CN102362591A - Insecticidal composition containing spinetoram and amide pesticides - Google Patents

Insecticidal composition containing spinetoram and amide pesticides Download PDF

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Publication number
CN102362591A
CN102362591A CN2011103689421A CN201110368942A CN102362591A CN 102362591 A CN102362591 A CN 102362591A CN 2011103689421 A CN2011103689421 A CN 2011103689421A CN 201110368942 A CN201110368942 A CN 201110368942A CN 102362591 A CN102362591 A CN 102362591A
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ethyl pleocidin
active ingredient
pesticidal combination
insecticidal composition
active ingredients
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葛大鹏
杜秀斌
杨波涛
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SHANDONG HAILIR CHEMICAL CO Ltd
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SHANDONG HAILIR CHEMICAL CO Ltd
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Abstract

The invention relates to an insecticidal composition in the field of formulation of pesticides. The insecticidal composition comprises two active ingredients of spinetoram and one of four amide compounds; the two active ingredients are mixed; the weight percentage of the two active ingredients is (1-90):(90-1), and preferably the weight percentage is (1-45):(60-3); the total mass percentage content of the active ingredients of the insecticidal composition is 1 to 90 percent, preferably 5 to 60 percent; the other ingredients comprise auxiliary ingredients which are allowable and acceptable in the pesticides; and the insecticidal composition can be prepared into water emulsion, microemulsion, missible oil, suspending agents, wettable powder, micro-capsule suspending agents and water dispersible granules. The insecticidal composition using the spinetoram and the amide compounds as the active ingredients has an obvious effect of preventing and controlling lepidoptera insects such as plutella xylostella, beet armyworm, prodenia litura, cotton bollworm, mealybug and the like, and homoptera sucking mouthpart pests such as aphid, aleyrodid, leafhopper and the like.

Description

A kind of Pesticidal combination that contains ethyl pleocidin and amides pesticide
Technical field
The present invention relates to the agriculture chemical compounding technical field, it is two yuan of Pesticidal combinations that are mixed of active ingredient with ethyl pleocidin and amides compound that tool relates to a kind of.
Background technology
Ethyl pleocidin, Spinetoram (XDE-175) are by the plain insecticides of many desinsections of a kind of novelty of Dow AgroSciences's exploitation, are the second generation product of pleocidin.He has well solved the good disinsection effect of pleocidin to vegetable crop; But unfavorable problem is controlled in the insect pest of crops such as fruit and nut; The pomaceous fruit heart-eating worm apple olethreutid that especially can not prevent and treat pleocidin has special efficacy, and its insecticidal spectrum is wider than the desinsection of manying element simultaneously.Advantages such as in addition, it also has main useful insect influence littler, and the unit are consumption is lower, and residual life is short in environment obtain 2008 " US President's green chemical challenge prize ".Its composition structural formula is:
Figure BDA0000110118840000011
Ethyl pleocidin is spinosyn J and the spinosyn L desinsection chlorins compound more than two kinds that is produced by fermentation, in the presence of catalyzer, reactant and solvent, and the novel pesticide that the process chemical modification finally obtains.Its mechanism of action is different from traditional organic phosphor and pyrethroid insecticides acts on acetylcholinesterase and Na +Passage, it is to act on nAChR, and is also variant with nicotinic insecticides such as Imidacloprids.It can be applied to fruit, nut, grape vine, cereal, soybean and greengrocery crop at present.Not only effective to fruit such as Lepidoptera, diptera, coleoptera, thrips and Homoptera, vegetable-crop pest-insect; And to preventing and treating the pest efficient of standard fruit-tree and nut etc.; Aspect insecticidal activity, it is plain that the insecticidal activity that ethyl pleocidin is selected various common economic crops insect pests such as tikka, beet armyworm, cabbage looper, sweet potato whitefly, leaf roller and cotton bollworm to tobacco budworm, cotten aphid, two is higher than many desinsections far away.
