CN103355302A - Insecticidal composition containing flubendiamide and pyriproxyfen - Google Patents
Insecticidal composition containing flubendiamide and pyriproxyfen Download PDFInfo
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- CN103355302A CN103355302A CN2013102669311A CN201310266931A CN103355302A CN 103355302 A CN103355302 A CN 103355302A CN 2013102669311 A CN2013102669311 A CN 2013102669311A CN 201310266931 A CN201310266931 A CN 201310266931A CN 103355302 A CN103355302 A CN 103355302A
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- nylar
- fipronil bisamide
- pyriproxyfen
- flubendiamide
- pesticidal combination
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- UCCBKNPOQWTJCB-UHFFFAOYSA-N CC(C)=C1CC2C3(CC3)CC2C1 Chemical compound CC(C)=C1CC2C3(CC3)CC2C1 UCCBKNPOQWTJCB-UHFFFAOYSA-N 0.000 description 1
- QARXCSDERIRMPK-UHFFFAOYSA-N CCC(C1)C11C(C2)C2CC1 Chemical compound CCC(C1)C11C(C2)C2CC1 QARXCSDERIRMPK-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention relates to an insecticidal composition containing flubendiamide and pyriproxyfen. The effective components of flubendiamide and pyriproxyfen are in binary compound, the mass ratio of flubendiamide to pyriproxyfen is 1-50 to 50-1, the total mass of the effective components of flubendiamide and pyriproxyfen in the preparation accounts for 1-80% the mass of the total preparation, the rest components in the preparation are auxiliary elements acceptable in pesticides, and the insecticidal composition can be prepared into missible oil, an suspending agent, wettable powder, water dispersible granule, emulsion in water, microemulsion, granula and microcapsule formulation. The insecticidal composition has excellent prevention and treatment effects on rice-stem borers, botyodes diniasalis walkers, bemisia tabacis, scale insects, plutella xylostellas, asparagus caterpillars, prodenia lituras, pear psyllids, thrips and the like.
Description
Technical field
The present invention relates to the agriculture chemical compounding technical field, particularly relate to a kind of Pesticidal combination that contains fipronil bisamide and Nylar.
Background technology
Fipronil bisamide is researched and developed by Nihon Nihyaku Co., Ltd, belongs to Novel ortho benzenedicarboxamide insecticides, and nearly all Lepidoptera class pest is all had to good activity, not only adult and larva are had to good activity, and speed of action is fast, the lasting period is long.To rice-stem borer and leaf roll snout moth's larva effect, be definitely first-class.The chemical name of fipronil bisamide be the iodo-N ＇ of 3--(2-mesyl-1,1-dimethyl ethyl group-N-{4-[1,2,2,2-tetrafluoro-1-(trifluoromethyl) ethyl]-the 0-tolyl phthalamide, its chemical structural formula is
.
Nylar is the insect growth regulator, IGR that the phenylate class upsets insect growth, belongs to the novel pesticide of juvenoid, in having, absorbs and moves activity, low toxicity, and the lasting period is long, to crop safety, and to the fish low toxicity, the little characteristics to eco-environmental impact.Bemisia tabaci, scale insect, diamond-back moth, beet armyworm, prodenia litura, pear psyllid, thrips etc. are had to good control efficiency, the chemical name of Nylar: 4-phenoxy phenyl (RS)-2-(2-pyridine radicals oxygen) propyl ether, its chemical structural formula is
.
In the real process of agricultural production, using chemical agent is the most effectively means of control plant pest, but the problem the most easily produced by the chemical control insect is the generation of pest resistance to insecticide.And long-term use single chemical insecticide continuously high dose, easily cause the series of problems such as residual, environmental pollution of medicament.Reasonably chemical insecticide is composite or be mixed and have the expansion insecticidal spectrum, improve control efficiency, extend the optimum period for applying fertilizer, reduce dosage, reduce poisoning, reduce residual, delay pest resistance and the positive characteristics such as drug-fast generation and development, pesticide compositional or to be mixed be one of the effective method the most addressed the above problem.We filter out fipronil bisamide and pyriproxyfen compound on the basis of lab screening and field trial, have obvious synergistic effect.And there is no at present the people about the Pesticidal combination of fipronil bisamide and pyriproxyfen compound and application reported.
