwards, and after medicine, 7 days preventive effects are respectively 72%, 83% and 65%, 78%.
Embodiment 11 8% sufluoximes and pirimiphos-methyl micro-capsule suspension
Press sufluoxime 2g, pirimiphos-methyl 6g, cyclohexanone 1g, polyphenyl polymethylene polyisocyanates 0.5g, fatty acid amide N methyl taurine sodium salt 2g, diphenyl phenol polyethenoxy polyformaldehyde condensation product 4g, polyvinylpyrrolidone 3g, ethylenediamine 0.5g, technique makes 8% sufluoxime and pirimiphos-methyl micro-capsule suspension routinely.This proportioning, by 800 times of dilution sprayings, is respectively 93% and 90% to the control efficiency of lesser grain borer and rice weevil in after medicine 7 days; 10% sufluoxime suspending agent and 25% pirimiphos-methyl missible oil, according to same method, dilute respectively 750 times and 1500 times and use afterwards, and after medicine, 7 days preventive effects are respectively 75%, 80% and 66%, 72%.
Embodiment 12 50% sufluoximes and pirimiphos-methyl micro-capsule suspension
By sufluoxime 5g, pirimiphos-methyl 45g, dimethylbenzene 5g, alkylene diisocyanate 2g, alkylphenol polyoxyethylene sulphate 4g, styrenated phenol APEO 5g, CMC 3g, triethanolamine 2g routinely technique make 50% sufluoxime and pirimiphos-methyl micro-capsule suspension.This proportioning, by 1500 times of dilution sprayings, is respectively 93% and 95% to the control efficiency of lesser grain borer and rice weevil in after medicine 7 days; 10% sufluoxime suspending agent and 25% pirimiphos-methyl missible oil, according to same method, dilute respectively 750 times and 1500 times and use afterwards, and after medicine, 7 days preventive effects are respectively 77%, 83% and 64%, 79%.
Embodiment 13 25% sufluoximes and pirimiphos-methyl micro-capsule suspension
By sufluoxime 2.5g, pirimiphos-methyl 22.5g, Lauxite 4g, alkylphenol polyoxyethylene 2g, diphenyl phenol polyethenoxy polyformaldehyde condensation product 3g, polyvinylpyrrolidone 5g, hydrochloric acid 1g, sodium hydroxide 2g routinely technique make 25% sufluoxime and pirimiphos-methyl micro-capsule suspension.This proportioning, by 500 times of dilution sprayings, is respectively 93% and 96% to the control efficiency of lesser grain borer and rice weevil in after medicine 7 days; 10% sufluoxime suspending agent and 25% pirimiphos-methyl missible oil, according to same method, dilute respectively 750 times and 1500 times and use afterwards, and after medicine, 7 days preventive effects are respectively 77%, 83% and 74%, 72%.
Claims (2)
1. the Pesticidal combination containing active ingredient sufluoxime and pirimiphos-methyl, the mass ratio that it is characterized in that sufluoxime and pirimiphos-methyl is 1～20 ︰ 1～10, the ratio that the gross weight of active ingredient accounts for composition total weight is 0.2%～68%, and the formulation of composition comprises water dispersible granules, granule, wetting powder, suspending agent, suspension emulsion, micro-capsule suspension.
2. according to claim 1 containing the Pesticidal combination of active ingredient sufluoxime and pirimiphos-methyl, while it is characterized in that composition is granule, each constituent content is:
When said composition is water dispersible granules, each constituent content is:
When said composition is wetting powder, each constituent content is:
When said composition is suspending agent, each constituent content is:
When said composition is suspension emulsion, each constituent content is:
When said composition is micro-capsule suspension, each constituent content is:
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 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, spaonin powder;
Described binding agent is one or more in carboxymethyl cellulose, polyvinyl alcohol, gelatin, gum Arabic;
Described disintegrant is selected from: one or more in bentonite, urea, ammonium sulfate, aluminium chloride, citric acid, succinic acid, sodium bicarbonate;
Described filler is selected from: one or more in kaolin, diatomite, bentonite, attapulgite, white carbon, starch, precipitated calcium carbonate;
Described thickener is a kind of or several in aluminium-magnesium silicate, xanthans, CMC, gum Arabic, polyvinylpyrrolidone;
Described antifreezing agent is selected from: one or more in ethylene glycol, propane diols, glycerine, polyethylene glycol;
Described defoamer is selected from: silicone oil, silicone compound, C
10-20saturated fat acid compounds, C
8-10one or more in aliphatic alcohols compound, polyoxyethylene glycerol ether;
Described capsule leather material is one or more in tolyl isocyanates, 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 the one in hydrochloric acid, glacial acetic acid, citric acid, sodium hydroxide, ammoniacal liquor, ethylenediamine, triethanolamine, triethylamine.
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