Amide-type insecticide of the present invention mainly comprises azoles insect amide, flonicamid, fipronil bisamide, chlorine insect amide; Their mechanism of action is basic identical; Mainly be to activate blue Buddhist nun's alkali acceptor, discharge the calcium ion of storing in smooth muscle and the striated muscle cell, cause that the muscle adjusting is weak; Paralysis, dead until last insect.This active ingredient shows mammal and the extremely significant selective difference of the blue Buddhist nun's alkali of insect acceptor, has improved greatly mammal and other vertebrate safeties.The O-formammidotiazol-benzamide insecticide all has excellent control effect to lepidopterous Noctuidae, Pyralidae, moth fruit moth section, tortricid, miller section, diamond-back moth section, Gracilariidae etc., can also control multiple non-lepidoptera pests such as coleoptera Culculionidae, Chrysomelidae, diptera Agromyzidae, Bemisia tabaci.
The above-mentioned amide-type insecticide of mentioning has very outstanding preventive effect to larva, but shortcoming is very limited to the adult control efficiency, does not have ovicidal action basically, and interior suction conduction is not strong yet.And use the agent of a kind of insecticide list for a long time, insect is easy to generate pesticide resistance, and the consumption of insecticide is increased; Medication increased frequency repeatedly; Increase the desinsection cost, and contaminated environment increases, last whole structure show as high poison, consumption big, residual many, drug effect is poor.If but both do not had cross resistance with two kinds; The agricultural chemicals that the mechanism of action there are differences is again attempted carrying out rationally composite, can finely overcome the above problems, and the initiative of the relative noval chemical compound of research in agriculture chemical compounding field wants the cycle shorter; Drop into lower; Also produce result than being easier to, it is little to meet present Chinese pesticide industry scope of the enterprise, the present situation that research and development have high input and can't support.But can carry out composite between not all agricultural chemicals; Every kind of agricultural chemicals all has physicochemical property parameter and the characteristic of oneself; Whether have compatibility between the agricultural chemicals, whether can be prepared into and be convenient to the formulations of pesticide that agricultural chemicals uses, whether have obvious synergistic effect; Whether having alleviated harm to environment or the like greatly, all is the problem that the research staff need consider and probe in R&D process.
Summary of the invention
Under above technical background,, make full use of two kinds of composite synergistic effects that produce of active component in order to satisfy the needs of pesticide producing; Enlarge insecticidal spectrum; Raising is to the preventive effect of insect, reduces agricultural cost and delays the generation of pest resistance to insecticide, and a kind of insecticide pesticide of environment-friendly high-efficiency more is provided.When I research staff of company carries out composite research between to the agricultural chemicals of different effects mechanism; Chance on; With in novel biological species agricultural chemicals ethyl pleocidin and four kinds of amides pesticide azoles insect amides, flonicamid, fipronil bisamide, the chlorine insect amide one of any carry out composite in twos; The interior absorption that can solve amide-type well strong with kill adult, kill the problem of ovum weak effect, to give full play to the problem of the stable and environmental protection of biological species agricultural chemicals.
Specifically; Promptly the present invention proposes a kind of new insecticides: said composition contains A, two kinds of active ingredients of B; Effective constituents A is selected from new bio class agricultural chemicals ethyl pleocidin, and active ingredient B is selected from four kinds of amide-type insecticide azoles insect amides, flonicamid, fipronil bisamide, the chlorine insect amide one of any.This Pesticidal combination has the notable synergistic effect, and dosage is few, and preventive effect is high, more environmental protection, and single composite between ethyl pleocidin and four kinds of amides pesticides do not see relevant report so far.
Composite between two kinds of active ingredient is one of key character of the present invention, and wherein the mass percent of the effective constituents A described in the present invention (ethyl pleocidin) and active ingredient B one of (in azoles insect amide, flonicamid, fipronil bisamide, the chlorine insect amide any) is 1~90: 90~1.Two kinds of compounds composite all shows certain synergistic effect in this scope.In the experiment later stage, we again emphasis done some specific aim proportioning screening tests of proportioning among a small circle, on this basis, we can be preferably 1~45 with the mass percent of two kinds of effective active composition A in the Pesticidal combination of the present invention and B: 60~3.
It is aqueous emulsion, microemulsion, missible oil, suspending agent, wetting powder, microcapsule suspending agent, water dispersible granules that another important technology of Pesticidal combination of the present invention is characterized as the formulations of pesticide that Pesticidal combination of the present invention can be prepared into.Wherein in pesticidal preparations, it is 1%-90% that the gross mass of two kinds of active ingredients accounts for total formulation gross mass percentage, preferred 5%-60%; All the other components are the relevant complementary component of usual auxiliaries and formulation preparation in the agricultural chemicals.
