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CN102696642A - Acaricidal composition containing spirodiclofen and cyflumetofen - Google Patents

Acaricidal composition containing spirodiclofen and cyflumetofen Download PDF

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Publication number
CN102696642A
CN102696642A CN2012102238547A CN201210223854A CN102696642A CN 102696642 A CN102696642 A CN 102696642A CN 2012102238547 A CN2012102238547 A CN 2012102238547A CN 201210223854 A CN201210223854 A CN 201210223854A CN 102696642 A CN102696642 A CN 102696642A
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mite
miticide
spiral shell
acid esters
dibasic acid
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CN102696642B (en
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吴华龙
徐黎婷
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Zhejiang Yulong Pharmaceutical Co ltd
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HANGZHOU UDRAGON CHEMICAL CO Ltd
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Abstract

The invention relates to an acaricidal composition, in particular to an acaricidal composition containing spirodiclofen and cyflumetofen, which is particularly used for preventing panonychus citri, European red mites, European red two-spotted spider mites and cotton leaf mites. The acaricidal composition has an obvious synergistic effect on mite killing as compared with a single pesticide, can kill egg, larva, nymph and adult of acarid, and is contributed to postponing the generation of pesticide resistance of bacteria.

Description

A kind of miticide composition that contains spiral shell mite dibasic acid esters and fourth fluorine mite ester
[technical field]
The present invention relates to pesticide field, particularly the present invention relates to a kind of miticide composition, especially, the present invention relates to contain the miticide composition of spiral shell mite dibasic acid esters and fourth fluorine mite ester.
[background technology]
Tetranychid is the main kind that parasitizes plant, is the important pests of harm fruit tree, vegetables, flowers.Mite class individuality is little, distribution is wide, adaptability is strong; Its breeding is rapid, and the history of life is short, and hibernacle changes greatly; Its population structure is complicated, in a colony, can have the mite of all vegetative stages, comprises ovum, if mite, young mite and become mite etc.; It is strong to poor environment adaptability, easily medicament is developed immunity to drugs etc.All these has determined that the control ratio of mite class is difficult.
Spiral shell mite dibasic acid esters molecular formula: C 20H 22Cl 2O 5, relative molecular mass: 413.29, chemical name is: 3-(2,4 dichloro benzene base)-2-oxo-1-oxaspiro [4,5]-last of the ten Heavenly stems-3-alkene-4-base butyl carbonate.
Has following structural formula
Mechanism of action as acaricidal spiral shell mite dibasic acid esters mainly is the lipogenesis that suppresses in the pest mite body, and does not have cross resistance between the existing miticide, is applicable to be used for preventing and treating the pest mite class that existing miticide is produced resistance.The broad spectrum acaricidal agents, adaptable, on spider, yellow spider, rust Pi lice, yellow tea mite, carmine spider mite and two-spotted spider mite, etc. have a good control effect, can be used for citrus, grapes and other fruit trees and eggplant, peppers, tomatoes and other solanaceous crops mites governance; ovicidal effect is particularly outstanding, while the immature nymphs have good contact action, and long duration to control citrus red mite damage up to 40-50 days .But spiral shell mite dibasic acid esters is to becoming mite weak effect, the defective that quick-acting is relatively poor.
The molecular formula of fourth fluorine mite ester (Cyflumetofen): C 24H 24F 3NO 4Molecular weight: 447.45; Chemical name: (RS)-2-(4-tert-butyl-phenyl)-2-cyanic acid-3-oxygen-3-(α, α, α-three fluoro-o-tolyl) propionic acid-2-methoxyl group ethyl ester.
Has following structural formula
It is by the novel acyl group acetonitrile class miticide of Japan big tomb chemical company exploitation, does not have cross resistance with existing miticide.Get permission registration and sell in Japan first in 2007, and be used for the main mite class that crops such as fruit tree, vegetables, tea tree and flowers control parasitize plant,
At present, the composite and application of spiral shell mite dibasic acid esters and fourth fluorine mite ester is not all seen open both at home and abroad.The inventor finds, spiral shell mite dibasic acid esters and fourth fluorine mite ester carried out composite, can reduce pesticide dosage, improves miticidal effect, reduces environmental pollution, solved harmful mite single agricultural chemicals is prone to the generation resistance problem.
[summary of the invention]
The objective of the invention is to overcome the defective that single agricultural chemicals is prone to produce resistance; Problems such as the lasting period is short; Provide a kind of and can reduce pesticide dosage, reduce environmental pollution, the expanding prevention spectrum, reduce agricultural cost, and the miticide composition that the most important thing is to have synergistic function.
Another object of the present invention provides the purposes that said miticide composition is used to prevent and treat various agricultural evil mite, especially for the purposes of control panonychus citri, European red mite, apple Tetranychus urticae, cotton red spider.
The present invention realizes through following technical scheme:
A kind of miticide composition of the present invention is characterized in that, this miticide composition contains active component spiral shell mite dibasic acid esters and fourth fluorine mite ester, and the weight ratio of the two is 1:50 to 50:1.
Preferably, the weight ratio of spiral shell mite dibasic acid esters and fourth fluorine mite ester is 1:20 to 20:1 in this miticide composition.
More preferably, the weight ratio of spiral shell mite dibasic acid esters and fourth fluorine mite ester is 4:1 to 1:4 in this miticide composition, and most preferably, the weight ratio of spiral shell mite dibasic acid esters and fourth fluorine mite ester is 4:1.