Summary of the invention
Based on above situation, the object of the invention is to provide a kind of new and effective agricultural insecticide composition.Rice-stem borer, leaf roll snout moth's larva, Bemisia tabaci, scale insect, diamond-back moth, beet armyworm, prodenia litura, pear psyllid, thrips etc. are had to good control efficiency.
Technical scheme of the present invention realizes by following measures:
A kind of Pesticidal combination that contains fipronil bisamide and Nylar, in this Pesticidal combination, the mass ratio of active ingredient fipronil bisamide and Nylar is 1～50: 50～1, described Pesticidal combination of the present invention is through the toxicity test experimental verification, the mass ratio of fipronil bisamide and Nylar is 1～20: 20～1 o'clock, synergistic effect was better.
The formulations of pesticide that described Pesticidal combination of the present invention can be prepared are missible oil, suspending agent, wetting powder, water dispersible granules, aqueous emulsion, microemulsion, granule, microcapsule formulations.Fipronil bisamide and the Nylar gross mass in preparation accounts for 1%～80% of the whole quality of the pharmaceutical preparations, while wherein accounting for 5%～50%, and toxicity and the residual balance preferably that reaches, cost is also lower.
The specific embodiments of the formulations of pesticide that Pesticidal combination of the present invention is mixed with is as follows:
Described Pesticidal combination is cream preparation, and the mass fraction of component is: 1～50 part of fipronil bisamide; 1～50 part of Nylar; 10～30 parts of conventional emulsifiers; 20～50 parts of conventional solvents; 1～5 part of conventional synergist.The concrete production stage of this cream preparation adds emulsifier, the synergist rear oily liquids that becomes transparent and homogeneous that stirs again for first active ingredient fipronil bisamide and Nylar being added in solvent after dissolving fully, filling, can be made into the cream preparation of the present composition.
Described Pesticidal combination is suspending agent, and the mass fraction of component is: 1～50 part of fipronil bisamide; 1～50 part of Nylar; 5～20 parts of dispersants; 1～5 part of antifreezing agent; 0.1～2 part of thickener; 0.1～0.8 part of defoamer; 0～10 part of penetrating agent; 0.1～5 part of pH value conditioning agent; Water, surplus.The concrete production stage of this suspending agent is for first mixing other auxiliary agents, mix through high speed shear, add active ingredient fipronil bisamide and Nylar, in ball crusher, abrading-ball is 2～3 hours, make a diameter all below 5mm, can be made into the suspending agent preparation of the present composition.
Described Pesticidal combination is wetting powder, and the mass fraction of component is: 1～50 part of fipronil bisamide; 1～50 part of Nylar; 3～10 parts of dispersants; 1～5 part of wetting agent; Filler, surplus.The concrete production stage of this wetting powder is: by above-mentioned formula, the active ingredient fipronil bisamide is mixed with Nylar and dispersant, wetting agent and filler, uniform stirring in stirred tank, mixing after airslide disintegrating mill, can be made into the wetting powder of the present composition.
Described Pesticidal combination is water dispersible granules, and the mass fraction of component is: 1～50 part of fipronil bisamide; 1～50 part of Nylar; 3～10 parts of dispersants; 1～10 part of wetting agent; 1～5 part of disintegrant; The filler surplus.The concrete production stage of this water dispersible granules is: by above-mentioned formula, the active ingredient fipronil bisamide is mixed with Nylar and dispersant, wetting agent, disintegrant and filler, with micro jet, pulverize, through mediating, then add in the fluidized bed prilling dryer and carry out granulation, drying, screening by sample analysis, can be made into the water dispersible granules of the present composition.