Wherein necessary component and the easy manufacture implementation method about the said composition formulations of pesticide is following in addition:
When Pesticidal combination of the present invention was wetting powder, the mass percent of component was: ethyl pleocidin 1~90%, and active ingredient B 1~90%; Dispersant 3~20%, wetting agent 3~10%, filler 10~70%; Press above-mentioned prescription with ethyl pleocidin and active ingredient B and dispersant, wetting agent and filler mixing; In stirred tank, evenly stir, behind airslide disintegrating mill, mixing, promptly can be made into the wetting powder of the present composition.
When Pesticidal combination of the present invention was suspending agent, the mass percent of component was: ethyl pleocidin 1~90%, and active ingredient B 1~90%; Dispersant 5~20%, antifreezing agent 1~5%, thickener 0.1~2%; Antifoaming agent 0.1~0.8%, water surplus is supplied, and earlier other auxiliary agents is mixed; Mix through high speed shear, add ethyl pleocidin and active ingredient B, abrading-ball is 2~3 hours in ball crusher; Make a diameter all below 5mm, make the suspending agent preparation of Pesticidal combination of the present invention.
When Pesticidal combination of the present invention was aqueous emulsion, the mass percent of component was: ethyl pleocidin 1~90%, and active ingredient B 1~90%; Emulsifier 3~30%, solvent 5~15%, stabilizing agent 2~15%; Antifreezing agent 1~5%; Antifoaming agent 0.1~8%, thickener 0.2~2%, water is supplied.Former medicine ethyl pleocidin added with active ingredient B, solvent and emulsifier, cosolvent be in the same place, make and be dissolved into uniform oil phase; With part water, antifreeze, other insecticides adjuvant such as antimicrobial mixes into uniform aqueous phase; When the agitated reactor high speed stirs, oil phase is added water, slowly add water, open clipper and carry out high speed shear, and add remaining water, shear half an hour approximately, form the aqueous emulsion of oil-in-water type until reaching the phase inversion point.Promptly make the aqueous emulsion of the present composition.
When described Pesticidal combination of the present invention was water dispersible granules, the mass percent of component was: ethyl pleocidin 1~90%, active ingredient B 1~90%, dispersant 3~20%, wetting agent 3~10%, disintegrant 2~5%, filler 10~70%.Ethyl pleocidin, active ingredient B and dispersant, wetting agent, disintegrant and filler are mixed; Pulverize with micro jet; Through mediating; Add then and carry out granulation, drying, screening in the fluidized bed prilling dryer after sample analysis, make the water dispersible granules of the present composition of the present invention.
When Pesticidal combination of the present invention was missible oil, the mass percent of component was: ethyl pleocidin 1~90%, active ingredient B 1~90%, emulsifier 1~15%, solvent complementary component.The missible oil preparation is dissolved in the solvent according to the ethyl pleocidin and the active ingredient B of formula rate with capacity, adds surfactant (using after the heating for dissolving in case of necessity) and other components, mixes and promptly makes the said composition cream preparation.
When Pesticidal combination of the present invention was microemulsion, the mass percent of component was: ethyl pleocidin 1~90%, active ingredient B 1~90%, emulsifier 10~30%, antifreezing agent 1~8%, stabilizing agent 0.5~10%, conventional solvent cosolvent 20~50%.Former medicine ethyl pleocidin, active ingredient B are dissolved with cosolvent fully, add other compositions such as emulsifier, antifreezing agent stabilizing agent again, evenly mix, add entry at last, can be made into microemulsion after fully stirring.