The present invention relates to a kind of miticide, it is characterized in that, this miticide contains the aforesaid miticide composition of 0.5~95 weight %, and surplus is acceptable carrier and an auxiliary agent on the agricultural chemicals.Carrier can be solid or liquid, and any carrier that is generally used for preparing miticide composition all can use.
Preferably, this miticide contains the aforesaid miticide composition of 3~80 weight %.
More preferably, this miticide contains the aforesaid miticide composition of 15~70 weight %.
Except as otherwise noted, " % " in this specification all is weight percentage.
Suitable solid carrier comprises: mineral substance, plant class, synthetic filling class and inorganic salts carrier.Wherein the mineral substance carrier comprises silicates, carbonate, Sulfates and oxide-based carrier; The silicates carrier comprises for example kaolin, sepiolite, nacrite, imvite, mica, vermiculite, pyrophyllite, talcum; The carbonate carrier comprises for example calcium carbonate, dolomite; The sulphate carrier comprises for example ammonium sulfate, sodium sulphate, calcium sulphate; Oxide-based carrier comprises for example quicklime, magnesium lime, diatomite; Plant class carrier for example comprises: oranges and tangerines slag, corncob cellulose, rice husk powder, rice husk, big soya bean stem meal, tobacco powder, walnut shell, sawdust; Synthetic filling class carrier comprises for example winnofil hydrate, winnofil, white carbon.Inorganic salts is potassium chloride for example, sodium chloride.
Liquid-carrier comprises water and organic solvent.When effective composition was aqueous emulsion or suspension emulsion, organic solvent played solubilising and antifreeze effect.Appropriate organic solvent comprises aromatic hydrocarbons, for example benzene, xylol, toluene, alkylbenzene, Fluhyzon and chlorinated aromatic hydrocarbons; Chlorinated aliphatic hydrocarbon, for example vinyl chloride, chloroform, carrene, chloroform, carbon tetrachloride and many chloroethanes; Aliphatic hydrocarbon, for example petroleum distillate, cyclohexane, light mineral oil and paraffin.Alcohols is methyl alcohol for example, ethanol, isopropyl alcohol, butanols, isobutanol, ethylene glycol, propane diols, glycerine, fatty alcohol etc.; Ethers is Propylene Glycol ether for example, ethohexadiol ether, benzinum.Ketone is acetone, MEK, methyl iso-butyl ketone (MIBK), cyclohexanone and different fluorine that ketone, N-methyl-pyrrolidones for example; Special solvent also has dimethyl formamide, dimethyl sulfoxide (DMSO), polyethylene glycol, nitrile; The vegetable oil and the vegetable oil that methylates.Above-mentioned organic solvent both can use separately, also can mix use, can also be mixed together use with water.
Auxiliary agent according to the invention can comprise one or more in surfactant, antifoaming agent, thickener, suspending agent and the antifreezing agent as required, can also comprise other auxiliary agents that the industry is commonly used as required.
Surfactant can be emulsifier, dispersant, stabilizing agent or wetting agent; Can be ion-type or nonionic.Suitable surfactant comprises: the sodium salt of polyacrylic acid and lignin sulfonic acid and calcium salt; The polycondensation product of fatty acid or fatty amine and oxirane that contains at least 12 carbon atoms in the molecule and/expoxy propane; The fatty acid ester of glycerine, dodecanol-1, tetradecanol-1, sorbierite, sucrose or pentaerythrite; And the polycondensation product of they and oxirane and/or expoxy propane; The sulphate of their polycondensation product or sulfonate; In molecule, contain the sulfuric acid of 10 carbon atoms or the alkali metal or the alkali salt of sulfonic acid at least, preferable is sodium salt, like sodium salt, alkylaryl sodium sulfonate and the neopelex of lauryl sodium sulfate, Teepol, sulfonated castor oil; The copolymer of polymers of ethylene oxide, oxirane and expoxy propane.
Emulsifier comprises nonionic emulsifier and commercially available emulsifier.The preferred polyoxyethylene fatty acid fat of nonionic emulsifier, polyoxyethylene aliphatic alcohol ether and polyoxyethylene fatty amine, for example ethoxylated castor oil, polyoxyethylene (n 20) phenethyl phenolic group oleic acid ester, alkylaryl polyoxyethylene poly-oxygen propylene aether, alkylaryl formaldehyde resin APEO, triphenyl vinyl phenol polyoxyethylene (n 20), ether phosphoric acid triethanolamine salt, hexichol ethyl phenolic group APEO (n 18) formaldehyde condensation products, diphenyl phenol polyethenoxy (n 18) polyethenoxy ether (n 20) etc.Commercially available emulsifier comprises: agricultural newborn 0201B, agricultural newborn 0203B, farming breast 100 #, farming breast 500 #, farming breast 600 #, agricultural newborn 600-2 #, farming breast 1601, farming breast 2201, agricultural newborn NP-10, agricultural newborn NP-15, farming breast 507 #, agricultural newborn OX-635, agricultural newborn OX-622, agricultural newborn OX-653, agricultural newborn OX-667, agricultural newborn CS-7, peaceful breast 36 #
Dispersant of the present invention comprises: sodium lignin sulfonate; Draw back powder; Calcium lignosulfonate; Condensation compound of methyl naphthalene sulfonic acid and formaldehyde; Naphthalene sulfonic acid-formaldehyde condensation product; The methanonaphthalene sodium sulfonate; Oleic acid methylamino ethylsulfonic acid sodium; Epoxidized polyether; To tertbutyl ether; The dibutyl naphthalene sulfonic acid-formaldehyde condensation product; Phosphate such as calgon; The alkylphenol-polyethenoxy based phosphates; Alkylphenol-polyethenoxy base ether formaldehyde condensation products sulphate; N-methyl-fatty acyl group-sodium taurocholate APES formaldehyde condensation products; Aralkyl phenol polyethenoxy ether phosphate APES; The castor oil ethylene oxide adduct; Ethylene oxide-propylene oxide block copolymer APES formaldehyde condensation products; Alkylphenol-polyethenoxy polyethenoxy ether and methylcellulose.
