CN102017978B - Pesticidal composition containing Sulfoxaflor and butene-fipronil - Google Patents

Pesticidal composition containing Sulfoxaflor and butene-fipronil Download PDF

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CN102017978B
CN102017978B CN 201110001905 CN201110001905A CN102017978B CN 102017978 B CN102017978 B CN 102017978B CN 201110001905 CN201110001905 CN 201110001905 CN 201110001905 A CN201110001905 A CN 201110001905A CN 102017978 B CN102017978 B CN 102017978B
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butene
fipronil
worm amine
amine nitrile
pyridine worm
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CN102017978A (en
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郑敬敏
何爱华
冯建雄
张崇斌
时晓磊
张�杰
李明甫
侯江利
孙瑞
赵海军
梅红玉
寇鹏斌
乌小瑜
苏蓓
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Shaanxi Sunger Road Bio Science Co Ltd
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Abstract

The invention discloses a pesticidal composition containing Sulfoxaflor and butene-fipronil. The weight ratio of the Sulfoxaflor to butene-fipronil in the composition is 8:1 to 1:8. The pesticidal composition can be prepared into water dispersible granules, wettable powders, suspending agents, dispersible oil suspending agents, missible oil and microemulsion. The invention has the advantages that the ingredients are reasonable, the pesticide effect is good, the drug cost is low, the activity and pesticide effect can be obtained rather than simple overlaid by each ingredient activity but has obvious synergistic effect, the generation resistance can be slowed down, has good safety effect to crops, meets the safety requirement of pesticide preparations, and has better prevention and cure effect on rice planthoppers, weevil, stem borer, cotton aphids, stink bugs, vegetable aphids, whitefly, flea beetle, thrips, citrus aphids, and tessaratoma papillosa drury.

Description

The Pesticidal combination of a kind of fluorine-containing pyridine worm amine nitrile and butene-fipronil
Technical field
The present invention relates to the Pesticidal combination of a kind of fluorine-containing pyridine worm amine nitrile and butene-fipronil, belong to technical field of compounded pesticide.
Background technology
Fluorine pyridine worm amine nitrile english common name sulfoxaflor, chemical name are [1-[6-(trifluoromethyl) pyridin-3-yl] ethyl] methyl (oxygen)-λ 4-sulfydryl cyanamide, chemical molecular formula C 10H 10F 3N 3OS.Fluorine pyridine worm amine nitrile is the sulfimide insecticides, and sulfimide acts on the nervous system of insect, promptly acts on binding site unique in the choline receptor and brings into play insecticidal function.Can be through leaf, stem, root absorption and enter in the plant corpus.Fluorine pyridine worm amine nitrile and other existing numerous insecticides do not have cross resistance, can prevent and treat most of homoptera pest, and especially aphid section, Aleyrodidae, Cicadellidae and Delphacidae insect are applicable to vegetables, paddy rice, cotton, fruit tree and multiple field crop.But in actual application, use the agent of fluorine pyridine worm amine nitrile list to exist use cost height, quick-acting general separately, insect easily produces the defective of resistance.
Butene-fipronil, chemical name: 3-cyano group-5-methylallyl amino-1-(2,6-dichlor-4-trifluoromethyl phenyl)-4-trifluoromethyl sulfinyl pyrazole; Molecular formula: C 16H 10Cl 2F 6N 4OS.Butene-fipronil is a kind of low toxicity Phenylpyrazole insecticides of developing by structural modification on N-substituted phenyl pyrazole compounds basis, novel structure, and mode of action uniqueness belongs to like product with fluorine worm nitrile, second worm nitrile or butene-fipronil.Insect based on stomach poison function, is had concurrently and tags and certain systemic function.Insecticidal mechanism is the chloride normal delivery metabolism that hinders the control of insect one aminobutyric acid, and destruction insect nervous centralis conducts and causes death.The test of pesticide effectiveness shows that this medicine can effectively be prevented and treated Lepidoptera, coleopteran pest adult and larva, as the snout moth's larva of rice, cotton bollworm, diamond-back moth, cabbage caterpillar and leaf miner, beetle etc.Toxicity to fish, shrimp is lower than sharp strength spy, is big characteristics of this medicine.The butene-fipronil of Xiao Shouing is 5% missible oil in the market, and butene-fipronil in use exists the use cost height, the risk that resistance increases gradually, the defective that the lasting period is general.
At present, the pesticidal preparations that with fluorine pyridine worm amine nitrile is effective ingredient is based on 22% fluorine pyridine worm amine nitrile suspending agent and 50% fluorine pyridine worm amine nitrile water dispersible granules, and in actual use, lasting effect is long, but quick-acting is general, the use cost height; Butene-fipronil is as a kind of pyrrole insecticides of brand-new mechanism of action, good disinsection effect, quick-acting is fast, but the use cost height, the risk that resistance increases, the defective that the lasting period is general, the inventor is unexpected to be found the use that is mixed of fluorine pyridine worm amine nitrile and butene-fipronil, have significant synergistic effect, can reduce use cost, slow down the effect that pest resistance produces.
Summary of the invention
The object of the present invention is to provide a kind of component reasonable, significantly synergy, good disinsection effect, drug cost is low, the fluorine pyridine worm amine nitrile that is difficult for developing immunity to drugs and the Pesticidal combination of butene-fipronil.
Another object of the present invention is to provide the application of the Pesticidal combination of fluorine-containing pyridine worm amine nitrile and butene-fipronil.
In order to overcome the defective of existing unitary agent, technical scheme of the present invention is to solve like this:
The Pesticidal combination of fluorine-containing pyridine worm amine nitrile comprises:
A) the first active component fluorine pyridine worm amine nitrile;
B) the second active component butene-fipronil;
The weight ratio of first active component and second active component is 8:1~1:8.
The cumulant of first active component and second active component (content sum) is 1%~80% of a described composition total weight, be preferably 5%~80%, the size of active component cumulant is also closely related with formulation, is no more than 50% as the active component cumulant of suspending agent.
But the preparation formulation that the Pesticidal combination of fluorine pyridine worm amine nitrile of the present invention and butene-fipronil can be prepared according to the known method of those skilled in the art of the present technique is water dispersible granules, wetting powder, suspending agent dispersed oil suspending agent, missible oil, microemulsion.
For water dispersible granules, those skilled in the art are familiar with the use corresponding adjuvants and finish the present invention very much.Dispersant is selected from polycarboxylate, lignosulfonates, alkylnaphthalene sulfonate, alkylphenol polyoxyethylene, EO/PO block polyether; Wetting agent is selected from alkyl sulfate, alkylsulfonate, naphthalene sulfonate, sodium lignin sulfonate, fatty alcohol-polyoxyethylene ether, alkylphenol polyoxyethylene; Disintegrant is selected from ammonium sulfate, sodium sulphate, sodium chloride, ammonium chloride, urea, sucrose, glucose; Binding agent is selected from diatomite, polyvinyl alcohol, polyethylene glycol, polyvinylpyrrolidone, soluble starch, dextrin, xanthans, carboxymethyl (or ethyl) cellulose family; Filler is selected from diatomite, kaolin, white carbon, precipitated calcium carbonate, talcum powder, attapulgite, potter's clay.
To wetting powder, spendable auxiliary agent has: dispersant is selected from polycarboxylate, lignosulfonates, alkylnaphthalene sulfonate; Wetting agent is selected from alkyl sulfate, alkylsulfonate, naphthalene sulfonate; Filler is selected from ammonium sulfate, urea, sucrose, glucose, diatomite, kaolin, white carbon, precipitated calcium carbonate, talcum powder, attapulgite, potter's clay.
To suspending agent, spendable auxiliary agent has: dispersant is selected from polycarboxylate, lignosulfonates, alkylnaphthalene sulfonate, TERSPERSE 2425(U.S. Huntsman Corporation product, alkyl naphthalene sulfonic acid salt); The sorbitan monostearate APEO), agricultural newborn 1601#(common name sorbitan monostearate), Tween-60 #(common name alkyl phenol formaldehyde resin polyoxyethylene ether), farming breast 2201, this dish-60#(common name emulsifier is selected from Nongru-700 #(common name:::: phenethyl phenol polyoxyethylene poly-oxygen propylene aether), TERSPERSE 4894(U.S. Huntsman Corporation produces); Wetting agent is selected from alkylphenol-polyethenoxy base ether formaldehyde condensation products sulphate, alkylphenol-polyethenoxy base ether phosphate, phenethyl phenol polyethenoxy base ether phosphate, alkyl sulfate, alkylsulfonate, naphthalene sulfonate, TERSPERSE 2500(U.S. Huntsman Corporation product); Thickener is selected from xanthans, polyvinyl alcohol, bentonite, aluminium-magnesium silicate; Preservative is selected from formaldehyde, benzoic acid, Sodium Benzoate; Defoamer is selected from silicone based defoamer; Antifreezing agent is selected from ethylene glycol, propane diols, glycerine, urea, inorganic salts such as sodium chloride.