When Pesticidal combination of the present invention was micro-capsule suspension, the mass percent of component was: ethyl pleocidin 1~90%, and active ingredient B 1~90%; Cyst material 1~8%, protection glue 0.1~3%, emulsifier 2~5%; Dispersant 3~5%; Adjuvant 0~14%, water surplus supplies 100%.The former medicine and the wetting dispersing agent of two kinds of compositions are dropped in the proper amount of solvent, then through the sand mill sand milling; An amount of isocyanates cyst material monomer of adding stirs and obtains oil phase in the good material of sand milling; In water, add emulsifier in advance, adjuvant stirs, and adds pre-configured oil phase then, the high speed homogenizing forms the stabilized oil-in-water emulsion; Reduce rotating speed, under the speed conditions that is fit to, add polyamine or polyatomic alcohol water solution and participate in interface polymerization reaction, reaction temperature rises to 20 ℃~65 ℃, keeps 2 hours~24 hours, makes cyst material solidify encystation; After treating into capsule material and solidifying encystation fully, add an amount of dispersant and adjuvant, stir and promptly process the microcapsule suspending agent of this composition.
Described cyst material is a carbamide resin, is to be made through interface polymerization reaction by isocyanates and water or polyamine.
Described protection glue is selected from wherein a kind of of polyvinyl alcohol, gelatin, gum Arabic, xanthans.
Emulsifier described in the preparation of above-mentioned formulation is selected from any one or more mixtures with the arbitrary proportion composition in calcium dodecyl benzene sulfonate and aliphatic acid polyethenoxy ether, APES sulfosuccinate, styryl phenol APEO, NPE, castor oil polyoxyethylene ether, aliphatic acid polyethenoxy base ester, the polyoxyethylene aliphatic alcohol ether.
Said solvent is any one or more mixed solvents formed with arbitrary proportion in xylol or biodiesel, toluene, diesel oil, methyl alcohol, ethanol, n-butanol, isopropyl alcohol, turpentine oil, solvent naphtha, dimethyl formamide, dimethyl sulfoxide (DMSO), water, xylol, aliphatic solvent oil, cyclohexanone, methylated vegetable oil, vegetable oil, mineral oil, aromatic solvent naphtha, N-Methyl pyrrolidone, carrene, methyl-sulfoxide, the benzinum equal solvent.
Described dispersant is selected from one or more in polycarboxylate, lignosulfonates, APES formaldehyde condensation products sulphate, alkyl benzene sulfonate calcium salt, naphthalene sulfonic acid-formaldehyde condensation product sodium salt, APES, aliphatic amine polyoxyethylene ether, polyoxyethylene carboxylate, the fatty acid glyceride APEO.
Described wetting agent is selected from: lauryl sodium sulfate, calcium dodecyl benzene sulfonate, draw back in powder active ingredient BX., wetting and penetrating agent F, alkylnaphthalene sulfonate, polyoxyethylene triphenylethylene phosphenylic acid salt, spaonin powder, silkworm excrement, the soapberry powder one or more.
Described disintegrant is selected from: one or more in bentonite, urea, ammonium sulfate, aluminium chloride, citric acid, succinic acid, the sodium bicarbonate.
Described thickener is selected from: one or more in xanthans, CMC, hydroxyethylcellulose, methylcellulose, Magnesiumaluminumsilicate, the polyvinyl alcohol.
Described stabilizing agent is selected from: a kind of in sodium citrate, the resorcinol.
Described antifreezing agent is selected from: one or more in ethylene glycol, propane diols, the glycerine.
Described antifoaming agent is selected from: silicone oil, silicone compound, C 10-20Saturated fat acid compounds, C 8-10In the aliphatic alcohols compound one or more.
Described sterilization antiseptic is selected from a kind of in potassium sorbate, Sodium Benzoate, formaldehyde, the isothiazolinone;
Described filler is selected from: one or more in kaolin, diatomite, bentonite, attapulgite, white carbon, starch, the precipitated calcium carbonate.
For example tobacco budworm, cotten aphid, two select various common economic crops insect pests such as tikka, beet armyworm, cabbage looper, sweet potato whitefly, leaf roller and cotton bollworm to agricultural insecticide composition of the present invention some other insects of control; And some ground plant stem-leaf insects; The pale brown thrips of thrips, onion thrips, flower thrips, the red aphid of the peach of Semiptera, cotten aphid, rice leafhopper, rice small brown rice planthopper, greenhouse whitefly; Lepidoptera has diamond-back moth, tomato moth, beet armyworm, striped rice borer, corn borer, cotton bollworm, cotton leafroller; The potato bug of coleoptera, America rice silk worm; The dipterous beans fly of diving; Underground plant root insect, the African mole cricket of orthoptera, the strawberry radical bud of Semiptera, lepidopterous black cutworn, Huang Dihu, the big green rutelian larva of coleoptera, yellow bent flea beetle larva, America rice silk worm, northern corn root-worm, bellicose first; Diptera has kind of a fly larva.The two-spotted spider mite of mite class, citrus red mite, citrus rust mite etc., insecticidal activity is all higher.