Wetting agent of the present invention comprises: sldium lauryl sulfate; Alkylol polyoxyethylene groups ether sodium sulfate; Octylphenol polyethylene oxyethylene group ether sulfate; Alkylphenol-polyethenoxy base ether formaldehyde condensation products sulphate; Sodium alkyl sulfonate; Neopelex; Negel; Dialkyl succinylsuccinate sulfonate; Lauryl alcohol polyethylene glycol oxide base ether sulfonic acid sodium; The alkyl amide sodium taurocholate; Aliphatic alcohol polyethenoxy base ether; Alkylphenol-polyethenoxy base ether; The polyoxyethylene polyoxypropylene block polymer; Sorbitan fatty acid ester polyoxyethylene groups ether etc.
Thickener of the present invention both can be a synthetic, for example carboxymethyl alcohol, polyvinyl alcohol or polyvinyl acetate; Also can be natural water-soluble polymer, for example xanthans, gelatin, gum Arabic, polyvinylpyrrolidone, Magnesiumaluminumsilicate, polyvinyl alcohol, polyethylene glycol, phenolic resins, shellac, carboxymethyl cellulose and sodium alginate etc.
Antifoaming agent of the present invention is preferably: bubble enemy, silicone, C 8~10Fatty alcohol, C 10~20Saturated fat acids and acid amides etc.
Miticide composition of the present invention can be mixed with agricultural and go up acceptable forms; Preferred dosage form is liquor, missible oil, suspending agent, microemulsion, aqueous emulsion, pulvis, wetting powder, soluble powder, granule or capsule etc., and said formulation adopts the method that well known to a person skilled in the art to process, prepare.
Miticide composition of the present invention can directly be processed the finished product preparation form, and promptly each material mixes in the composition, directly is used for mite extremely; The composition of composition also can directly mix in bucket (jar) before using to be provided by independent preparation.Concentrate of the present invention mixes the concentration that obtains required active substance usually with water.
The present invention also provides a kind of method of preventing and treating agricultural evil mite, before or after crops and/or fruit infection evil mite, uses above-mentioned miticide composition of the present invention or miticide to the place of crops and/or fruit and growth or storage.Application process is the conventional application process of agricultural chemicals, like cast, injection, spraying etc.Amount of application is with weather conditions or crop state variation.Miticide of the present invention is used field do farmland, orchard or warehouse etc.
Miticide composition of the present invention can be used for preventing and treating various agricultural evil mite, particularly is applicable to panonychus citri, European red mite, apple Tetranychus urticae, cotton red spider on the crops such as control oranges and tangerines, apple, hawthorn, cotton, eggplant.
Miticide composition of the present invention also can have the compound use of mite, weeding, bactericidal property extremely with other, also can mix use with nematocide, protective agent, growth regulator, nutrient for plants or soil conditioner.
Compared with prior art, beneficial effect of the present invention is:
(1) compare with single agent, miticide composition according to the invention has significant synergistic effect to the evil mite, can kill ovum, young mite, if mite with become mite;
(2) miticide composition according to the invention or miticide have long characteristics of lasting period;
(3) reduce using dosage, reduced peasant's drug cost; Utilize 2 kinds of agricultural chemicals that the different mode of action of evil mite, the different mechanism of action reasonably are mixed, both prolonged agricultural chemicals service life, delay the drug-fast generation of evil mite again.
[embodiment]
Come the present invention is further specified below in conjunction with specific embodiment, but do not limit the invention to these embodiments.One skilled in the art would recognize that the present invention contained in claims scope all alternatives, improvement project and the equivalents that possibly comprise.
Among the present invention in the proportioning of all solids preparation percentage all be weight percentage, percentage is percent by volume in the proportioning of liquid preparation, active ingredient is than the weight ratio that all refers to spiral shell mite dibasic acid esters and fourth fluorine mite ester.
One, preparation embodiment
1, the preparation of missible oil
General preparation method is: by the prescription requirement, add solvent, former medicine, emulsifier respectively, mix, use the water-bath heating for dissolving in case of necessity, promptly obtain transparence missible oil.
Embodiment 1 (30% missible oil, active ingredient is than 2:1)
Spiral shell mite dibasic acid esters 20%, fourth fluorine mite ester 10%, farming breast 2201 #7.5%, farming breast 600 #4.5%, dimethyl formamide 8%, solvent naphtha 150 complements to 100%.
Embodiment 2 (25% missible oil, active ingredient is than 4:1)
Spiral shell mite dibasic acid esters 20%, fourth fluorine mite ester 5%, farming breast 500 #5%, agricultural newborn 0201B10%, dimethyl formamide 12%, solvent naphtha 150 complements to 100%.