But to the dispersed oil suspending agent, spendable auxiliary agent has: dispersant is selected from polycarboxylate, lignosulfonates, alkylnaphthalene sulfonate (dispersing agent NNO), TERSPERSE 2425; Emulsifier is selected from the BY(castor oil polyoxyethylene ether) serial emulsifier (BY-110, BY-125, BY-140), Nongru-700 #, agricultural newborn 2201#, this dish-60#, Tween-60 #, agricultural newborn 1601#, TERSPERSE 4894; Wetting agent is selected from alkylphenol-polyethenoxy base ether formaldehyde condensation products sulphate, alkylphenol polyoxyethylene phosphate, phenethyl phenol polyethenoxy base ether phosphate, alkyl sulfate, alkylsulfonate, naphthalene sulfonate, TERSPERSE 2500; Thickener is selected from white carbon, polyvinyl alcohol, bentonite, aluminium-magnesium silicate; Antifreezing agent is selected from ethylene glycol, propane diols, glycerine, urea, inorganic salts such as sodium chloride; Stabilizing agent is selected from epoxidized soybean oil, epoxychloropropane, triphenyl phosphate; Dispersion medium is selected from soybean oil, rapeseed oil, corn oil, methyl oleate, diesel oil, machine oil, mineral oil.
Octyl phenol polyoxy ethene (10) ether), agricultural newborn 1601#, agricultural newborn 600#, agricultural newborn 400# for missible oil, spendable auxiliary agent has: emulsifier is selected from calcium dodecyl benzene sulfonate (agricultural newborn 500#), Nongru-700 #, agricultural newborn 2201#, this dish-60#, Tween-60 #, TX-10(common name:; Solvent is selected from dimethylbenzene, solvent naphtha (S-150, S-180, S-200), toluene, biodiesel, methylated vegetable oil, cosolvent, ethyl acetate, methyl alcohol, ethanol, dimethyl formamide, cyclohexanone, acetone, dimethyl sulfoxide (DMSO); Stabilizing agent is selected from triphenyl phosphite, epoxychloropropane, aceticanhydride.
To microemulsion, spendable auxiliary agent has: emulsifier is selected from calcium dodecyl benzene sulfonate (agricultural newborn 500#), Nongru-700 #, agricultural newborn 2201#, this dish-60#, Tween-60 #, TX-10, agricultural newborn 1601#, agricultural newborn 600#, agricultural newborn 400#; Assistant for emulsifying agent is selected from methyl alcohol, isopropyl alcohol, n-butanol, ethanol; Solvent is selected from cyclohexanone, N-Methyl pyrrolidone, acetone, dimethylbenzene, toluene, solvent naphtha (trade mark: S-150, S-180, S-200).
Component of the present invention is reasonable, good disinsection effect, and drug cost is low, and its active and insecticidal effect is not the simple superposition of each composition activity, but significant synergistic effect is arranged, and can slow down the generation of resistance, and is good to crop safety, meets the security requirement of pesticidal preparations.The present invention has the better prevention effect to insects such as rice hoppers, weevil, snout moth's larva, vegetable aphid, trialeurodes vaporariorum, flea beetle, thrips, cotton aphid, stinkbug silk worm, oranges and tangerines aphid, lichee stinkbug silk worms.
Embodiment
In order to prevent and treat rice hoppers, weevil, the snout moth's larva of rice, vegetable aphid, trialeurodes vaporariorum, flea beetle, thrips, cotton aphid, stinkbug silk worm, oranges and tangerines aphid, the lichee stinkbug silk worm in the agricultural production, the inventor has carried out mutual composite synergy research with compositions such as fluorine pyridine worm amine nitrile, butene-fipronils.
1) rice fulgorid (brown planthopper Nilaparvata lugens) test method reference " the agricultural industry criteria NY/T1154.7-2006 of the People's Republic of China (PRC) ".At first single agent and each Mixed Pharmacy are provided with 5 variable concentrations gradients, the concentration gradient of fluorine pyridine worm amine nitrile is 1ug/g, 2ug/g, 4ug/g, 8ug/g, 16ug/g, and the concentration gradient of butene-fipronil and mixture is 0.25ug/g, 0.5ug/g, 1ug/g, 2ug/g, 4ug/g; The examination worm is rice fulgorid (brown planthopper) pupa that picks up from the field, the water rice seedling raised for 3 generations in the greenhouse, select uniformity four age nymph, be pressed into the culture dish of putting rice seedling (with the cotton ball processing of preserving moisture) diameter 12cm, every ware connects and anaesthetizes 30 of nymphs, every processing connects 4 culture dishes, spray under 50PSI pressure with the potter spray tower, ware of each spray, every ware spraying liquid 3ml, treat that insect revives after, the culture dish of handling is put into the 12H/12H illumination box cultivates, check dead borer population in 72 hours, calculate lethality.Blank spray equivalent clear water.Carry out statistical analysis with DPS data processor software, calculate the LC of each medicament 50Value is estimated the activity of reagent agent to the examination worm with this.
The co-toxicity coefficient of mixture (CTC value) calculates by following formula:
Figure 651200DEST_PATH_IMAGE001
In the formula:
ATI---mixture actual measurement toxicity index;
S---standard insecticide LC 50, unit is every liter (mg/L) of milligram;
The LC of M---mixture 50, unit is every liter (mg/L) of milligram;
TTI=TI A×P A+ TI B×P B
In the formula:
The theoretical toxicity index of TTI---mixture;
TI A---A medicament toxicity index;
P A---the percentage composition of A medicament in mixture, unit are percentage (%);
TI B---B medicament toxicity index;
P B---the percentage composition of B medicament in mixture, unit are percentage (%);
Figure 11774DEST_PATH_IMAGE002
In the formula:
CTC---co-toxicity coefficient;
ATI---mixture actual measurement toxicity index;
The theoretical toxicity index of TTI---mixture;
Figure 24992DEST_PATH_IMAGE003
2) paddy rice weevil (Echinocnemus squameus Billherg) coleoptera, Culculionidae.Test method is with reference to " the agricultural industry criteria NY/T1154.6-2006 of the People's Republic of China (PRC) ".At first single agent and each Mixed Pharmacy are provided with 5 variable concentrations gradients (on preliminary experiment result's basis, the weevil lethality is set by geometric progression in 5%~90% scope), the concentration gradient of fluorine pyridine worm amine nitrile is 1ug/g, 2ug/g, 4ug/g, 8ug/g, 16ug/g, and the concentration gradient of butene-fipronil and mixture is 0.25ug/g, 0.5ug/g, 1ug/g, 2ug/g, 4ug/g; The examination worm is the Lissorhoptrus oryzophilus Kuschel that picks up from the field, select the weevil of uniformity in the length of time in the laboratory, weevil is immersed in the ready soup, draw unnecessary soup with filter paper, weevil is transferred under the normal condition raises, every processing repeats for 4 times, whenever repeats to soak 30 of worms, check dead borer population in 24 hours, calculate lethality.
Figure 519427DEST_PATH_IMAGE004
3) rice-stem borer formal name used at school Chilo supperssalis (Walker) Lepidoptera, Pyralidae, another name borer.Test method is with reference to " the agricultural industry criteria NY/T1282-2007 of the People's Republic of China (PRC) ".At first single agent and each Mixed Pharmacy are provided with 5 variable concentrations gradients (on preliminary experiment result's basis, the rice-stem borer lethality is set by geometric progression) in 5%~90% scope.The examination worm is the striped rice borer of picking up from the field, select the striped rice borer of uniformity in the length of time in the laboratory, put into blade-carrying culture dish, every ware 40 cephalont, 4 culture dishes of every processing, repeat 3 times, under 50PSI pressure, spray, spray a ware at every turn with the potter spray tower, every ware spraying liquid 3ml, the culture dish that to handle is put into the 12H/12H illumination box and is cultivated then, checks in 48 hours to calculate lethality by dead borer population.Blank spray equivalent clear water.
Figure 36121DEST_PATH_IMAGE005
4) (Phyllotreta striolata (Fabricius) test method is with reference to " the agricultural industry criteria NY/T1154.6-2006 of the People's Republic of China (PRC) " for the yellow bent flea beetle of vegetables flea beetle (cauliflower).