Described Pesticidal combination is aqueous emulsion, and the mass fraction of component is: 1～50 part of fipronil bisamide; 1～50 part of Nylar; 3～30 parts of emulsifier; 5～15 parts of solvents; 2～15 parts of stabilizing agents; 1～5 part of antifreezing agent; 0.1～8 part of defoamer; 0.2～2 part of thickener; Water, surplus.The concrete production stage of this aqueous emulsion is: at first fipronil bisamide and Nylar, solvent and emulsifier, cosolvent are added together, make to be dissolved into uniform oil phase; By part water, antifreeze, other the insecticides adjuvant such as antimicrobial mixes into uniform water; When the reactor high speed stirs, oil phase is added to water, slowly add water until reach the phase inversion point, open clipper and carry out high speed shear, and add remaining water, shear about half an hour, form the aqueous emulsion of oil-in-water type, can be made into the aqueous emulsion of the present composition.
Described Pesticidal combination is microemulsion, and the mass fraction of component is: 1～50 part of fipronil bisamide amine; 1～50 part of Nylar; 10～30 parts of emulsifier, 1～8 part of antifreezing agent, 0.5～10 part of stabilizing agent, 20～50 parts of conventional solvent cosolvents.Fipronil bisamide and Nylar are dissolved fully with cosolvent, then add other compositions such as emulsifier, antifreezing agent stabilizing agent, evenly mix, finally add water, after fully stirring, can be made into microemulsion.
Described Pesticidal combination is granule, and the mass fraction of component is: 1～50 part of fipronil bisamide; 1～50 part of Nylar; 1～10 part of wetting dispersing agent; 0.1～5 part of thickener; 0.1～5 part of defoamer; Castor oil, surplus is supplied.The active ingredient fipronil bisamide is mixed in the ratio of formula with each components such as Nylar, dispersant, stabilizing agent, defoamer and solvents, after putting into the grinding of sand milling still, send in mixer for well-distribution and mix and get product.
Described Pesticidal combination is microcapsule formulations, and the mass fraction of component is: 1～50 part of fipronil bisamide; 1～50 part of Nylar; 5～20 parts, urea; 5～20 parts, formaldehyde; 5～20 parts of emulsifying dispersants; 1～5 part of antifreezing agent; 0.1～2 part of thickener; 0.1～0.8 part of defoamer; Water, surplus.In being housed, the there-necked flask of agitating device adds urea and formaldehyde (the amount of substance ratio is about l:1.5～2.0), with the pH value to 8 of sodium hydroxide solution regulator solution～9 left and right, then be warming up to 70～80 ℃, reaction obtains stable urea resin prepolymer.The former medicine of getting a certain amount of fipronil bisamide and Nylar is dissolved in cyclohexane, and adds emulsifying dispersant in solution, follows vigorous stirring, the O/W type stable emulsion that to be made into the aqueous solution of take containing emulsifying dispersant be water.Above-mentioned urea resin prepolymer is added in emulsion, regulate the pH value, polymerization reaction take place under the acid catalysis condition, be wrapped oil phase substance, forms microcapsule granule.Slowly heat up, solidify, temperature is controlled at 40～50 ℃, hardening time 1h.Selection adds appropriate auxiliary agent, the microcapsule suspending agent that gets final product stablely.
Wherein above-described emulsifier is selected from calcium dodecyl benzene sulfonate and aliphatic acid polyethenoxy ether, the alkylphenol polyoxyethylene sulfosuccinate, styrylphenol polyoxyethylene ether, polyoxyethylene nonylphenol ether, castor oil polyoxyethylene ether, aliphatic acid polyethenoxy base ester, any or more than one any mixtures than forming in polyoxyethylene aliphatic alcohol ether.
Described solvent is dimethylbenzene or biodiesel, toluene, diesel oil, methyl alcohol, ethanol, n-butanol, isopropyl alcohol, the turpentine-based vegetable oil code name is ND-45, solvent naphtha, dimethyl formamide, dimethyl sulfoxide (DMSO), one or more in the water equal solvent are arbitrarily than the mixture formed.