Pesticidal combination of the present invention has obvious synergistic effect, can reduce effective ingredient consumption, reduces cost, and delays the generation of pest resistance to insecticide, the low and easy decomposition of residue of pesticide, and environmental protection more is a kind of environmentally friendly highly effective pesticide.And preventive effect is remarkable in the time of aspect Homoptera suckings pest such as lepidopterous insects such as control diamond-back moth, beet armyworm, prodenia litura, cotton bollworm, mealybug class and aphid, tea lesser leafhopper.
Embodiment
In order to make the object of the invention, technical scheme and advantage clearer, the present invention describes with following specific embodiment, but the present invention is limited to these examples absolutely not.The following stated is merely the present invention embodiment preferably, only is used to explain the present invention, can not therefore be interpreted as the restriction to claim of the present invention.Should be pointed out that all any modifications of within spirit of the present invention and principle, being made, be equal to replacement and improvement etc., all should be included within protection scope of the present invention.Therefore, the protection domain of patent of the present invention should be as the criterion with appended claims.
Crop sequences is applicable to the different formulations of pesticide, and the researcher of these formulations of pesticide technical field can be made into the formulations of pesticide that adapt, and its simple component and embodiment are following:
The formulation embodiment:
Embodiment 1: the processing and the embodiment of ethyl pleocidin and Rynaxypyr suspending agent
Ethyl pleocidin 18g, Rynaxypyr 15g, sodium lignin sulfonate 6g, ethylene glycol 3g; Xanthans 5g, silicone oil 1g, water surplus complements to 300g; Other auxiliary agents are mixed, mix, add ethyl pleocidin and Rynaxypyr through high speed shear; Abrading-ball is 2~3 hours in ball crusher, makes a diameter all below 5mm, makes the suspending agent preparation that contains the Pesticidal combination of ethyl pleocidin and Rynaxypyr of the present invention.
Ethyl pleocidin 1g, Rynaxypyr 30g, sodium lignin sulfonate 9g, ethylene glycol 2g; Xanthans 3g, silicone oil 1g, water surplus complements to 100g; Other auxiliary agents are mixed, mix, add ethyl pleocidin and Rynaxypyr through high speed shear; Abrading-ball is 2~3 hours in ball crusher, makes a diameter all below 5mm, makes the suspending agent preparation that contains the Pesticidal combination of ethyl pleocidin and Rynaxypyr of the present invention.
Ethyl pleocidin 30g, Rynaxypyr 3g, sodium lignin sulfonate 8g, ethylene glycol 2.5g; Xanthans 3g, silicone oil 1g, water surplus complements to 100g; Other auxiliary agents are mixed, mix, add ethyl pleocidin and Rynaxypyr through high speed shear; Abrading-ball is 2~3 hours in ball crusher, makes a diameter all below 5mm, makes the suspending agent preparation that contains the Pesticidal combination of ethyl pleocidin and Rynaxypyr of the present invention.
Embodiment 2: the processing and the embodiment of ethyl pleocidin and fipronil bisamide aqueous emulsion
Ethyl pleocidin 5g, fipronil bisamide 7g, polyoxyethylene aliphatic alcohol ether 4g, carrene 8g, sodium citrate 4g, ethylene glycol 3g, silicone oil 2g, xanthans 4g, water complements to 100g.Former medicine ethyl pleocidin added with fipronil bisamide, solvent and emulsifier, cosolvent be in the same place, make and be dissolved into uniform oil phase; With part water, antifreeze, other insecticides adjuvant such as antimicrobial mixes into uniform aqueous phase; When the agitated reactor high speed stirs, oil phase is added water, slowly add water, open clipper and carry out high speed shear, and add remaining water, shear half an hour approximately, form the aqueous emulsion of oil-in-water type until reaching the phase inversion point.Promptly make the aqueous emulsion of the Pesticidal combination that contains ethyl pleocidin and fipronil bisamide.