Figure 833176DEST_PATH_IMAGE006
5) vegetable aphid (cabbage aphid Brevicoryne brassicae), test method is with reference to " the agricultural industry criteria NY/T1154.6-2006 of the People's Republic of China (PRC) ".
Figure 442012DEST_PATH_IMAGE007
6) vegetables trialeurodes vaporariorum (tomato) (Trialeurodes vaporariorum) Homoptera, Aleyrodidae, test method is with reference to " the agricultural industry criteria NY/T1154.6-2006 of the People's Republic of China (PRC) ".
Figure 740138DEST_PATH_IMAGE008
7) vegetables thrips (cucumber) thrips (Frankliniella occidentalis) test method is with reference to " the agricultural industry criteria NY/T1154.6-2006 of the People's Republic of China (PRC) ".
8) oranges and tangerines aphid (citrus aphid Toxoptera citricidus (Kirkaldy), test method reference " the agricultural industry criteria NY/T1154.6-2006 of the People's Republic of China (PRC) ".
Figure 339015DEST_PATH_IMAGE010
9) lichee stinkbug silk worm ( Tessaratoma papillosaDrury), test method is with reference to " the agricultural industry criteria NY/T1154.1-2006 of the People's Republic of China (PRC) ".At first single agent and each Mixed Pharmacy are provided with 5 variable concentrations gradients, the concentration gradient of fluorine pyridine worm amine nitrile is 1ug/g, 2ug/g, 4ug/g, 8ug/g, 16ug/g, and the concentration gradient of butene-fipronil and mixture is 0.25ug/g, 0.5ug/g, 1ug/g, 2ug/g, 4ug/g; The examination worm is the stinkbug silk worm that picks up from the field, and the test of selecting uniformity in the laboratory places culture dish standby, examination worm in the culture dish is carried out drop by head handle, and every drop medicament 0.06ug/L checked behind the medicine and calculates lethality by dead borer population in 24 hours.Carry out statistical analysis with DPS data processor software, calculate the LC of each medicament 50Value is estimated the activity of reagent agent to the examination worm with this.
Figure 435147DEST_PATH_IMAGE011
10) cotton aphid (Aphis gossypii G10ver), test method is with reference to " the agricultural industry criteria NY/T1154.7-2006 of the People's Republic of China (PRC) ".
Figure 271384DEST_PATH_IMAGE012
11) cotton green plant bug (Lygocoris lucor μ m), test method is with reference to " the agricultural industry criteria NY/T1154.1-2006 of the People's Republic of China (PRC) ".
Figure 136572DEST_PATH_IMAGE013
From table 1-11 as can be seen, fluorine pyridine worm amine nitrile and butene-fipronil composite (1:8)~(8:1), rice hoppers, weevil, snout moth's larva, vegetable aphid, trialeurodes vaporariorum, flea beetle, thrips, cotton aphid, stinkbug silk worm, oranges and tangerines aphid, lichee stinkbug silk worm are all had very high synergistic effect, and co-toxicity coefficient is between 125~270.
Below in conjunction with embodiment content of the present invention is described further.
Example of formulations 1
Take by weighing 40% fluorine pyridine worm amine nitrile, 5% butene-fipronil, 4% TERSPERSE 2700(polycarboxylate, U.S. Huntsman Corporation produces), 2% dispersing agent NNO (alkylnaphthalene sulfonate formaldehyde condensation products), 1% Nekal BX (nekal), 1% K-12(lauryl sodium sulfate), 3% soluble starch, 5% glucose, kaolin add to 100% weight portion.The method of the frequent regulation of above-mentioned raw materials water intaking dispersible granule is promptly mixed, ultra micro comminution by gas stream, mixing, granulation step are produced 45% fluorine pyridine worm amine nitrile butene-fipronil water dispersible granules.
The part by weight of fluorine pyridine worm amine nitrile and butene-fipronil can change between 8:1~1:8 in the present embodiment, and both total weight items still are 45%, form new embodiment.
Example of formulations 2
Take by weighing 40% fluorine pyridine worm amine nitrile, 10% butene-fipronil, 3% TERSPERSE 2700,4% sodium lignin sulfonate, 1% Nekal BX, 1%K-12,1% carboxymethyl cellulose, 5% urea, diatomite and add to 100% weight portion.The method of the frequent regulation of above-mentioned raw materials water intaking dispersible granule is promptly mixed, ultra micro comminution by gas stream, mixing, granulation step are produced 50% fluorine pyridine worm amine nitrile butene-fipronil water dispersible granules.
The part by weight of fluorine pyridine worm amine nitrile and butene-fipronil can change between 8:1~1:8 in the present embodiment, and both total weight items still are 50%, form new embodiment.
Example of formulations 3
Take by weighing 60% fluorine pyridine worm amine nitrile, 20% butene-fipronil, 3% TERSPERSE 2700,3%TERSPERSE 2425,1% Nekal BX, 1%K-12,0.8% dextrin, 5% ammonium sulfate, attapulgite and add to 100% weight portion.The method of the frequent regulation of above-mentioned raw materials water intaking dispersible granule is promptly mixed, ultra micro comminution by gas stream, mixing, granulation step are produced 80% fluorine pyridine worm amine nitrile butene-fipronil water dispersible granules.
The part by weight of fluorine pyridine worm amine nitrile and butene-fipronil can change between 8:1~1:8 in the present embodiment, and both total weight items still are 80%, form new embodiment.
Example of formulations 4:
Take by weighing 6% fluorine pyridine worm amine nitrile, 48% butene-fipronil, 4% Morwet D-425(alkylnaphthalene sulfonate, Akzo Nobel N.V. produces), 3% sodium lignin sulfonate, 2% Nekal BX, 2%K-12,1% polyvinylpyrrolidone, 10% sodium sulphate, diatomite add to 100% weight portion.The method of the frequent regulation of above-mentioned raw materials water intaking dispersible granule is promptly mixed, ultra micro comminution by gas stream, mixing, granulation step are produced 54% fluorine pyridine worm amine nitrile butene-fipronil water dispersible granules.
The part by weight of fluorine pyridine worm amine nitrile and butene-fipronil can change between 8:1~1:8 in the present embodiment, and both total weight items still are 54%, form new embodiment.
Example of formulations 5
Take by weighing 50% fluorine pyridine worm amine nitrile, 10% butene-fipronil, 5% calcium lignosulfonate, 3% Morwet D-425,2% Nekal BX, 1%K-12,3% white carbon black, kaolin and add to 100% weight portion.Above-mentioned raw materials makes 60% fluorine pyridine worm amine nitrile butene-fipronil wetting powder through mixing behind the comminution by gas stream.
The part by weight of fluorine pyridine worm amine nitrile and butene-fipronil can change between 8:1~1:8 in the present embodiment, and both total weight items still are 60%, form new embodiment.
Example of formulations 6
Take by weighing 20% fluorine pyridine worm amine nitrile, 10% butene-fipronil, 4% calcium lignosulfonate, 3% TERSPERSE 2700,2% Nekal BX, 1%K-12, precipitated calcium carbonate and add to 100% weight portion.Above-mentioned raw materials makes 30% fluorine pyridine worm amine nitrile butene-fipronil wetting powder through mixing behind the comminution by gas stream.
The part by weight of fluorine pyridine worm amine nitrile and butene-fipronil can change between 8:1~1:8 in the present embodiment, and both total weight items still are 30%, form new embodiment.
Example of formulations 7
Take by weighing 10% fluorine pyridine worm amine nitrile, 20% butene-fipronil, 4% sodium lignin sulfonate, 4% dispersing agent NNO, 2% Nekal BX, 2%K-12,5% white carbon black, attapulgite and add to 100% weight portion.Above-mentioned raw materials makes 30% fluorine pyridine worm amine nitrile butene-fipronil wetting powder through mixing behind the comminution by gas stream.
The part by weight of fluorine pyridine worm amine nitrile and butene-fipronil can change between 8:1~1:8 among the embodiment, and both total weight items still are 30%, form new embodiment.
Example of formulations 8
Take by weighing 5% fluorine pyridine worm amine nitrile, 20% butene-fipronil, 4% sodium lignin sulfonate, 2% TERSPERSE 2700,2%K-12,10% ammonium sulfate, potter's clay and add to 100% weight portion.Above-mentioned raw materials makes 25% fluorine pyridine worm amine nitrile butene-fipronil wetting powder through mixing behind the comminution by gas stream.
The part by weight of fluorine pyridine worm amine nitrile and butene-fipronil can change between 8:1~1:8 in the present embodiment, and both total weight items still are 25%, form new embodiment.