Embodiment 3 (42% missible oil, active ingredient is than 20:1)
Spiral shell mite dibasic acid esters 40%, fourth fluorine mite ester 2%, agricultural newborn 0203B 6%, agricultural newborn 0201B 9%, cyclohexanone 8%, solvent naphtha 150 complements to 100%.
2, the preparation of wetting powder
General preparation method is: by the prescription requirement, former medicine, various auxiliary agent and filler etc. are fully mixed, after ultrafine crusher is pulverized, promptly obtain converted products.
Embodiment 4 (25% wetting powder, active ingredient is than 1:4)
Spiral shell mite dibasic acid esters 5%, fourth fluorine mite ester 20%, neopelex 2.0%, white carbon black 5%, sodium lignin sulfonate 10%, precipitated calcium carbonate complements to 100%.
Embodiment 5 (45% wetting powder, active ingredient is than 1:8)
Spiral shell mite dibasic acid esters 5%, fourth fluorine mite ester 40%, lauryl sodium sulfate 1.5%, naphthalene sulfonic acid-formaldehyde condensation product 5%, sodium lignin sulfonate 3%, white carbon black 8%, precipitated calcium carbonate complements to 100%.
Embodiment 6 (42% wetting powder, active ingredient is than 1:20)
Spiral shell mite dibasic acid esters 2%, fourth fluorine mite ester 40%, neopelex 1.8%, to tertbutyl ether 2%, white carbon black 10%, sodium lignin sulfonate 10%, precipitated calcium carbonate complements to 100%.
3, the preparation of water-dispersible granules
General preparation method is: former medicine and powder carrier, wetting spreader-sticker and binding agent etc. are mixed pulverizing, after adding water again and mediating, add in the comminutor that the certain specification screen cloth is housed and carry out granulation.And then warp is dry, screening (pressing the screen cloth scope) promptly gets granular product.
Embodiment 7 (30% water-dispersible granules, active ingredient is than 2:1)
Spiral shell mite dibasic acid esters 20%, fourth fluorine mite ester 10%, sodium lignin sulfonate 15%, methyl naphthalene sulfonate formaldehyde condensate 5%, epoxidized polyether 5%, bentonite 10%, kaolin complements to 100%.
Embodiment 8 (40% water-dispersible granules, active ingredient is than 1:1)
Spiral shell mite dibasic acid esters 20%, fourth fluorine mite ester 20%, N-methyl-oleoyl-sodium taurocholate 8%, naphtholsulfonic acid formaldehyde condensation products 10%, soluble starch 8%, sodium sulphate 10%, kaolin complements to 100%.
Embodiment 9 (50% water-dispersible granules, active ingredient is than 4:1)
Spiral shell mite dibasic acid esters 40%, fourth fluorine mite ester 10%, N-methyl-oleoyl-sodium taurocholate 8%, naphtholsulfonic acid formaldehyde condensation products 10%, soluble starch 8%, sodium sulphate 10%, kaolin complements to 100%.
Embodiment 10 (45% water-dispersible granules, active ingredient is than 8:1)
Spiral shell mite dibasic acid esters 40%, fourth fluorine mite ester 5%, sodium lignin sulfonate 15%, methyl naphthalene sulfonate formaldehyde condensate 5%, epoxidized polyether 5%, bentonite 10%, kaolin complements to 100%.
4, the preparation of suspending agent
General preparation method is: by the prescription requirement, be medium with water, with former medicine, dispersant, wetting agent, add in the sand mill after suspending agent and antifreezing agent etc. mixes, carry out sand milling to certain particle diameter filtration back adding thickener shear agitation and evenly get final product.
Embodiment 11 (30% suspending agent, active ingredient is than 2:1)
Spiral shell mite dibasic acid esters 20%, fourth fluorine mite ester 10% draws back powder 1.5%, Soproplot SC 3%, xanthans 0.15%, aluminium-magnesium silicate 1.5%, 418G 0.3%, and BIT 0.05%, ethylene glycol 3%, water complements to 100%.
Embodiment 12 (40% suspending agent, active ingredient is than 1:1)
Spiral shell mite dibasic acid esters 20%, fourth fluorine mite ester 20%, sodium lignin sulfonate 5%, white carbon black 0.3%, attapulgite 1.0%, potassium dihydrogen phosphate 0.2%, ethylene glycol 4%, tributyl phosphate 0.2%, water complements to 100%.
Embodiment 13 (25% suspending agent, active ingredient is than 4:1)
Spiral shell mite dibasic acid esters 20%, fourth fluorine mite ester 5%, methyl naphthalene sulfonate formaldehyde condensate 2.5%, bentonite 1.0%, agricultural newborn OX-656 5.0%, glycerine 4%, tributyl phosphate 0.2%, water complements to 100%.
Embodiment 14 (36% suspending agent, active ingredient is than 8:1)
Spiral shell mite dibasic acid esters 32%, fourth fluorine mite ester 4%, phenethyl phenol polyethenoxy polyethenoxy ether 3%, Magnesiumaluminumsilicate 1.0%, xanthans 0.1%, propane diols polyoxyethylene poly-oxygen propylene aether 1.0%, water complements to 100%.
5, the preparation of aqueous emulsion
General preparation method is: with former medicine, and solvent, emulsifier stirs and is made into the homogeneous oil phase, and with water, ethylene glycol mixes stirring and is made into water, under high shear conditions, oil phase is joined aqueous phase slowly, can obtain aqueous emulsion.