Embodiment 3: the processing and the embodiment of ethyl pleocidin and flonicamid water dispersible granules
Ethyl pleocidin 5g, flonicamid 8g, sodium lignin sulfonate 3.5g, spaonin powder 5g, citric acid 4g, white carbon 78g.Ethyl pleocidin, flonicamid and dispersant, wetting agent, disintegrant and filler are mixed; Pulverize with micro jet; Through mediating; Add then and carry out granulation, drying, screening in the fluidized bed prilling dryer after sample analysis makes the water dispersible granules that contains the Pesticidal combination of ethyl pleocidin and flonicamid of the present invention.
Ethyl pleocidin 3g, flonicamid 20g, sodium lignin sulfonate 6g, spaonin powder 7g, citric acid 5g, white carbon 60g.Ethyl pleocidin, flonicamid and dispersant, wetting agent, disintegrant and filler are mixed; Pulverize with micro jet; Through mediating; Add then and carry out granulation, drying, screening in the fluidized bed prilling dryer after sample analysis makes the water dispersible granules that contains the Pesticidal combination of ethyl pleocidin and flonicamid of the present invention.
Ethyl pleocidin 15g, flonicamid 5g, sodium lignin sulfonate 6.5g, spaonin powder 6.5g, citric acid 4g, white carbon 63g.Ethyl pleocidin, flonicamid and dispersant, wetting agent, disintegrant and filler are mixed; Pulverize with micro jet; Through mediating; Add then and carry out granulation, drying, screening in the fluidized bed prilling dryer after sample analysis makes the water dispersible granules that contains the Pesticidal combination of ethyl pleocidin and flonicamid of the present invention.
Embodiment 4: the processing and the embodiment of ethyl pleocidin and azoles insect amide missible oil
Ethyl pleocidin 5g, azoles insect amide 8g, calcium dodecyl benzene sulfonate 4g, aliphatic acid polyethenoxy ether 3g, toluene, xylol are supplied 100g.Be dissolved in the solvent according to the ethyl pleocidin and the azoles insect amide of formula rate, add surfactant (using after the heating for dissolving in case of necessity) and other components, mix and promptly make the said composition cream preparation capacity.
Embodiment 5: the processing and the embodiment of ethyl pleocidin and fipronil bisamide wetting powder
Ethyl pleocidin 6g, fipronil bisamide 9g, sodium lignin sulfonate 6g; Lauryl sodium sulfate 5g; White carbon 74g, evenly stirs in stirred tank ethyl pleocidin and fipronil bisamide and sodium lignin sulfonate, lauryl sodium sulfate and white carbon mixing by above-mentioned prescription; Behind airslide disintegrating mill, mixing, promptly can be made into the wetting powder of the present composition.
Embodiment 6: the processing and the embodiment of ethyl pleocidin and Rynaxypyr microemulsion
Ethyl pleocidin 4g, Rynaxypyr 7g, aliphatic acid polyethenoxy ether 6g, ethylene glycol 4g, sodium citrate 3g, conventional solvent cosolvent 20g.Former medicine ethyl pleocidin, Rynaxypyr are dissolved with cosolvent fully, add other compositions such as emulsifier, antifreezing agent stabilizing agent again, evenly mix, add entry at last, can be made into microemulsion after fully stirring.
Embodiment 7: the processing and the embodiment of ethyl pleocidin and Rynaxypyr microcapsule suspending agent
Ethyl pleocidin 4g, Rynaxypyr 8g, carbamide resin 4g, xanthans 4g, aliphatic acid polyethenoxy ether 5g, sodium lignin sulfonate 4g, adjuvant 7g, water surplus is supplied 100g.The former medicine and the spaonin powder of two kinds of compositions are dropped in the proper amount of solvent, then through the sand mill sand milling; An amount of isocyanates cyst material monomer of adding stirs and obtains oil phase in the good material of sand milling; In water, add aliphatic acid polyethenoxy ether in advance, adjuvant stirs, and adds pre-configured oil phase then, the high speed homogenizing forms the stabilized oil-in-water emulsion; Reduce rotating speed, under the speed conditions that is fit to, add polyamine or polyatomic alcohol water solution and participate in interface polymerization reaction, reaction temperature rises to 20 ℃~65 ℃, keeps 2 hours~24 hours, makes cyst material solidify encystation; After treating into capsule material and solidifying encystation fully, add an amount of sodium lignin sulfonate and adjuvant, stir and promptly process the microcapsule suspending agent of this composition.