Example of formulations 9
Take by weighing 25% fluorine pyridine worm amine nitrile, 15% butene-fipronil, 3%TERSPERSE 4894,2%TERSPERSE 2500,1%TERSPERSE 2425,0.2% xanthans, 5% ethylene glycol, 0.3% benzoic acid, 0.5% silicone defoaming agent (trade name: s-29 Nanjing "four news" (new ideas applied chemistry product company produces), deionized water adds to 100% weight portion.Above-mentioned raw materials is through mixing, and high speed shear is disperseed 30min, with making 40% fluorine pyridine worm amine nitrile butene-fipronil suspending agent behind the sand mill sand milling.
The part by weight of fluorine pyridine worm amine nitrile and butene-fipronil can change between 8:1~1:8 in the present embodiment, and both total weight items still are 40%, form new embodiment.
Example of formulations 10:
Take by weighing 20% fluorine pyridine worm amine nitrile, 5% butene-fipronil, 1.5%NNO(alkylnaphthalene sulfonate formaldehyde condensation products), 1%TERSPERSE 2500,2% Tween-60 #, 3% Nongru-700 #, 0.1% xanthans, 5% propane diols, 0.5% formaldehyde, 0.3% silicone defoaming agent s-29, deionized water adds to 100% weight portion.Above-mentioned raw materials is through mixing, and high speed shear is disperseed 30min, with making 25% fluorine pyridine worm amine nitrile butene-fipronil suspending agent behind the sand mill sand milling.
The part by weight of fluorine pyridine worm amine nitrile and butene-fipronil can change between 8:1~1:8 in the present embodiment, and both total weight items still are 25%, form new embodiment.
Example of formulations 11:
Take by weighing 20% fluorine pyridine worm amine nitrile, 15% butene-fipronil, 3%TERSPERSE 4894,2% octylphenol polyethylene oxyethylene group (10EO) ether phosphate (alkylphenol-polyethenoxy base ether phosphate), 1%TERSPERSE 2425,0.2% xanthans, 1% aluminium-magnesium silicate, 5% ethylene glycol, 0.3% Sodium Benzoate, 0.5% silicone defoaming agent s-29, deionized water adds to 100% weight portion.Above-mentioned raw materials is through mixing, and high speed shear is disperseed 30min, with making 35% fluorine pyridine worm amine nitrile butene-fipronil suspending agent behind the sand mill sand milling.
The part by weight of fluorine pyridine worm amine nitrile and butene-fipronil can change between 8:1~1:8 in the present embodiment, and both total weight items still are 35%, form new embodiment.
Example of formulations 12:
Take by weighing 10% fluorine pyridine worm amine nitrile, 10% butene-fipronil, 3% Nongru-700 #, 2% agricultural newborn 1601#, 1.5%TERSPERSE 2500,1.5%TERSPERSE 2425,0.2% xanthans, 5% ethylene glycol, 0.3% benzoic acid, 0.5% silicone defoaming agent s-29, deionized water adds to 100% weight portion.Above-mentioned raw materials is through mixing, and high speed shear is disperseed 30min, with making 20% fluorine pyridine worm amine nitrile butene-fipronil suspending agent behind the sand mill sand milling.
The part by weight of fluorine pyridine worm amine nitrile and butene-fipronil can change between 8:1~1:8 in the present embodiment, and both total weight items still are 20%, form new embodiment.
Example of formulations 13
Take by weighing 10% fluorine pyridine worm amine nitrile, 5% butene-fipronil, 2%TERSPERSE 2425,4% this dish-60#, 3% Tween-60 #, 4% agricultural newborn 2201#, 3% Nongru-700 #, 1%TERSPERSE 2500,0.5% white carbon, 5% propane diols, 1% epoxychloropropane, methyl oleate and add to 100% weight portion.Above-mentioned raw materials is through mixing, and high speed shear is disperseed 30min, but with making 15% fluorine pyridine worm amine nitrile butene-fipronil dispersed oil suspending agent behind the sand mill sand milling.
The part by weight of fluorine pyridine worm amine nitrile and butene-fipronil can change between 8:1~1:8 among the embodiment, and both total weight items still are 15%, form new embodiment.
Example of formulations 14
Take by weighing 15% fluorine pyridine worm amine nitrile, 5% butene-fipronil, 2% dispersing agent NNO, 3% agricultural newborn 2201#, 10% BY-110,1%TERSPERSE 2500,1% aluminium-magnesium silicate, 3% glycerine, 15% epoxidized soybean oil, soybean oil and add to 100% weight portion.Above-mentioned raw materials is through mixing, and high speed shear is disperseed 30min, but with making 20% fluorine pyridine worm amine nitrile butene-fipronil dispersed oil suspending agent behind the sand mill sand milling.
The part by weight of fluorine pyridine worm amine nitrile and butene-fipronil can change between 8:1~1:8 among the embodiment, and both total weight items still are 20%, form new embodiment.
Example of formulations 15
Take by weighing 10% fluorine pyridine worm amine nitrile, 8% butene-fipronil, 1.5%TERSPERSE 2425,3% this dish-60#, 3% Tween-60 #, 8% BY-110,1%TERSPERSE 2500,0.5% white carbon, 5% propane diols, 20% epoxidized soybean oil, methyl oleate and add to 100% weight portion.Above-mentioned raw materials is through mixing, and high speed shear is disperseed 30min, but with making 18% fluorine pyridine worm amine nitrile butene-fipronil dispersed oil suspending agent behind the sand mill sand milling.
The part by weight of fluorine pyridine worm amine nitrile and butene-fipronil can change between 8:1~1:8 among the embodiment, and both total weight items still are 18%, form new embodiment.
Example of formulations 16
Take by weighing 20% fluorine pyridine worm amine nitrile, 2.5% butene-fipronil, 1% dispersing agent NNO, 5% BY-125,3% this dish-60#, 3% Tween-60 #, 4% agricultural newborn 1601#, 1% phenethyl phenol polyethenoxy base ether phosphate, 0.5% bentonite, 5% glycerine, 3% triphenyl phosphate, rapeseed oil and add to 100% weight portion.Above-mentioned raw materials is through mixing, and high speed shear is disperseed 30min, but with making 22.5% fluorine pyridine worm amine nitrile butene-fipronil dispersed oil suspending agent behind the sand mill sand milling.
The part by weight of fluorine pyridine worm amine nitrile and butene-fipronil can change between 8:1~1:8 among the embodiment, and both total weight items still are 22.5%, form new embodiment.
Example of formulations 17
Take by weighing 5% fluorine pyridine worm amine nitrile, 10% butene-fipronil, 1%TERSPERSE 2425,4% agricultural newborn 2201#, 2% Nongru-700 #, 5% BY-110,1%TERSPERSE 2500,1.5% aluminium-magnesium silicate, 5% propane diols, 20% epoxidized soybean oil, methyl oleate and add to 100% weight portion.Above-mentioned raw materials is through mixing, and high speed shear is disperseed 30min, but with making 15% fluorine pyridine worm amine nitrile butene-fipronil dispersed oil suspending agent behind the sand mill sand milling.
The part by weight of fluorine pyridine worm amine nitrile and butene-fipronil can change between 8:1~1:8 among the embodiment, and both total weight items still are 15%, form new embodiment.
Example of formulations 18
Take by weighing 5% fluorine pyridine worm amine nitrile, 2.5% butene-fipronil, 4%TX-10,5% Nongru-700 #, 6% agricultural newborn 500#, 4% agricultural newborn 1601#, 15% cyclohexanone, 5%N-methyl pyrrolidone, 5% n-butanol, through dissolving fully and mixing, deionized water adds to 100% weight portion, makes 7.5% fluorine pyridine worm amine nitrile butene-fipronil microemulsion after the stirring.
The part by weight of fluorine pyridine worm amine nitrile and butene-fipronil can change between 8:1~1:8 among the embodiment, and both total weight items still are 7.5%, form new embodiment.
Example of formulations 19
Take by weighing 9% fluorine pyridine worm amine nitrile, 3% butene-fipronil, 5% agricultural newborn 400#, 4% agricultural newborn 500#, 6% agricultural newborn 1601#, 25% cyclohexanone, 5% dimethylbenzene, 5% isopropyl alcohol, through dissolving fully and mixing, deionized water adds to 100% weight portion, makes 12% fluorine pyridine worm amine nitrile butene-fipronil microemulsion after the stirring.
The part by weight of fluorine pyridine worm amine nitrile and butene-fipronil can change between 8:1~1:8 among the embodiment, and both total weight items still are 12%, form new embodiment.