It is LG-3, GY-D1252, GY-D1256, SNWGF-01 that described dispersant is selected from the polycarboxylate code name, the lignosulfonates code name is 201107,21108, alkylphenol polyoxyethylene methyl ether condensate sulfate, the alkylsulfonate calcium salt, the naphthalene sulfonic acid-formaldehyde condensation product sodium salt, alkylphenol polyoxyethylene, polyoxyethylene carboxylate, aliphatic amine polyoxyethylene ether, one or more in the fatty acid glyceride APEO.
Described wetting agent is selected from lauryl sodium sulfate, calcium dodecyl benzene sulfonate, and Nekal BX, moistening bleeding agent F, alkylbenzenesulfonate polyoxyethylene triphen is phosphenylic acid salt dimly, spaonin powder, silkworm excrement, one or more in the soapberry powder.
Described disintegrant is selected from bentonite, urea, ammonium sulfate, aluminium chloride, citric acid, succinic acid, one or more in sodium bicarbonate.
Described thickener is selected from xanthans, carboxymethyl cellulose, carboxyethyl cellulose, methylcellulose, Magnesiumaluminumsilicate, in polyvinyl alcohol one or more.
Described stabilizing agent is selected from sodium citrate, a kind of in resorcinol.
Described antifreezing agent is selected from ethylene glycol, propane diols, one or more in glycerine.
Described defoamer is selected from silicone oil, silicone compound, C
10-20the saturated fat acid compounds, C
8-10one or more of fatty alcohol.
Described filler is selected from kaolin, diatomite, bentonite, attapulgite, white carbon, starch, one or more in precipitated calcium carbonate.
The present invention be take the compounded pesticides that active ingredient is fipronil bisamide and Nylar and is had obvious synergistic effect, delay the drug-fast generation in key, and reduced to become to produce cost and use cost, rice-stem borer, leaf roll snout moth's larva, Bemisia tabaci, scale insect, diamond-back moth, beet armyworm, prodenia litura, pear psyllid, thrips etc. are had to good control efficiency.
Embodiment
For making technical scheme of the present invention, purpose and advantage are clearer, and the present invention describes with following specific embodiment, but the present invention is not limited to these examples.The mode that effect experiment of the present invention adopts indoor biometrics and field trial to combine, if no special instructions, the ratio of below mentioning is all ratio of quality and the number of copies.
Embodiment: fipronil bisamide proportioning co-toxicity experiments different from Nylar.
1.1 reagent agent
The former medicine of 96% fipronil bisamide, the former medicine of 96% Nylar, above-mentioned former medicine provides by research and development department of extra large rel medicine company limited company.
1.2 test target
Diamond-back moth: the third-instar larvae of the responsive type diamond-back moth that 5 generations of indoor continuous raising and its Individual Size are consistent with physiological status.Temperature (25 ± 2) ℃.Relative moisture 65% ± 5%, periodicity of illumination 12/12h (L/D).
1.3 experimental procedure
1.3.1 medicament preparation
First use the former medicine of acetone solution, according to the result of preliminary experiment, two appropriate former medicines are made into to several different proportionings, then it is stand-by with acetone, each processing to be diluted to respectively to several concentration gradients.
The drop method that adopts NY/T1 154.1-2006 to recommend is measured.By micro intravenous drip device solvent clean, regulate dropper to stand-by state.Choose the examination worm CO of neat and consistent with writing brush
2slight paralysis is placed in the 9cm culture dish, then with the micro intravenous drip device by medicament by a belly that drips to polypide, every some drops physic liquor 0.1L, the corresponding acetone contained with drop 0.1L be treated to contrast, the examination worm after drop is moved to (28
2) ℃, in the culture dish of relative moisture 75%, normally cultivate.Every processing repeats for 4 times, 20 examination worms of every repetition.
1.4 control time
After processing, 24h investigation examination worm death condition (judgement examination worm death standard is gently to sting without autonomic response with pin), record total borer population and dead borer population.