Ethyl pleocidin 5g, Rynaxypyr 16g, carbamide resin 6g, xanthans 7g, aliphatic acid polyethenoxy ether 7g, sodium lignin sulfonate 8g, adjuvant 7g, water surplus is supplied 100g.The former medicine and the spaonin powder of two kinds of compositions are dropped in the proper amount of solvent, then through the sand mill sand milling; An amount of isocyanates cyst material monomer of adding stirs and obtains oil phase in the good material of sand milling; In water, add aliphatic acid polyethenoxy ether in advance, adjuvant stirs, and adds pre-configured oil phase then, the high speed homogenizing forms the stabilized oil-in-water emulsion; Reduce rotating speed, under the speed conditions that is fit to, add polyamine or polyatomic alcohol water solution and participate in interface polymerization reaction, reaction temperature rises to 20 ℃~65 ℃, keeps 2 hours~24 hours, makes cyst material solidify encystation; After treating into capsule material and solidifying encystation fully, add an amount of sodium lignin sulfonate and adjuvant, stir and promptly process the microcapsule suspending agent of this composition.
Ethyl pleocidin 18g, Rynaxypyr 4g, carbamide resin 8g, xanthans 6g, aliphatic acid polyethenoxy ether 8g, sodium lignin sulfonate 9g, adjuvant 5g, water surplus is supplied 100g.The former medicine and the spaonin powder of two kinds of compositions are dropped in the proper amount of solvent, then through the sand mill sand milling; An amount of isocyanates cyst material monomer of adding stirs and obtains oil phase in the good material of sand milling; In water, add aliphatic acid polyethenoxy ether in advance, adjuvant stirs, and adds pre-configured oil phase then, the high speed homogenizing forms the stabilized oil-in-water emulsion; Reduce rotating speed, under the speed conditions that is fit to, add polyamine or polyatomic alcohol water solution and participate in interface polymerization reaction, reaction temperature rises to 20 ℃~65 ℃, keeps 2 hours~24 hours, makes cyst material solidify encystation; After treating into capsule material and solidifying encystation fully, add an amount of sodium lignin sulfonate and adjuvant, stir and promptly process the microcapsule suspending agent of this composition.
Above formulation embodiment is illustrating of preparation just, can not simply be interpreted as these, and for example ethyl pleocidin all can be prepared into suspending agent with four kinds of amides compounds mentioning, and content shows crop and the pest control of location and decides.The real protection scope of patent of the present invention should be as the criterion with the protection of the formulation in the appended claims.
Indoor biometrics screening and field experiment:
The method that the present invention adopts indoor bioassay and field trial to combine goes to prove the synergistic effect of the present composition.If no special instructions, the ratio of below mentioning (comprising percentage) all is a mass ratio.
Determination of activity instance 1:
(1) test medicine
The former medicine of 81.2% ethyl pleocidin, The Dow Agrosciences, LLC., the former medicine of 95.3% chlorine insect amide, Shanghai Dubang Agricultural Chemicals Co., Ltd..
Earlier with the former medicine of acetone solution, according to the result of preliminary experiment two an amount of former medicines are made into 5 different proportionings, it is for use with acetone each processing to be diluted to 5 series concentration gradients respectively again.
(2) subjects
Indoor Turnip Sprouts are raised continuously the third-instar larvae of the diamond-back moth in 10 generations, temperature (25 ± 2) ℃, relative moisture 50% ± 4%, periodicity of illumination 14/10h (L/D).
(3) test method
Adopt dip method with two former medicines all with the small amount of acetone dissolving, be diluted to into 5 dense solution of equal difference again with 0.1% Tween solution, be diluted in the beaker with subsequent use, and with clear water as contrast.With of the same size three age diamondback moth larvae in the soup that soaks the worm cage, flood 5S, inhale and to go to be placed in the culture dish that diameter is 9cm behind the unnecessary soup, be placed with fresh cabbage leaves in the ware and add a cover.Every concentration is handled 10, repeats 4 times, establishes blank, in (27 ± 1) ℃ illumination box, keeps checking lethality behind the 24h, uses group pin to touch the polypide nonresponder and is death.Lethality is used the Abbott formula correction, again according to the concentration logarithm---and the lethality probit value is analyzed (Bliss) method, obtains virulence regression equation and puts dead middle amount LC 50Value.