Example of formulations 20
Take by weighing 2% fluorine pyridine worm amine nitrile, 5% butene-fipronil, 6% agricultural newborn 2201#, 5% Nongru-700 #, 6% agricultural newborn 600#, 10% cyclohexanone, 5%N-methyl pyrrolidone, 5% toluene, 5% ethanol, through dissolving fully and mixing, deionized water adds to 100% weight portion, makes 7% fluorine pyridine worm amine nitrile butene-fipronil microemulsion after the stirring.
The part by weight of fluorine pyridine worm amine nitrile and butene-fipronil can change between 8:1~1:8 among the embodiment, and both total weight items still are 7%, form new embodiment.
Example of formulations 21
Take by weighing 1% fluorine pyridine worm amine nitrile, 5% butene-fipronil, 4%TX-10,8% agricultural newborn 600#, 6% agricultural newborn 500#, 20% cyclohexanone, 5%N-methyl pyrrolidone, 5% toluene, through dissolving fully and mixing, deionized water adds to 100% weight portion, makes 6% fluorine pyridine worm amine nitrile butene-fipronil microemulsion after the stirring.
The part by weight of fluorine pyridine worm amine nitrile and butene-fipronil can change between 8:1~1:8 among the embodiment, and both total weight items still are 6%, form new embodiment.
Example of formulations 22
Take by weighing 8% fluorine pyridine worm amine nitrile, 4% butene-fipronil, 4% agricultural newborn 500#, 2% agricultural newborn 600#, 3% agricultural newborn 2201#, 3% triphenyl phosphite, 15% dimethyl formamide, dimethylbenzene add to 100% weight portion.Above-mentioned raw materials makes 12% fluorine pyridine worm amine nitrile butene-fipronil missible oil after mix, stirring and dissolving is complete.
The part by weight of fluorine pyridine worm amine nitrile and butene-fipronil can change between 8:1~1:8 among the embodiment, and both total weight items still are 12%, form new embodiment.
Example of formulations 23
Take by weighing 10% fluorine pyridine worm amine nitrile, 6% butene-fipronil, 4% agricultural newborn 500#, 3% agricultural newborn 400#, 5% agricultural newborn 1601#, 1% epoxychloropropane, 15% ethyl acetate, 10% acetone, S-150 and add to 100% weight portion.Above-mentioned raw materials makes 16% fluorine pyridine worm amine nitrile butene-fipronil missible oil after mix, stirring and dissolving is complete.
The part by weight of fluorine pyridine worm amine nitrile and butene-fipronil can change between 8:1~1:8 among the embodiment, and both total weight items still are 16%, form new embodiment.
Example of formulations 24
Take by weighing 5% fluorine pyridine worm amine nitrile, 5% butene-fipronil, 4% this dish-60#, 3% Tween-60 #, 5% agricultural newborn 2201#,, 1% epoxychloropropane, 10% cyclohexanone, 10% dimethyl sulfoxide (DMSO), biodiesel add to 100% weight portion.Above-mentioned raw materials makes 10% fluorine pyridine worm amine nitrile butene-fipronil missible oil after mix, stirring and dissolving is complete.
The part by weight of fluorine pyridine worm amine nitrile and butene-fipronil can change between 8:1~1:8 among the embodiment, and both total weight items still are 10%, form new embodiment.
Example of formulations 25
Take by weighing 2% fluorine pyridine worm amine nitrile, 8% butene-fipronil, 4% agricultural newborn 500#, 3% agricultural newborn 1601#, 3% agricultural newborn 2201#, 3% triphenyl phosphite, 15% methyl alcohol, 10% dimethyl formamide, toluene add to 100% weight portion.Above-mentioned raw materials makes 10% fluorine pyridine worm amine nitrile butene-fipronil missible oil after mix, stirring and dissolving is complete.
The part by weight of fluorine pyridine worm amine nitrile and butene-fipronil can change between 8:1~1:8 among the embodiment, and both total weight items still are 10%, form new embodiment.
Biological Examples 1: prevent and treat the rice hoppers field trial
The inventor prevents and treats the field control effectiveness test of rice hoppers at 80% fluorine pyridine worm amine nitrile butene-fipronil (60+20) water dispersible granules that Sichuan Province's Guangyuan City carries out example of formulations 3, verified that this medicament is to the control efficiency of rice hoppers, effective dose and to the safety of paddy rice.Trial crops is a paddy rice, the controlling object rice hoppers.Test medicine and dosage are 80% fluorine pyridine worm amine nitrile butene-fipronil water dispersible granules mu consumption, 3 grams, 4 grams, 5 grams, 22% fluorine pyridine worm amine nitrile suspending agent, 20 gram/mus, and 5% butene-fipronil missible oil, 40 gram/mus adopt conventional spray-on process.Investigation insect population radix before the dispenser, 3d, 7d behind the medicine, 14d, investigate residual borer population alive respectively, take the random sampling of balance great-jump-forward, 10 every 2 clumps of every sub-districts (totally 20 clumps) during investigation, with basin bat method record rice fulgorid borer population, by before the every clump of medicine, the borer population calculation correction preventive effect behind the medicine, and carry out the significance of difference and measure.2,7,14 days observation paddy growth situations behind medicine are estimated reagent agent and are had or not poisoning to produce to paddy rice simultaneously.
Figure 901528DEST_PATH_IMAGE014
In the formula: Pt 0Before-----treatment region medicine; Pt 1Behind-----treatment region medicine
CK 0Before the medicine of-----check plot; CK 1Behind the medicine of-----check plot
Figure 484956DEST_PATH_IMAGE015
Table 12 for behind the medicine the 14th day the time each sub-district preventive effect carry out the biostatistics analysis, analysis result shows: handle differences and reach utmost point significance level, district's group difference is not remarkable.Significance of difference comparative result shows: consistent with the significance of difference on 0.01 level on 0.05 level, 80% fluorine pyridine worm amine nitrile butene-fipronil water dispersible granules, 4 gram/mus, 5 gram/mus are respectively handled differences with other and are all reached utmost point significance level, and comparing difference is not remarkable between 80% fluorine pyridine worm amine nitrile butene-fipronil water dispersible granules 3 gram/mus and contrast medicament 22% fluorine pyridine worm amine nitrile suspending agent 20 gram/mus, 2 processing of 5% butene-fipronil missible oil, 40 gram/mus.
Field trial shows: 80% fluorine pyridine worm amine nitrile butene-fipronil water dispersible granules has than remarkable prevention effect rice hoppers, its 4 gram, the control efficiency of 5 grams obviously is better than contrasting medicament 22% fluorine pyridine worm amine nitrile suspending agent 20 gram/mus, the control efficiency of 5% butene-fipronil missible oil, 40 gram/mus, its mu restrains and 22% fluorine pyridine worm amine nitrile suspending agent, 20 gram/mus with 3, the control efficiency of 5% butene-fipronil missible oil, 40 gram/mus is suitable, after result of the test shows that fluorine pyridine worm amine nitrile and butene-fipronil are mixed, quick-acting and lasting period have obviously been improved to rice hoppers, greatly reduce dosage, to paddy growth safety.
Biological Examples 2: control paddy rice weevil field trial
The inventor carried out the field control effectiveness test of 25% fluorine pyridine worm amine nitrile butene-fipronil (20+5) the suspending agent control paddy rice water weevil in the example of formulations 10 on May 11st, 2010 in the ChangSha, Hunan Province county, verified that this medicament is to the control efficiency of paddy rice water weevil, effective dose and to the safety of paddy rice.Trial crops is a paddy rice, controlling object paddy rice water weevil.Test medicine and dosage are 25% fluorine pyridine worm amine nitrile butene-fipronil suspending agent mu consumption, 9 grams, 12 grams, 15 grams, 22% fluorine pyridine worm amine nitrile suspending agent, 15 gram/mus, 5% butene-fipronil missible oil, 30 gram/mus, adopt conventional spray-on process. investigation insect population radix before the dispenser, 3d, 14d behind the medicine, investigate residual borer population alive respectively, take 5 point samplings, investigate 10 clumps at every, 50 clumps of every sub-district investigation, by before every clump of medicine, the borer population calculation correction preventive effect behind the medicine, and carry out the significance of difference and measure.3,14 days observation paddy growth situations behind medicine are estimated reagent agent and are had or not poisoning to produce to paddy rice simultaneously.
