CN103355329A - Acaricide composition containing cyflumetofen and spirotetramat - Google Patents
Acaricide composition containing cyflumetofen and spirotetramat Download PDFInfo
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- CN103355329A CN103355329A CN 201310342940 CN201310342940A CN103355329A CN 103355329 A CN103355329 A CN 103355329A CN 201310342940 CN201310342940 CN 201310342940 CN 201310342940 A CN201310342940 A CN 201310342940A CN 103355329 A CN103355329 A CN 103355329A
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Abstract
The invention relates to an acaricide composition containing cyflumetofen and spirotetramat, of which the effective components are a two-element compound of cyflumetofen and spirotetramat in a mass ratio of (1-50):(50-1). In the preparation, the effective components cyflumetofen and spirotetramat account for 1-80 wt% of the whole preparation, and the rest is allowable and acceptable auxiliary components in the pesticide. The formulation of the acaricide composition can be missible oil, suspending agent, wettable powder, water-dispersible granules, aqueous emulsion, microemulsion, granules or microcapsules. The invention is used for controlling main mites parasitized on plants, such as fruit trees, vegetables, tea trees and other crops.
Description
Technical field
The present invention relates to the agriculture chemical compounding technical field, particularly relate to a kind of miticide composition that contains cyflumetofen and spiral shell worm ethyl ester.
Background technology
Cyflumetofen is the novel acyl group acetonitrile class miticide by Japan large tomb chemical company exploitation, with existing insecticide without cross resistance.All without poisoning, all fool proof to non-target organisms such as mammal and aquatile, beneficial organism, natural enemies to each Plants.Parasitize the main mite class of plant for the crops such as fruit tree, vegetables, tea tree and flowers control.To the ovum of tetranychid with to become mite all effective, if higher to the activity of mite.The chemical name of cyflumetofen is (RS)-2-(4-t-butyl-phenyl) 2-cyano group-3-oxo-3-(α, α, the fluoro-o-methyl-benzene of α-tri-) propionic acid-2-methoxyethyl acid, and its chemical structural formula is
.
Spiral shell worm ethyl ester is the tetronic acid compounds, and spiral shell worm ethyl ester has unique function Characteristics, is unique modern insecticide with two-way interior suction conductive performance so far.Spiral shell worm ethyl ester high-efficiency broad spectrum, can effectively prevent and treat various suckings pest, as aphid, thrips, wood louse, mealybug, aleyrodid and scale insect etc.Applicable chief crop comprises, cotton, soybean, oranges and tangerines, tropical fruit tree, nut, grape, lupulus, potato and vegetables etc.The chemical name of spiral shell worm ethyl ester: cis-3-(2,5-3,5-dimethylphenyl)-8-methoxyl group-2-oxo-1-azaspiro [4.5]-last of the ten Heavenly stems 3-alkene-4-guanidine-acetic acid ethyl ester, 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 acaricide is composite or be mixed to have to enlarge and kill the mite 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 cyflumetofen and spiral shell worm ethyl ester is composite on the basis of lab screening and field trial, have obvious synergistic effect.And there is no at present the people about cyflumetofen and the composite miticide composition of spiral shell worm ethyl ester 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 chemicals miticide composition.Parasitize the main mite class of plant for the crops such as fruit tree, vegetables, tea tree and flowers control.
Technical scheme of the present invention realizes by following measures:
A kind of miticide composition that contains cyflumetofen and spiral shell worm ethyl ester, in this miticide composition, the mass ratio of active ingredient cyflumetofen and spiral shell worm ethyl ester is 1～50: 50～1, described miticide composition of the present invention is through the toxicity test experimental verification, the mass ratio of cyflumetofen and spiral shell worm ethyl ester is 1～20: 20～1 o'clock, synergistic effect was better.