Embodiment 15 (25% aqueous emulsion, active ingredient is than 4:1)
Spiral shell mite dibasic acid esters 20%, fourth fluorine mite ester 5%, solvent naphtha S-150 30%, calcium dodecyl benzene sulfonate 3%, styryl phenyl APEO 6%, ethylene glycol 3%, water is mended to 100%.
Embodiment 16 (36% aqueous emulsion, active ingredient is than 8:1)
Spiral shell mite dibasic acid esters 32%, fourth fluorine mite ester 4%, solvent naphtha S-150 30%, triphen ethyl phenol polyoxyethylene ether phosphate 4%, terminal hydroxy group polyoxyethylene poly-oxygen propylene aether block copolymer 5%, ethylene glycol 3%, water is mended to 100%.
Embodiment 17 (20% aqueous emulsion, active ingredient is than 4:1)
Spiral shell mite dibasic acid esters 16%, fourth fluorine mite ester 4%, solvent naphtha S-150 30%, triphen ethyl phenol polyoxyethylene ether phosphate 3%, styryl phenol formaldehyde resin polyoxyethylene poly-oxygen propylene aether 5%, propane diols 3%, water is mended to 100%.
6, microemulsion processing technology:
General preparation method is: with former medicine, and solvent, emulsifier stirs and is made into the homogeneous oil phase, and water is joined in the oil phase gradually, is stirred to transparent and homogeneous and gets final product.
Embodiment 18 (25% microemulsion, active ingredient is than 4:1)
Spiral shell mite dibasic acid esters 20%, fourth fluorine mite ester 5%, N-Methyl pyrrolidone 6%, solvent naphtha S-15015%, calcium dodecyl benzene sulfonate 2%, terminal hydroxy group polyoxyethylene poly-oxygen propylene aether 18%, water is mended to 100%.
Embodiment 19 (36% microemulsion, active ingredient is than 8:1)
Spiral shell mite dibasic acid esters 32%, fourth fluorine mite ester 4%, isopropyl alcohol 10%, solvent naphtha S-150 15%, calcium dodecyl benzene sulfonate 2%, styryl phenyl APEO 19%, water is mended to 100%.
Embodiment 20 (40% microemulsion, active ingredient is than 1:1)
Spiral shell mite dibasic acid esters 20%, fourth fluorine mite ester 20%, N-octylpyrrolidone 6%, solvent naphtha S-15015%, calcium dodecyl benzene sulfonate 2%, alkyl phenol formaldehyde resin polyoxyethylene ether 16%, water is mended to 100%.
Embodiment 21 (40.8% microemulsion, active ingredient is than 1:50)
Spiral shell mite dibasic acid esters 0.8%, fourth fluorine mite ester 40%, N-octylpyrrolidone 6%, solvent naphtha S-15015%, calcium dodecyl benzene sulfonate 2%, alkyl phenol formaldehyde resin polyoxyethylene ether 16%, water is mended to 100%.
Embodiment 20 (51% microemulsion, active ingredient is than 50:1)
Spiral shell mite dibasic acid esters 50%, fourth fluorine mite ester 1%, N-octylpyrrolidone 6%, solvent naphtha S-15015%, calcium dodecyl benzene sulfonate 2%, alkyl phenol formaldehyde resin polyoxyethylene ether 16%, water is mended to 100%.
Two, biologically active embodiment
Biologically active embodiment is divided into indoor biologically active embodiment and land for growing field crops biologically active embodiment.
1. indoor biologically active
Embodiment 1 spiral shell mite dibasic acid esters and fourth fluorine mite ester are to the Toxicity Determination of panonychus citri
Further understand the virulence of the complex composition of spiral shell mite dibasic acid esters and fourth fluorine mite ester, carried out a large amount of formulation screening tests insect.Test is estimated SOP (insecticide volume) with reference to pesticide indoor bioassay test rule (agricultural industry criteria NY/T1154.7-2006) and initiative pesticide bioactivity, adopts infusion process.Citrus leaflet tablet band handle is cut, inserted in the ampere bottle that adds water.Connect the one-tenth mite of some.Mite to be become lays eggs behind the 24h, removes into mite, and the blade that will have abundant ovum is dipped in 10s in the soup, inhales with blotting paper rapidly and removes unnecessary soup, and blade is placed the ampere bottle again, dries naturally.Place observation ward (to cultivate in 25 ± 1 ℃, humidity 70% ~ 80%, 16h illumination/d).Test repetition 4 times, and establish blank is investigated after waiting to contrast whole hatchings.Be regarded as dead worm with the young mite that can not hatch He can not normally creep during investigation.
Figure BDA00001819292000101
Theory is used the content (%) of toxicity index * B in using with of content (the %)+B of toxicity index * A in using with of toxicity index (TTI)=A with
Figure BDA00001819292000102
If co-toxicity coefficient is greater than 120, and showing has synergistic effect; If less than 80, be indicated as antagonism; If, be indicated as summation action greater than 80 less than 120.
The result shows: result of the test: spiral shell mite dibasic acid esters and fourth fluorine mite ester are mixed to supplying the examination target that very high activity is all arranged; After being mixed, spiral shell mite dibasic acid esters and fourth fluorine mite ester show significant synergistic effect; Spiral shell mite dibasic acid esters: during fourth fluorine mite ester=4:1, co-toxicity coefficient is maximum, and synergistic effect is the most remarkable.The result sees following table 1 for details.