Figure 859306DEST_PATH_IMAGE016
Table 13 for behind the medicine the 14th day the time each sub-district preventive effect carry out the biostatistics analysis, analysis result shows: handle differences and reach utmost point significance level, district's group difference is not remarkable.Significance of difference comparative result shows: consistent with the significance of difference on 0.01 level on 0.05 level, 25% fluorine pyridine worm amine nitrile butene-fipronil suspending agent mu is respectively handled differences with 12 grams with other with 15 grams, mu and is all reached utmost point significance level, and 25% fluorine pyridine worm amine nitrile butene-fipronil suspending agent mu is not remarkable with comparing difference between 15 grams, 3 processing in twos of 5% butene-fipronil missible oil, 30 gram/mus with 9 grams and contrast medicament 22% fluorine pyridine worm amine nitrile suspending agent mu.
Field trial shows: 25% fluorine pyridine worm amine nitrile butene-fipronil suspending agent has than remarkable prevention effect the paddy rice water weevil, and the control efficiency of its mu usefulness 12 grams, 15 grams obviously is better than contrasting the control efficiency of medicament 22% fluorine pyridine worm amine nitrile suspending agent 15 gram/mus, 5% butene-fipronil missible oil, 30 gram/mus.Its mu usefulness 9 grams are suitable with the control efficiency of 22% fluorine pyridine worm amine nitrile suspending agent, 15 gram/mus, 5% butene-fipronil missible oil, 30 gram/mus, after result of the test shows that fluorine pyridine worm amine nitrile and butene-fipronil are mixed, quick-acting and lasting period have obviously been improved to the paddy rice water weevil, greatly reduce dosage, to paddy growth safety.
Biological Examples 3: control rice-stem borer field trial
The inventor on June 27th, 2010 carried out 15% fluorine pyridine worm amine nitrile butene-fipronil (10+5) in the example of formulations 13 in the Hengdong County, Hunan Province but the field control effectiveness test of dispersed oil suspending agent control rice-stem borer has verified that this medicament is to the control efficiency of rice-stem borer, effective dose and to the safety of paddy rice.Trial crops is a paddy rice, the controlling object rice-stem borer.But test medicine and dosage are 15% fluorine pyridine worm amine nitrile butene-fipronil dispersed oil suspending agent mu consumption, 20 grams, 25 grams, 30 grams, 22% fluorine pyridine worm amine nitrile suspending agent, 20 gram/mus, 5% butene-fipronil missible oil, 40 gram/mus, adopt conventional spray-on process in rice plant of tillering stage, generation striped rice borer egg development is incubated the initial stage to ovum latter stage, adopt the conventional spraying of manual sprayer, 45 liters of every mu of spouting liquids are investigated the control efficiency of each sub-district when generation striped rice borer borer pest is stablized.Take the random sampling of balance great-jump-forward, 25 clumps of rice of every sub-district investigation are added up withered heart rate and lethality.While is 4,10 days observation paddy growth situations behind medicine, and the visual test medicament has or not poisoning to produce to paddy rice.
Computational methods:
Figure 780437DEST_PATH_IMAGE018
In the formula: Pt 0Withered heart rate behind-----chemicals treatment district medicine;
CK 0Withered heart rate behind-----blank district medicine
Figure 851161DEST_PATH_IMAGE019
As can be seen from the above table, fluorine pyridine worm amine nitrile and butene-fipronil combination are composite, incubate the initial stage dispenser in striped rice borer egg development latter stage to ovum and once can effectively control striped rice borer harm, and dosage is less than the contrast dosing, tangible synergistic effect is arranged, can be used for the control of rice-stem borer, and to rice safety.
Biological Examples 4: the field control effectiveness test of the yellow bent flea beetle of control cauliflower
The inventor carried out the field control effectiveness test of the yellow bent flea beetle of 7.5% fluorine pyridine worm amine nitrile butene-fipronil (5+2.5) microemulsion control cauliflower in the example of formulations 18 on September 21st, 2010 in the Shantou City, Guangdong Province, verified that this medicament is to the control efficiency of the yellow bent flea beetle of cauliflower, effective dose and to the safety of cauliflower.Trial crops is a cauliflower, the yellow bent flea beetle of controlling object cauliflower.Test medicine and dosage are 7.5% fluorine pyridine worm amine nitrile butene-fipronil microemulsion mu consumption, 40 grams, 50 grams, 60 grams, 22% fluorine pyridine worm amine nitrile suspending agent, 30 gram/mus, 5% butene-fipronil missible oil, 40 gram/mus, adopt conventional spray-on process. investigation insect population radix before the dispenser, 2d, 14d investigate residual borer population alive respectively behind the medicine, take accidental sampling, and 20 strains are investigated in every sub-district, by before the every clump of medicine, the borer population calculation correction preventive effect behind the medicine, and carry out the significance of difference and measure.2,14 days observation cauliflower growing states behind medicine are estimated reagent agent and are had or not poisoning to produce to cauliflower simultaneously.
Figure 904567DEST_PATH_IMAGE020
Table 15 for behind the medicine the 14th day the time each sub-district preventive effect carry out the biostatistics analysis, analysis result shows: handle differences and reach utmost point significance level, district's group difference is not remarkable.Significance of difference comparative result shows: consistent with the significance of difference on 0.01 level on 0.05 level, 7.5% fluorine pyridine worm amine nitrile butene-fipronil microemulsion, 50 gram/mus, 60 gram/mus are respectively handled differences with other and are all reached utmost point significance level, and comparing difference is not remarkable between 7.5% fluorine pyridine worm amine nitrile butene-fipronil microemulsion 40 gram/mus and contrast medicament 22% fluorine pyridine worm amine nitrile suspending agent 30 gram/mus, 3 processing in twos of 5% butene-fipronil missible oil, 40 gram/mus.
Field trial shows: 7.5% fluorine pyridine worm amine nitrile butene-fipronil microemulsion has than remarkable prevention effect the yellow bent flea beetle of cauliflower, and the control efficiency of its 50 gram, 60 grams obviously is better than contrasting the control efficiency of medicament 22% fluorine pyridine worm amine nitrile suspending agent 30 gram/mus, 5% butene-fipronil missible oil, 40 gram/mus.Its mu usefulness 40 grams are suitable with the control efficiency of 22% fluorine pyridine worm amine nitrile suspending agent, 30 gram/mus, 5% butene-fipronil missible oil, 40 gram/mus, after result of the test shows that fluorine pyridine worm amine nitrile and butene-fipronil are mixed, quick-acting and lasting period have obviously been improved to the yellow bent flea beetle of cauliflower, greatly reduce dosage, to cauliflower growth safety.
Biological Examples 5: the field control effectiveness test of control tomato trialeurodes vaporariorum
Carried out the field control effectiveness test of 40% fluorine pyridine worm amine nitrile butene-fipronil suspending agent (25+15) the control tomato trialeurodes vaporariorum in the example of formulations 9 in the Wugong County, Shaanxi Province, verified that this medicament is to the control efficiency of tomato trialeurodes vaporariorum, effective dose and to the safety of tomato.Trial crops is a tomato, controlling object tomato trialeurodes vaporariorum.Test medicine and dosage are 40% fluorine pyridine worm amine nitrile butene-fipronil suspending agent, 6 gram/mus, 8 gram/mus, 10 gram/mus, 22% fluorine pyridine worm amine nitrile suspending agent, 25 gram/mus, and 5% butene-fipronil missible oil, 40 gram/mus adopt conventional spray-on process.Each sub-district is selected 5 points at random before the test, every point selection is easy to tomato 2 strains of observation survey, and use red line mark, the trialeurodes vaporariorum of estimating on the whole blades of every strain tomato at 0.5 meter of plant of mark becomes borer population, this is the insect population radix, 1 d, 3d, 7d investigate the plant of mark behind the medicine, carry out the control efficiency statistics.
Figure 868981DEST_PATH_IMAGE021
Table 16 for behind the medicine the 7th day the time each sub-district preventive effect carry out the biostatistics analysis, analysis result shows: handle differences and reach extremely outstanding level, district's group difference is not remarkable.Significance of difference comparative result shows: consistent with the significance of difference on 0.01 level on 0.05 level, 40% fluorine pyridine worm amine nitrile butene-fipronil suspending agent, 10 gram/mus, 8 gram/mus are respectively handled differences with other and are all reached utmost point significance level, 40% fluorine pyridine worm amine nitrile butene-fipronil suspending agent, 6 gram/mus are suitable with contrast medicament 22% fluorine pyridine worm amine nitrile suspending agent 25 gram/mus, and are extremely remarkable with 5% butene-fipronil missible oil, 40 gram/mus processing differences.