The formulations of pesticide that described miticide composition of the present invention can be prepared are missible oil, suspending agent, wetting powder, water dispersible granules, aqueous emulsion, microemulsion, granule, microcapsule formulations.Cyflumetofen and the gross mass of spiral shell worm ethyl ester in preparation account for 1%～80% of the whole quality of the pharmaceutical preparations, while wherein accounting for 5%～60%, and toxicity and the residual balance preferably that reaches, cost is also lower.
The specific embodiments of the formulations of pesticide that miticide composition of the present invention is mixed with is as follows:
Described miticide composition is cream preparation, and the mass fraction of component is: 1～50 part of cyflumetofen; 1～50 part of spiral shell worm ethyl ester; 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 cyflumetofen and spiral shell worm ethyl ester being added in solvent after dissolving fully, filling, can be made into the cream preparation of the present composition.
Described miticide composition is suspending agent, and the mass fraction of component is: 1～50 part of cyflumetofen; 1～50 part of spiral shell worm ethyl ester; 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 cyflumetofen and spiral shell worm ethyl ester, 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 miticide composition is wetting powder, and the mass fraction of component is: 1～50 part of cyflumetofen; 1～50 part of spiral shell worm ethyl ester; 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 cyflumetofen is mixed with spiral shell worm ethyl ester 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 miticide composition is water dispersible granules, and the mass fraction of component is: 1～50 part of cyflumetofen; 1～50 part of spiral shell worm ethyl ester; 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 cyflumetofen is mixed with spiral shell worm ethyl ester 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 miticide composition is aqueous emulsion, and the mass fraction of component is: 1～50 part of cyflumetofen; 1～50 part of spiral shell worm ethyl ester; 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 cyflumetofen and spiral shell worm ethyl ester, 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 miticide composition is microemulsion, and the mass fraction of component is: 1～50 part of cyflumetofen; 1～50 part of spiral shell worm ethyl ester; 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.Cyflumetofen and spiral shell worm ethyl ester 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 miticide composition is granule, and the mass fraction of component is: 1～50 part of cyflumetofen; 1～50 part of spiral shell worm ethyl ester; 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 cyflumetofen is mixed in the ratio of formula with each components such as spiral shell worm ethyl ester, 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 miticide composition is microcapsule formulations, and the mass fraction of component is: 1～50 part of cyflumetofen; 1～50 part of spiral shell worm ethyl ester; 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.Get a certain amount of cyflumetofen and spiral shell worm ethyl ester is dissolved in cyclohexane, and add emulsifying dispersant in solution, follow 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 Compositional acaricide that active ingredient is cyflumetofen and spiral shell worm ethyl ester and is had obvious synergistic effect, delay the drug-fast generation in key, and reduced and become to have produced cost and use cost, parasitize the main mite class of plant for the crops such as fruit tree, vegetables, tea tree and flowers control.
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: cyflumetofen proportioning co-toxicity experiments different from spiral shell worm ethyl ester.
1.1 reagent agent
The former medicine of 96% cyflumetofen, 96% the former medicine of spiral shell worm ethyl ester, above-mentioned former medicine provides by research and development department of extra large rel medicine company limited company.
1.2 test target
The examination mite is picked up from the Citrus Research Institute Of Chinese Academy Of Agricultural Sciences test site, and the cultivation management term harmonization, do not use medicament in the recent period, adopts the blade that rewinds citrus red mite (crm), standby after normal temperature laboratory (25 ℃ of left and right) raised for 2 generations by fresh citrus leaves down.
1.3 single dose assay method slide infusion process
The female mite that Individual Size is consistent, body colour is scarlet if choose, to try the mite back side with writing brush sticks on the slide that posts cloth insertion sheet, every slide dilution intervals, on the basis of prerun, respectively two kinds of former medicines are dissolved in to acetone, be diluted to several concentration gradient liquids with the 0.1% Tween 80 aqueous solution again, be placed in beaker standby.