Table 1 spiral shell mite dibasic acid esters and the composite Toxicity Determination result of fourth fluorine mite ester to panonychus citri
Figure BDA00001819292000111
Embodiment 2 spiral shell mite dibasic acid esters and fourth fluorine mite ester are to the Toxicity Determination of European red mite
Understand the virulence of the complex composition of spiral shell mite dibasic acid esters and fourth fluorine mite ester, carried out a large amount of formulation screening tests insect.Test is estimated SOP (insecticide volume) with reference to pesticide indoor bioassay test rule (agricultural industry criteria NY/T1154.7-2006) and initiative pesticide bioactivity, adopts infusion process.Apple leaflet tablet band handle is cut, inserted in the ampere bottle that adds water.Connect the one-tenth mite of some.Mite to be become lays eggs behind the 24h, removes into mite, and the blade that will have abundant ovum is dipped in 10s in the soup, inhales with blotting paper rapidly and removes unnecessary soup, and blade is placed the ampere bottle again, dries naturally.Place observation ward (to cultivate in 25 ± 1 ℃, humidity 70% ~ 80%, 16h illumination/d).Test repetition 4 times, and establish blank is investigated after waiting to contrast whole hatchings.Be regarded as dead worm with the young mite that can not hatch He can not normally creep during investigation.
Figure BDA00001819292000121
Theory is used the content (%) of toxicity index * B in using with of content (the %)+B of toxicity index * A in using with of toxicity index (TTI)=A with
If co-toxicity coefficient is greater than 120, and showing has synergistic effect; If less than 80, be indicated as antagonism; If, be indicated as summation action greater than 80 less than 120.
The result shows: result of the test: spiral shell mite dibasic acid esters and fourth fluorine mite ester are mixed to supplying the examination target that very high activity is all arranged; After being mixed, spiral shell mite dibasic acid esters and fourth fluorine mite ester show significant synergistic effect; Spiral shell mite dibasic acid esters: during fourth fluorine mite ester=4:1, co-toxicity coefficient is maximum, and synergistic effect is the most remarkable.The result sees following table 2 for details.
Table 2 spiral shell mite dibasic acid esters and the composite Toxicity Determination result of fourth fluorine mite ester to European red mite
Embodiment 3 spiral shell mite dibasic acid esters and fourth fluorine mite ester are to the Toxicity Determination of apple Tetranychus urticae
The complex composition of spiral shell mite dibasic acid esters and fourth fluorine mite ester has carried out a large amount of formulation screening tests to the virulence of insect.Test is estimated SOP (insecticide volume) with reference to pesticide indoor bioassay test rule (agricultural industry criteria NY/T1154.7-2006) and initiative pesticide bioactivity, adopts infusion process.Apple leaflet tablet band handle is cut, inserted in the ampere bottle that adds water.Connect the one-tenth mite of some.Mite to be become lays eggs behind the 24h, removes into mite, and the blade that will have abundant ovum is dipped in 10s in the soup, inhales with blotting paper rapidly and removes unnecessary soup, and blade is placed the ampere bottle again, dries naturally.Place observation ward (to cultivate in 25 ± 1 ℃, humidity 70% ~ 80%, 16h illumination/d).Test repetition 4 times, and establish blank is investigated after waiting to contrast whole hatchings.Be regarded as dead worm with the young mite that can not hatch He can not normally creep during investigation.
Figure BDA00001819292000131
Theory is used the content (%) of toxicity index * B in using with of content (the %)+B of toxicity index * A in using with of toxicity index (TTI)=A with
Figure BDA00001819292000132
If co-toxicity coefficient is greater than 120, and showing has synergistic effect; If less than 80, be indicated as antagonism; If, be indicated as summation action greater than 80 less than 120.
The result shows: result of the test: spiral shell mite dibasic acid esters and fourth fluorine mite ester are mixed to supplying the examination target that very high activity is all arranged; After being mixed, spiral shell mite dibasic acid esters and fourth fluorine mite ester show significant synergistic effect; Spiral shell mite dibasic acid esters: during fourth fluorine mite ester=4:1, co-toxicity coefficient is maximum, and synergistic effect is the most remarkable.The result sees following table 3 for details.
Table 3 spiral shell mite dibasic acid esters and the composite Toxicity Determination result of fourth fluorine mite ester to the apple Tetranychus urticae
Figure BDA00001819292000133
Embodiment 4 spiral shell mite dibasic acid esters and fourth fluorine mite ester are to the Toxicity Determination of cotton red spider
The complex composition of spiral shell mite dibasic acid esters and fourth fluorine mite ester has carried out a large amount of formulation screening tests to the virulence of insect.Test is estimated SOP (insecticide volume) with reference to pesticide indoor bioassay test rule (agricultural industry criteria NY/T1154.7-2006) and initiative pesticide bioactivity, adopts infusion process.Cotton leaflet tablet band handle is cut, inserted in the ampere bottle that adds water.Connect the one-tenth mite of some.Mite to be become lays eggs behind the 24h, removes into mite, and the blade that will have abundant ovum is dipped in 10s in the soup, inhales with blotting paper rapidly and removes unnecessary soup, and blade is placed the ampere bottle again, dries naturally.Place observation ward (to cultivate in 25 ± 1 ℃, humidity 70% ~ 80%, 16h illumination/d).Test repetition 4 times, and establish blank is investigated after waiting to contrast whole hatchings.Be regarded as dead worm with the young mite that can not hatch He can not normally creep during investigation.