Field trial shows: 40% fluorine pyridine worm amine nitrile butene-fipronil suspending agent has than remarkable prevention effect the tomato trialeurodes vaporariorum, 8 gram/mus, the control efficiency of 10 gram/mus obviously is better than contrasting medicament 22% fluorine pyridine worm amine nitrile suspending agent 25 gram/mus, the control efficiency of 5% butene-fipronil missible oil, 40 gram/mus, its 6 gram/mu is suitable with 22% fluorine pyridine worm amine nitrile suspending agent, 25 gram/mus, the control efficiency that obviously is better than 5% butene-fipronil missible oil, 40 gram/mus, after result of the test shows that fluorine pyridine worm amine nitrile and butene-fipronil are mixed, obviously improved control efficiency to the tomato trialeurodes vaporariorum, greatly reduce dosage, to tomato growth safety.
Biological Examples 6: the field control effectiveness test of control cabbage aphid
Carried out the field control effectiveness test of 60% fluorine pyridine worm amine nitrile butene-fipronil (50+10) the wetting powder control cabbage aphid in the example of formulations 5 in the Xiamen City, Fujian Province, verified that this medicament is to the control efficiency of cabbage aphid, effective dose and to the safety of wild cabbage.Trial crops is a wild cabbage, the controlling object cabbage aphid.Test medicine and dosage are 60% fluorine pyridine worm amine nitrile butene-fipronil wetting powder, 3 gram/mus, 4 gram/mus, 5 gram/mus, 22% fluorine pyridine worm amine nitrile suspending agent, 15 gram/mus, and 5% butene-fipronil missible oil, 20 gram/mus adopt conventional spray-on process.Investigation insect population radix before the dispenser, 1d, 3d, 7d investigate residual borer population alive respectively behind the medicine, and 5 samplings in every sub-district during investigation are fixed the investigation of 2 strain wild cabbages at every, and investigation is the aphid number on the strain blade fixedly, and the record borer population of living carries out control efficiency and adds up.
Figure 349641DEST_PATH_IMAGE022
Table 17 for behind the medicine the 7th day the time each sub-district preventive effect carry out the biostatistics analysis, analysis result shows: handle differences and reach extremely outstanding level, district's group difference is not remarkable.Significance of difference comparative result shows: consistent with the significance of difference on 0.01 level on 0.05 level, it is extremely remarkable that 60% fluorine pyridine worm amine nitrile butene-fipronil wetting powder, 4 gram/mus, 5 gram/mus are handled difference, its 3 gram/mu is suitable with contrast medicament 22% fluorine pyridine worm amine nitrile suspending agent 15 gram/mus, and 5% butene-fipronil missible oil, 20 gram/mus processing differences remarkable.
Field trial shows: 60% fluorine pyridine worm amine nitrile butene-fipronil wetting powder has remarkable prevention effect to cabbage aphid, and the control efficiency of its 4 gram/mu, 5 gram/mus obviously is better than contrasting the control efficiency of medicament 22% fluorine pyridine worm amine nitrile suspending agent 15 gram/mus, 5% butene-fipronil missible oil, 20 gram/mus.Result of the test shows: after fluorine pyridine worm amine nitrile and butene-fipronil are mixed, obviously improved the quick-acting and lasting period to cabbage aphid, reduced dosage and drug cost, to wild cabbage growth safety.
Biological Examples 7: the field control effectiveness test of control cucumber thrips
Carried out the field control effectiveness test of 12% fluorine pyridine worm amine nitrile butene-fipronil (8+4) the missible oil control cucumber thrips in the example of formulations 22 in the Xiamen City, Fujian Province, verified that this medicament is to the control efficiency of cucumber thrips, effective dose and to the safety of cucumber.Trial crops is a cucumber, controlling object cucumber thrips.Test medicine and dosage are 12% fluorine pyridine worm amine nitrile butene-fipronil missible oil, 20 gram/mus, 30 gram/mus, 40 gram/mus, 22% fluorine pyridine worm amine nitrile suspending agent, 25 gram/mus, and 5% butene-fipronil missible oil, 40 gram/mus adopt conventional spray-on process.Investigation insect population radix before the dispenser, 3d, 7d investigate residual borer population alive respectively behind the medicine, and 5 samplings in every sub-district during investigation are fixed the investigation of 2 strain cucumber at every, and investigation is the thrips number on the strain blade fixedly, and the record borer population of living carries out control efficiency and adds up.
Figure 268181DEST_PATH_IMAGE024
Table 18 for behind the medicine the 7th day the time each sub-district preventive effect carry out the biostatistics analysis, analysis result shows: handle differences and reach extremely outstanding level, district's group difference is not remarkable.Significance of difference comparative result shows: consistent with the significance of difference on 0.01 level on 0.05 level, it is extremely remarkable that 12% fluorine pyridine worm amine nitrile butene-fipronil missible oil, 30 gram/mus, 40 gram/mus are handled difference, its 20 gram/mu and contrast medicament 22% fluorine pyridine worm amine nitrile suspending agent 25 gram/mus, 5% butene-fipronil missible oil, 40 gram/mu differences are not remarkable.
Field trial shows: 12% fluorine pyridine worm amine nitrile butene-fipronil missible oil has remarkable prevention effect to the cucumber thrips, and the control efficiency of its 30 gram/mu, 40 gram/mus obviously is better than contrasting the control efficiency of medicament 22% fluorine pyridine worm amine nitrile suspending agent 25 gram/mus, 5% butene-fipronil missible oil, 40 gram/mus.Result of the test shows: after fluorine pyridine worm amine nitrile and butene-fipronil are mixed, obviously improved the quick-acting and lasting period to the cucumber thrips, reduced dosage and drug cost, to cucumber growth safety.
Biological Examples 8: the field control effectiveness test of control oranges and tangerines aphid
Carried out the field control effectiveness test of 16% fluorine pyridine worm amine nitrile butene-fipronil (10+6) the missible oil control oranges and tangerines aphid of example of formulations 23 in the Deqing County, Guangdong Province, verified that this medicament is to the control efficiency of oranges and tangerines aphid, effective dose and to the safety of oranges and tangerines.Trial crops is oranges and tangerines, controlling object oranges and tangerines aphid.Test medicine and dosage are 4000 times, 5000 times, 6000 times of 16% fluorine pyridine worm amine nitrile butene-fipronil missible oil, 3000 times of 22% fluorine pyridine worm amine nitrile suspending agents, and 2000 times of 5% butene-fipronil missible oil adopt conventional spray-on process.Investigation insect population radix before the dispenser, 1d, 3d, 7d, 14d investigate residual borer population alive respectively behind the medicine, mark two fruit trees in every sub-district during investigation, every fruit tree is fixed 5 killed tips by all directions, aphid number on the tip blade of investigation top, record borer population alive carries out the control efficiency statistics.
Table 19 for behind the medicine the 7th day the time each sub-district preventive effect carry out the biostatistics analysis, analysis result shows: handle differences and reach extremely outstanding level, district's group difference is not remarkable.Significance of difference comparative result shows: consistent with the significance of difference on 0.01 level on 0.05 level, it is extremely remarkable that 4000 times, 5000 times of 16% fluorine pyridine worm amine nitrile butene-fipronil missible oil are handled difference, its and its 6000 times of processing, contrast medicament 22% 3000 times of fluorine pyridine worm amine nitrile suspending agents, 2000 times of processing of 5% butene-fipronil missible oil differences is remarkable.
Field trial shows: 16% fluorine pyridine worm amine nitrile butene-fipronil missible oil has remarkable prevention effect to the oranges and tangerines aphid, and its 4000 times, 5000 times control efficiency obviously is better than contrasting the control efficiency of medicament 22% 3000 times of fluorine pyridine worm amine nitrile suspending agents, 2000 times of 5% butene-fipronil missible oil.Result of the test shows: after fluorine pyridine worm amine nitrile and butene-fipronil are mixed, obviously improved quick-acting and lasting period, reduced dosage and drug cost, to oranges and tangerines growth safety.
Biological Examples 9: the field control effectiveness test of control lichee stinkbug silk worm
But carried out the field control effectiveness test of 20 % fluorine pyridine worm amine nitrile butene-fipronil dispersed oil suspending agents (15+5) the control lichee stinkbug silk worm in the example of formulations 14 in the Longyan, Fujian Province, verified that this medicament is to the control efficiency of lichee stinkbug silk worm, effective dose and to the safety of lichee.Trial crops is a lichee, controlling object lichee stinkbug silk worm.But test medicine and dosage are 3000 times, 4000 times, 5000 times of 20% fluorine pyridine worm amine nitrile butene-fipronil dispersed oil suspending agents, 2000 times of 22% fluorine pyridine worm amine nitrile suspending agents, and 2000 times of 5% butene-fipronil missible oil adopt conventional spray-on process.Investigation insect population radix before the dispenser, 1d, 3d, 7d investigate residual borer population alive respectively behind the medicine, and two strains are investigated in every sub-district during investigation, every strain tree is by the nymph on 30 branches of 5 investigation in all directions, borer population in the strain of investigation fixed point, record borer population alive carries out the control efficiency statistics.