1.5 data statistics and analysis
According to investigation statistics, calculate the corrected mortality that each is processed.And adopt the abundant method of Sun Yun to calculate the co-toxicity coefficient (CTC value) of mixture with reference to NY/T1 154.7-2006.If contrast lethality<5%, do not proofread and correct, the contrast lethality, between 5%-20%, is proofreaied and correct by formula 2, the contrast lethality > 20%, test need be reformed.
The logarithm value of drug concentration (mg/L) of take is independent variable X, and the probability value of corrected mortality of take is dependent variable y, sets up respectively the virulence regression equation formula, adopts DPS software to calculate the EC of single dose and each proportioning mixture
50calculate co-toxicity coefficient (CTC) according to the abundant method of Sun Yun.Co-toxicity coefficient CTC, computing formula is as follows: (take fipronil bisamide as the standard medicament, its toxicity index is 100):
The EC of the toxicity index of Nylar (TI)=fipronil bisamide
50the EC of/Nylar
50* 100
The EC of the true toxicity index (ATI) of M=fipronil bisamide
50the EC of/M
50* 100
The TI of the TI of the theoretical toxicity index (TTI) of M=fipronil bisamide * P fipronil bisamide+Nylar * P Nylar
The TTI of the ATI/M of the co-toxicity coefficient of M (CTC)=M * 100
In formula:
M is fipronil bisamide and the mixture of the different proportionings of Nylar
The P fipronil bisamide is fipronil bisamide shared ratio in mixture
The P Nylar is Nylar shared ratio in mixture.
2.1 toxicity test result
Table 1 fipronil bisamide and the Nylar indoor measurement result to diamond-back moth
As can be seen from the table, while in active ingredient fipronil bisamide and Nylar ratio, being 1:50～50:1 dilution, its co-toxicity coefficient all is greater than 120, shows certain synergistic effect, and the synergistic effect that wherein fipronil bisamide and Nylar are 1:20～20:1 is the most obvious.Result of the test shows, under indoor conditions, fipronil bisamide and pyriproxyfen compound all have higher activity to diamond-back moth, and suggestion is carried out further field control effectiveness test to suitable proportion 1:20～20:1 left and right mixture preparation, to estimate its field practical application effect.
3, the experimental result of field trial control diamond-back moth, rice leaf folder
3.1 field trial control diamond-back moth
3.1.1 test method
Test is carried out at Kaiping City, Guangdong Province suburb truck garden.Process design concentration by each and carry out routine to water spray.Spraying equipment is WF-16 type knapsack hand sprayer, and shower nozzle is single fan nozzle, and operating pressure is 0.2-0.4Mpa, and spray amount is 0.36-0.48L/min, carries out the routine spraying, makes every effort to evenly thoughtful during the spray medicine.During dispenser, the field diamond-back moth is 1～2 instar larvae peak period.
3.1.2 investigation method
In dispenser Qian Mei community by 5 samplings of diagonal. every wild cabbage 2～3 strains (depending on insect density) of choosing Eggs of Diamondback Moth and larva.Statistics is demarcated diamondback moth larvae head number in strain. using this as dispenser before the insect population radix.Within the 7th day, 14 days, 21 days after dispenser, investigate respectively the diamondback moth larvae number of determining residual survival in strain.Using and proofread and correct the insect population decline rate as control efficiency.
3.1.3 drug effect computational methods
Insect population decline rate (%)=(larva number after medicine prelarva number-medicine)/medicine prelarva number * 100
Preventive effect (%)=(treatment region insect population decline rate-contrast insect population decline rate)/(100-check plot insect population decline rate) * 100.
3.1.4 poisoning investigation method
Within 7 days after medicine, observe the wild cabbage growing state, the range estimation medicament to wild cabbage without poisoning.
3.1.5 field control effectiveness test result
As can be seen from Table 2, the Mixed Pharmacy of different proportion, carry out field experiment by different consumptions, after medicine, its control efficiency to diamond-back moth is better than contrasting medicament, with fipronil bisamide and Nylar with the composite control of 2:1 ratio diamond-back moth instant effect, efficiency time is long, and control efficiency is good, and insecticidal effect increases progressively along with the increase of consumption.This is mixed, and can effectively control the harm of diamond-back moth to the host, to the raising of quality of vegetable with increase production significantly, stronger popularizing value is arranged.