Figure BDA00001819292000141
Theory is used the content (%) of toxicity index * B in using with of content (the %)+B of toxicity index * A in using with of toxicity index (TTI)=A with
Figure BDA00001819292000142
If co-toxicity coefficient is greater than 120, and showing has synergistic effect; If less than 80, be indicated as antagonism; If, be indicated as summation action greater than 80 less than 120.
The result shows: result of the test: spiral shell mite dibasic acid esters and fourth fluorine mite ester are mixed to supplying the examination target that very high activity is all arranged; After being mixed, spiral shell mite dibasic acid esters and fourth fluorine mite ester show significant synergistic effect; Spiral shell mite dibasic acid esters: during fourth fluorine mite ester=4:1, co-toxicity coefficient is maximum, and synergistic effect is the most remarkable.The result sees following table 4 for details.
Table 4 spiral shell mite dibasic acid esters and the composite Toxicity Determination result of fourth fluorine mite ester to cotton red spider
Figure BDA00001819292000151
2, land for growing field crops biologically active embodiment
The field control effectiveness test of land for growing field crops biologically active embodiment 1 control panonychus citri
Under field condition, measure the control efficiency of the prepared miticide of embodiment 3,6,9,10,12,13,15,17,18,21 and 22 to panonychus citri.Experimental field be positioned at Dai Jia village, township, sound hole, Kaihua County, Zhejiang Province, be the outdoor cropping oranges and tangerines, 20 centimetres of spacing in the rows, 30 centimetres of line-spacings.Formulation rate is 750kg/hm 220% spiral shell mite dibasic acid esters suspending agent: 37.5mg a.i./hm 220% fourth fluorine mite ester suspending agent: 50g a.i./hm 2Use " closing U.S.A " HM-16A type back-pack electric sprayer, plant blade face even spraying.Repeat for 4 times, district's group is arranged at random.3 days, 10 days, 20 days investigation results behind the medicine.Regulation according to " pesticide field efficacy medicine test criterion ()---insecticide control panonychus citri " is carried out; Every experimental plot oranges and tangerines blade adopts 5 fixed points by east, south, west, 5 azimuth marks in north; 2 strains are investigated in every sub-district, investigate all borer populations of living in every strain.
Result of the test: use the prepared miticide of FORMULATION EXAMPLE 3,6,9,10,12,13,15,17,18,21 and 22; The panonychus citri preventive effect was respectively 91.3%-97.6% and 84.3%-92.3% in 10 days, 20 days behind the medicine, control panonychus citri effect all is better than 20% fourth fluorine mite ester suspending agent 50g a.i./hm 2With 20% spiral shell mite dibasic acid esters suspending agent 37.5g a.i./hm 2
Data in please supplementary table.If there is not definite experimental data, please replenish reasonably can the anticipation value
Table 5 fourth fluorine mite ester spiral shell mite dibasic acid esters is mixed to the field control effectiveness test result of panonychus citri
Figure BDA00001819292000161
The field control effectiveness test of land for growing field crops biologically active embodiment 2 control cotton red spiders
Under field condition, measure the control efficiency of the prepared miticide of FORMULATION EXAMPLE 3,4,6,8,9,11,13,15,17,18,21 and 22 to cotton red spider.Experimental field be positioned at experiment station, Linqing, cotton research center, Shandong Province, cotton variety grinds No. 28 for the Shandong cotton.Formulation rate is 750kg/hm 220% spiral shell mite dibasic acid esters suspending agent: 37.5g a.i./hm 220% fourth fluorine mite ester suspending agent: 50g a.i./hm 2Use " closing U.S.A " HM-16A type back-pack electric sprayer, plant blade face even spraying.Sub-district area: 33.3m 2, 4 repetitions, district's group is arranged at random.Before the control of spray medicine, 5 samplings of every sub-district diagonal, fixed point investigation cotton red spider number, the strain number and the borer population of living of the investigation of record fixed point.
Result of the test: use FORMULATION EXAMPLE 3,4,6,8,9,11,13,15,17,18,21 and 22; The cotton red spider preventive effect was respectively 92.7%-98.3% and 89.0%-97.7% in 10 days, 20 days behind the medicine, control cotton red spider effect all is better than 20% fourth fluorine mite ester suspending agent 50ga.i./hm 2With 20% spiral shell mite dibasic acid esters suspending agent 37.5g a.i./hm 2
Table 6 fourth fluorine mite ester spiral shell mite dibasic acid esters is mixed to the field control effectiveness test of cotton red spider
Figure BDA00001819292000171
The field control effectiveness test of land for growing field crops biologically active embodiment 3 control apple Tetranychus urticaes
Under field condition, measure the control efficiency of 3,6,9,13,15,18,21,22 pairs of European red mites of FORMULATION EXAMPLE.Experimental field be positioned at Fei Chenganzhuan town, Shandong Province, kind is new Red Star, seeding row spacing 3m*4m.Formulation rate is 750kg/hm 220% spiral shell mite dibasic acid esters suspending agent: 37.5mg a.i./hm 220% fourth fluorine mite ester suspending agent: 50g a.i./hm 2Use " closing U.S.A " HM-16A type back-pack electric sprayer, plant blade face even spraying.Repeat for 4 times, district's group is arranged at random.3 days, 10 days, 20 days investigation results behind the medicine.Every experimental plot apple blade adopts 5 fixed points by east, south, west, 5 azimuth marks in north, and 2 strains are investigated in every sub-district, investigates all borer populations of living in every strain.