The glutinous slide that the examination mite arranged is immersed in good liquid 5 seconds, each processes four repetitions, after taking-up tiltedly is put in porcelain dish edge drying, be put in Glass carrier box, do not add a cover the illumination box of putting into (25 ± 1) ℃, humidity 7O%～80%, illumination every day 10 hours, microscopy life or death mite number (with its foot of fine, soft fur style of writing, the nonresponder is dead) after 24 hours.
1.4 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 cyflumetofen as the standard medicament, its toxicity index is 100):
The EC of the toxicity index (TI) of spiral shell worm ethyl ester=cyflumetofen
50the EC of/spiral shell worm ethyl ester
50* 100
The EC of the true toxicity index (ATI) of M=cyflumetofen
50the EC of/M
50* 100
The TI of the TI of the theoretical toxicity index (TTI) of M=cyflumetofen * P cyflumetofen+spiral shell worm ethyl ester * P spiral shell worm ethyl ester
The TTI of the ATI/M of the co-toxicity coefficient of M (CTC)=M * 100
In formula:
M is cyflumetofen and the mixture of the different proportionings of spiral shell worm ethyl ester
The P cyflumetofen is cyflumetofen shared ratio in mixture
P spiral shell worm ethyl ester is spiral shell worm ethyl ester shared ratio in mixture
2.1 toxicity test result
Table 1 cyflumetofen and the spiral shell worm ethyl ester indoor measurement result to panonychus citri
As can be seen from the table, while in active ingredient cyflumetofen and spiral shell worm ethyl ester 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 cyflumetofen and spiral shell worm ethyl ester are 1:20～20:1 is the most obvious.Result of the test shows, under indoor conditions, cyflumetofen and spiral shell worm ethyl ester are composite all has higher activity to panonychus citri, 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, field experiment control apple Tetranychus urticae, two spotted spider mite
3.1 field experiment control apple Tetranychus urticae
3.1.1 application method
Test is carried out in red temple orchard, the Tai’an province village, this Plain, place, field, and clay loam, the content of organic matter is about 0.9%.Test tree kind is 17 years living Fuji apples, distance between rows and hills 3m * 3m.Carry out the complete stool spraying and process, the community spouting liquid is used by 675 liters/hectare, only sprays medicine one time.The orchard management level is general, and the test region fruit tree growth is basically identical.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.
3.1.2 investigation method
Each community is at East, West, South, North, the tender tip of middle five positions mark of every strain tree, movable mite quantity on 20 leaves of random searching, hand magnifier is directly observed blade face, investigation mite mouth radix before medicine, after medicine, 1d, 5d, 10d investigate respectively the remaining mite number alive in each community, calculate mite mouth decline rate, and contrast decline rate relatively, the calculating relative control effect.
3.1.3 drug effect computational methods
Mite number * 100 before decline rate (%)=(mite number after the front several dispensers of mite of dispenser)/dispenser
Proofread and correct decline rate or preventive effect (%)=(treatment region mite mouth decline rate-check plot mite mouth decline rate)/(1-check plot mite mouth decline rate) * 100
3.1.4 poisoning investigation method
After dispenser, whether continuous 10d range estimation medicament has poisoning to crop.
3.2 field control effectiveness test result of the test
Table 2 treatment agent control apple Tetranychus urticae 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, each investigation all shows its control efficiency to the apple Tetranychus urticae and all is better than contrasting medicament, cyflumetofen and spiral shell worm ethyl ester after dispenser 1 day, 5 days, within 10 days, the control efficiency to the apple Tetranychus urticae obviously is better than contrasting medicament, according to the observation to field experiment process whole process, in the test dose scope, apple tree grows fine, and the poisoning phenomenon does not all appear in each treatment agent, illustrates that it is safe to apple.