3.2 field trial control rice leaf folder
3.2.1 test method
Test site is selected in Qing Feng village, Shuan Feng town, Taicang, and the Rice Cropping mode is transplanting, and kind is " southern round-grained rice 46 ", and the leaf-roller field is evenly distributed.With the manual sprayer spraying, after dispenser, 24h is interior without rain.
3.2.2 investigation method
7d before medicine and after medicine, 14d, 30d investigates drug effect, adopts every community 8 point samplings, investigates the 5 white numbers of sheets in cave, remaining borer population alive, calculates respectively the residual worm amount in white leaf rate, protecting effect of leaves and hundred caves, insecticidal effect for every.
3.2.3 drug effect computational methods
Insecticidal effect=(the residual borer population of the residual borer population-treatment region in the check plot)/residual borer population in check plot * 100%
Protecting effect of leaves=(the white leaf rate of the white leaf rate-treatment region in the check plot)/white leaf rate in check plot * 100%.
3.2.4 poisoning investigation method
Within 7 days after medicine, observe the paddy growth situation, the range estimation medicament to paddy rice without poisoning.
3.2.5 field control effectiveness test result (table 3)
As can be seen from Table 3, the Mixed Pharmacy of different proportion, carry out field experiment by different consumptions, after medicine, its control efficiency to rice leaf folder is better than contrasting medicament, fipronil bisamide and Nylar are with the composite control rice leaf folder of 2:1 ratio instant effect, efficiency time is long, control efficiency is good, insecticidal effect increases progressively along with the increase of consumption, fipronil bisamide and Nylar are better too with the composite protecting effect of leaves of 2:1 ratio simultaneously, to the raising of rice quality with increase production significantly, stronger popularizing value is arranged.
To sum up indoor biometrics and twice field experiment result are described, of the present inventionly take fipronil bisamide and Nylar and carry out two yuan of composite Pesticidal combinations as active ingredient, to diamond-back moth, the insects such as rice leaf folder show good control efficiency, to the target crop safety, with single dose, compare, Pesticidal combination of the present invention has mechanism of action uniqueness, the unit consumption is few, quick-acting is good, lasting period is long, the plurality of advantages such as the effect field is more wide in range, to plant diseases, insect pest can have better control, so, produce very large economic worth in research and development of the present invention and promotion conference, to vast vegetables, the protection tool of the increasing both production and income of the peasant household in fruit tree producing region and local environment is of great significance.
Claims (4)
1. a Pesticidal combination that contains fipronil bisamide and Nylar, it is characterized in that: the active ingredient of this Pesticidal combination is fipronil bisamide and Nylar binary built, all the other are auxiliary element, and wherein the mass ratio of active ingredient fipronil bisamide and Nylar is 1～50: 50～1.
2. Pesticidal combination according to claim 1, it is characterized in that: fipronil bisamide and the Nylar gross mass in preparation accounts for 1%～80% of the whole quality of the pharmaceutical preparations.
3. Pesticidal combination according to claim 2, it is characterized in that: fipronil bisamide and the Nylar gross weight in preparation accounts for 5%～50% of the whole quality of the pharmaceutical preparations.
4. according to claim 1 or 2 or 3 described Pesticidal combinations, it is characterized in that: the formulation of this Pesticidal combination is missible oil, suspending agent, wetting powder, water dispersible granules, aqueous emulsion, microemulsion, granule, microcapsule formulations
.
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| CN103734177A (en) * | 2013-12-30 | 2014-04-23 | 孙蒙蒙 | Flubendiamide-contained insecticidal composition |
| CN104115845A (en) * | 2013-04-24 | 2014-10-29 | 陕西美邦农药有限公司 | Efficient pesticide composition containing flubendiamide |
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