Figure 819565DEST_PATH_IMAGE026
Table 20 for behind the medicine the 7th day the time each sub-district preventive effect carry out the biostatistics analysis, analysis result shows: handle differences and reach utmost point significance level.Significance of difference comparative result shows: consistent with the significance of difference on 0.01 level on 0.05 level, it is extremely remarkable that but 3000 times, 4000 times of 20% fluorine pyridine worm amine nitrile butene-fipronil dispersed oil suspending agents are handled difference, and to handle differences remarkable with 2000 times of contrast medicament 22% 2000 times of fluorine pyridine worm amine nitrile suspending agents, 5% butene-fipronil missible oil for it.
Field trial shows: but 20% fluorine pyridine worm amine nitrile butene-fipronil dispersed oil suspending agent has remarkable prevention effect to lichee stinkbug silk worm, and its 3000 times, 4000 times control efficiency obviously is better than contrasting the control efficiency of medicament 22% 2000 times of fluorine pyridine worm amine nitrile suspending agents, 2000 times of 5% butene-fipronil missible oil.Result of the test shows: after fluorine pyridine worm amine nitrile and butene-fipronil are mixed, obviously improved quick-acting and lasting period to lichee stinkbug silk worm, reduced dosage and drug cost, to lichee growth safety.
Biological Examples 10: the field control effectiveness test of control cotton aphid
Carried out the field control effectiveness test of 30% fluorine pyridine worm amine nitrile butene-fipronil (20+10) the wetting powder control cotton aphid of example of formulations 6 in Weinan City Dali County, Shaanxi Province, verified that this medicament is to the control efficiency of cotton aphid, effective dose and to the safety of cotton.Trial crops is a cotton, the controlling object cotton aphid.Test medicine and dosage are 30% fluorine pyridine worm amine nitrile butene-fipronil wetting powder, 8 gram/mus, 10 gram/mus, 12 gram/mus, 22% fluorine pyridine worm amine nitrile suspending agent, 20 gram/mus, and 5% butene-fipronil missible oil, 40 gram/mus adopt conventional spray-on process.Investigation insect population radix before the dispenser, 1d, 3d, 7d, 14d investigate residual borer population alive respectively behind the medicine, 5 samplings in every sub-district during investigation, fix the investigation of 2 strain cottons at every, every strain fixedly middle and upper part blade has 5, the aphid number on the investigation fixed blade, record borer population alive carries out the control efficiency statistics.
Figure 595760DEST_PATH_IMAGE027
Table 21 for behind the medicine the 7th day the time each sub-district preventive effect carry out the biostatistics analysis, analysis result shows: handle differences and reach extremely outstanding level, district's group difference is not remarkable.Significance of difference comparative result shows: consistent with the significance of difference on 0.01 level on 0.05 level, it is extremely remarkable that but 30 % fluorine pyridine worm amine nitrile butene-fipronil dispersed oil suspending agents, 8 gram/mus, 10 gram/mus, 12 gram/mus are handled difference, and it is remarkable with contrast medicament 22% fluorine pyridine worm amine nitrile suspending agent 20 gram/mus, 5% butene-fipronil missible oil, 40 gram/mus processing differences.
Field trial shows: but 30% fluorine pyridine worm amine nitrile butene-fipronil dispersed oil suspending agent has remarkable prevention effect to cotton aphid, and the control efficiency of its 8 gram/mu, 10 gram/mus, 12 gram/mus obviously is better than contrasting the control efficiency of medicament 22% fluorine pyridine worm amine nitrile suspending agent 20 gram/mus, 5% butene-fipronil missible oil, 40 gram/mus.Result of the test shows: after fluorine pyridine worm amine nitrile and butene-fipronil are mixed, obviously improved the quick-acting and lasting period to cotton aphid, reduced dosage and drug cost, to cotton growth safety.
Biological Examples 11: control cotton green plant bug field trial
The field control effectiveness test of 20% fluorine pyridine worm amine nitrile butene-fipronil (10+10) suspending agent in the embodiment 12 on July 20 of Anxin County, Hebei province control cotton green plant bug has verified that this medicament is to the control efficiency of cotton green plant bug, effective dose and to the safety of cotton.Trial crops is a cotton, controlling object cotton green plant bug.Test medicine and dosage are 20% fluorine pyridine worm amine nitrile butene-fipronil suspending agent, 8 gram/mus, 10 gram/mus, 12 gram/mus, 22% fluorine pyridine worm amine nitrile suspending agent, 15 gram/mus, and 5% butene-fipronil missible oil, 30 gram/mus adopt conventional spray-on process.Investigate the insect population radix before the dispenser, 1d, 3d, 5 d, 7d investigate residual borer population alive respectively behind the medicine, and 5 samplings in every sub-district during investigation are fixed the investigation of 20 strain cottons at every, the borer population in the strain of investigation fixed point, and record borer population alive carries out the control efficiency statistics.
Figure 641076DEST_PATH_IMAGE028
Table 22 for behind the medicine the 7th day the time each sub-district preventive effect carry out the biostatistics analysis, analysis result shows: handle differences and reach utmost point significance level.Significance of difference comparative result shows: consistent with the significance of difference on 0.01 level on 0.05 level, it is extremely remarkable that 20% fluorine pyridine worm amine nitrile butene-fipronil suspending agent, 10 gram/mus, 8 gram/mus are handled difference, and it is remarkable with contrast medicament 22% fluorine pyridine worm amine nitrile suspending agent 15 gram/mus, 5% butene-fipronil missible oil, 30 gram/mus processing differences.
Field trial shows: 20% fluorine pyridine worm amine nitrile butene-fipronil suspending agent has remarkable prevention effect to the cotton green plant bug, and the control efficiency of its 10 gram/mu, 8 gram/mus obviously is better than contrasting the control efficiency of medicament 22% fluorine pyridine worm amine nitrile suspending agent 15 gram/mus, 5% butene-fipronil missible oil, 30 gram/mus.Result of the test shows: after fluorine pyridine worm amine nitrile and butene-fipronil are mixed, obviously improved quick-acting and lasting period to the cotton green plant bug, reduced dosage and drug cost, to cotton growth safety.
In sum, composition of the present invention is to adopt two kinds of active component compound schemes, its activity and insecticidal effect are not the simple superposition of each composition activity, compare with existing unitary agent, except that having significant insecticidal effect, and significant synergistic effect arranged, slow down the generation of resistance, the preparation less residue, pollution-free to crop, safety is good, meets the security requirement of pesticidal preparations.

Claims (6)

1. the Pesticidal combination of fluorine-containing pyridine worm amine nitrile and butene-fipronil is characterized in that the Pesticidal combination active component is
Fluorine pyridine worm amine nitrile and butene-fipronil, the weight ratio of fluorine pyridine worm amine nitrile and butene-fipronil is 1:8~8:1.
2. the Pesticidal combination of fluorine-containing pyridine worm amine nitrile according to claim 1 and butene-fipronil, it is characterized in that: the content sum of fluorine pyridine worm amine nitrile and butene-fipronil is 1%~80% of a described composition total weight.
3. the Pesticidal combination of fluorine-containing pyridine worm amine nitrile according to claim 2 and butene-fipronil, it is characterized in that: the content sum of fluorine pyridine worm amine nitrile and butene-fipronil is 5%~50% of a described composition total weight.
4. the Pesticidal combination of fluorine-containing pyridine worm amine nitrile according to claim 1 and butene-fipronil, it is characterized in that: described composition is water dispersible granules, wetting powder, suspending agent, missible oil or microemulsion.
5. the Pesticidal combination of fluorine-containing pyridine worm amine nitrile according to claim 1 and butene-fipronil is characterized in that: but described composition is the dispersed oil suspending agent.
6. the purposes of Pesticidal combination in preventing and treating rice hoppers, weevil, snout moth's larva, cotton aphid, stinkbug silk worm, vegetable aphid, trialeurodes vaporariorum, flea beetle, thrips, oranges and tangerines aphid, lichee stinkbug silk worm insect of described fluorine-containing pyridine worm amine nitrile of claim 1 and butene-fipronil.
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