3.2 field experiment control two spotted spider mite
3.2.1 test method
Test selects Guizhou Can Ye research institute citrus orchard to carry out.Kind is citrus reticulata“Unshiu”, and field planting is 25 years.Sprayed medicine the morning that is peak period citrus red mite, by working concentration, reagent agent is diluted water, with workers and peasants' one 16 type knapsack sprayers, according to a conventional method tree crown is sprayed, being sprayed onto blade at the Citrus leaf positive and negative has and drips on a small quantity for degree, contrast spray equivalent clear water.
3.2.2 investigation method
Carry out the insect density investigation respectively at 2d, 4d, 6d before dispenser and after dispenser, 4 directions of the East, West, South, North of setting in each community are respectively selected 1 branch, 5 blades of every tip mark, the movable mite quantity on 20 blades of 4 tips of investigation records altogether.
3.2.3 drug effect computational methods
Calculate insect population decline rate and control efficiency with following formula.Mite number alive * 100 before insect population decline rate (%)=(the mite number of living after the mite number-medicine of living before medicine)/medicine
Preventive effect (%)=(treatment region insect population decline rate-contrast insect population decline rate)/(100-check plot insect population decline rate) * 100
3.2.4 poisoning investigation method
Within 1,3,5,7 days after medicine, observe the Ci trus growth situation, the range estimation medicament to oranges and tangerines without poisoning.
3.2 field control effectiveness test result
Table 3 is treatment agent control citrus red mite field test results
From table 3, can find out, the Mixed Pharmacy of different proportion, carry out field experiment by different consumptions, and after medicine, its control efficiency to citrus red mite all is better than contrasting medicament, and the miticidal effect of cyflumetofen and spiral shell worm ethyl ester increases progressively along with the increase of consumption.According to the field range estimation, in the test dose scope, plant growth is normal, and the poisoning phenomenon to oranges and tangerines does not all appear in each treatment agent, illustrates that it is safe to oranges and tangerines.Advise that the insecticide different from the mechanism of action mixes use to delay the generation of pest resistance to insecticide.
To sum up indoor biometrics and twice field experiment result are described, of the present inventionly take cyflumetofen and spiral shell worm ethyl ester and carry out two yuan of composite miticide compositions as active ingredient, equity apple Tetranychus urticae, two spotted spider mite evil mite shows good control efficiency, to the target crop safety, with single dose, compare, miticide composition 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 the plant damage by disease and insect, better control can be arranged, 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 miticide composition that contains cyflumetofen and spiral shell worm ethyl ester, it is characterized in that: the active ingredient of this miticide composition is cyflumetofen and spiral shell worm ethyl ester binary built, all the other are auxiliary element, and wherein the mass ratio of active ingredient cyflumetofen and spiral shell worm ethyl ester is 1～50: 50～1.
2. miticide composition according to claim 1, it is characterized in that: cyflumetofen and the gross mass of spiral shell worm ethyl ester in preparation account for 1%～80% of the whole quality of the pharmaceutical preparations.
3. miticide composition according to claim 2, it is characterized in that: cyflumetofen and the gross weight of spiral shell worm ethyl ester in preparation account for 5%～60% of the whole quality of the pharmaceutical preparations.
4. according to claim 1 or 2 or 3 described miticide compositions, it is characterized in that: the formulation of this miticide composition is missible oil, suspending agent, wetting powder, water dispersible granules, aqueous emulsion, microemulsion, granule, microcapsule formulations
.
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| CN103734156A (en) * | 2014-01-26 | 2014-04-23 | 上海艳紫化工科技有限公司 | Compound oil suspension agent containing cyflumetofen and spirotetramat |
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| CN103734156A (en) * | 2014-01-26 | 2014-04-23 | 上海艳紫化工科技有限公司 | Compound oil suspension agent containing cyflumetofen and spirotetramat |
| CN103734156B (en) * | 2014-01-26 | 2015-09-16 | 上海艳紫化工科技有限公司 | Cyflumetofen and the composite oil-suspending agent of spiral shell worm ethyl ester |
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Application publication date: 20131023 |