Result of the test: use FORMULATION EXAMPLE 3,6,9,13,15,18,21,22; The European red mite preventive effect was respectively 95.5%-97.7% and 93.7%-95.9% in 10 days, 20 days behind the medicine, control European red mite effect all is better than 20% fourth fluorine mite ester suspending agent 50g a.i./hm 2With 20% spiral shell mite dibasic acid esters suspending agent 37.5g a.i./hm 2
Table 7 fourth fluorine mite ester spiral shell mite dibasic acid esters is mixed to the field control effectiveness test of apple Tetranychus urticae
The field control effectiveness test of land for growing field crops biologically active embodiment 4 control European red mites
Under field condition, measure the control efficiency of 3,6,9,13,15,18,21,22 pairs of European red mites of FORMULATION EXAMPLE.Experimental field be positioned at Fei Chenganzhuan town, Shandong Province, kind is new Red Star, seeding row spacing 3m*4m.Formulation rate is 750kg/hm 220% spiral shell mite dibasic acid esters suspending agent: 37.5mg a.i./hm 220% fourth fluorine mite ester suspending agent: 50g a.i./hm 2Use " closing U.S.A " HM-16A type back-pack electric sprayer, plant blade face even spraying.Repeat for 4 times, district's group is arranged at random.3 days, 10 days, 20 days investigation results behind the medicine.Every experimental plot apple blade adopts 5 fixed points by east, south, west, 5 azimuth marks in north, and 2 strains are investigated in every sub-district, investigates all borer populations of living in every strain.
Result of the test: use FORMULATION EXAMPLE 3,6,9,13,15,18,21,22; The European red mite preventive effect was respectively 95.5%-97.7% and 93.7%-95.9% in 10 days, 20 days behind the medicine, control European red mite effect all is better than 20% fourth fluorine mite ester suspending agent 50g a.i./hm 2With 20% spiral shell mite dibasic acid esters suspending agent 37.5g a.i./hm 2
Table 8 fourth fluorine mite ester spiral shell mite dibasic acid esters is mixed to the field control effectiveness test of European red mite
Figure BDA00001819292000191
The miticide composition that contains spiral shell mite dibasic acid esters and fourth fluorine mite ester of the present invention is described through concrete embodiment.Those skilled in the art can use for reference links such as content appropriate change raw material of the present invention, process conditions and realize corresponding other purpose; Its relevant change does not all break away from content of the present invention; All similar replacements and change will become apparent to those skilled in the art that all to be regarded as and are included within the scope of the present invention.

Claims (8)

1. a miticide composition is characterized in that said miticide composition contains active component spiral shell mite dibasic acid esters and fourth fluorine mite ester, and the weight ratio of said spiral shell mite dibasic acid esters and fourth fluorine mite ester is 1:50 to 50:1.
2. miticide composition according to claim 1 is characterized in that the weight ratio of spiral shell mite dibasic acid esters and fourth fluorine mite ester is 1:20 to 20:1 in the said miticide composition.
3. miticide composition according to claim 1 is characterized in that the weight ratio of spiral shell mite dibasic acid esters and fourth fluorine mite ester is 4:1 in the said miticide composition.
4. a miticide is characterized in that said miticide contains the described miticide composition of each claim of claim 1-3 of 0.5~95 weight %, and surplus is acceptable carrier and an auxiliary agent on the agricultural chemicals.
5. miticide according to claim 4 is characterized in that said miticide contains the described miticide composition of each claim of claim 1-3 of 3~80 weight weight %.
6. miticide according to claim 4 is characterized in that said miticide contains the described miticide composition of each claim of claim 1-3 of 15~70 weight weight %.
7. the purposes of preventing and treating panonychus citri, European red mite, apple Tetranychus urticae, cotton red spider according to the described miticide composition of each claim of claim 1-4.
8. prevent and treat the method that agricultural does harm to mite for one kind; Before or after crops and/or fruit infection evil mite, use described miticide composition of each claim of claim 1-3 or the described miticide of each claim of claim 4-6 to the place of crops and/or fruit and growth or storage.
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CN104585179A (en) * 2014-12-25 2015-05-06 广东中迅农科股份有限公司 Synergistic acaricidal composition containing tebufenpyrad and spirodiclofen
CN107318862A (en) * 2016-04-28 2017-11-07 江苏龙灯化学有限公司 A kind of Pesticidal combination

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WO2010145999A2 (en) * 2009-06-18 2010-12-23 Basf Se Fungicidal mixtures

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Publication number Priority date Publication date Assignee Title
CN101203135A (en) * 2005-04-28 2008-06-18 拜尔农作物科学股份公司 Combinations of pesticidal active substance combinations
WO2010145999A2 (en) * 2009-06-18 2010-12-23 Basf Se Fungicidal mixtures

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Publication number Priority date Publication date Assignee Title
CN104585179A (en) * 2014-12-25 2015-05-06 广东中迅农科股份有限公司 Synergistic acaricidal composition containing tebufenpyrad and spirodiclofen
CN104585179B (en) * 2014-12-25 2017-12-12 广东中迅农科股份有限公司 A kind of Synergistic mite killing composition containing tebufenpyrad and spirodiclofen
CN107318862A (en) * 2016-04-28 2017-11-07 江苏龙灯化学有限公司 A kind of Pesticidal combination

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