(4) data statistics and analysis
According to the toxicity test result of single agent, be 8% quality than ethyl pleocidin by active ingredient: the chlorine insect amide was respectively 2: 6,3: 5,4: 4,5: 3,6: 2.Adopt above-mentioned 1.3 methods to carry out toxicity test, calculate LC 50, and press the abundant method of Sun Yun and calculate co-toxicity coefficient (CTC).Co-toxicity coefficient CTC, computing formula is following: (with the chlorine insect amide is the standard medicament, and its toxicity index is 100):
The LC of the toxicity index of ethyl pleocidin (TI)=chlorine insect amide 50The LC of/ethyl pleocidin 50* 100
The LC of actual toxicity index (ATI)=chlorine insect amide of M 50The LC of/M 50* 100
TI * P the ethyl pleocidin of the TI of theoretical toxicity index (TTI)=chlorine insect amide of M * P chlorine insect amide+ethyl pleocidin
TTI * 100 of the ATI/M of the co-toxicity coefficient of M (CTC)=M
In the formula:
M is an ethyl pleocidin and the mixture of the different proportionings of chlorine insect amide
The P ethyl pleocidin is ethyl pleocidin shared ratio in mixture
P chlorine insect amide is chlorine insect amide shared ratio in mixture
(5) toxicity test result and analysis
Table 1 chlorine insect amide, ethyl pleocidin are to the indoor measurement result of diamond-back moth
Figure BDA0000110118840000091
Can find out that from table in being mixed of different proportion, its co-toxicity coefficient shows certain synergistic effect, wherein ethyl pleocidin all greater than 120: the chlorine insect amide is that synergistic effect in 3: 5 o'clock is the most obvious, and co-toxicity coefficient is 183.02.Result of the test shows; Ethyl pleocidin, two kinds of medicaments of chlorine insect amide all have higher activity to diamond-back moth under indoor conditions; The result of the test of different proportionings shows, in active ingredient ratio ethyl pleocidin: the chlorine insect amide is when testing respectively in 2: 6,3: 5,4: 4,5: 3,6: 2, all shows stronger synergistic effect; Wherein with ethyl pleocidin: the chlorine insect amide is 3: 5 o'clock, and synergistic effect is best.Suggestion is carried out further field control effectiveness test to the mixture preparation of 3: 5 left and right sides scopes of suitable proportion, to estimate its field practical application effect.
Experimental example 2, same former medicine and target are provided with different component and whether have synergistic effect with checking, and experimental technique is also roughly the same.
Result and analysis:
Table 2 chlorine insect amide, ethyl pleocidin are to the indoor measurement result of diamond-back moth
Figure BDA0000110118840000101
Can find out that from table 2 in being mixed of different proportion, its co-toxicity coefficient shows certain synergistic effect, wherein ethyl pleocidin all greater than 120: the chlorine insect amide is that synergistic effect in 14: 36 o'clock is the most obvious, and co-toxicity coefficient is 168.71.
Determination of activity instance 2:
(1) experiment supplies the reagent agent
The former medicine of 81.2% ethyl pleocidin, The Dow Agrosciences, LLC., 98% azoles insect amide, Nihon Nihyaku Co., Ltd.
(2) test target
The indoor diamond-back moth of for many generations raising, indoor conditions: temperature (26 ± 2) ℃, relative moisture 70% ± 5%, periodicity of illumination 16/8h (L/D).
Experimental technique is with determination of activity instance 1
(3) toxicity test result and analysis:
Table 3 ethyl pleocidin, azoles insect amide are to the indoor measurement result of diamond-back moth
Figure BDA0000110118840000102
Can find out that from table in being mixed of different proportion, its co-toxicity coefficient shows certain synergistic effect, wherein ethyl pleocidin all greater than 120: the azoles insect amide is that 4: 8 synergistic effect is the most obvious, and co-toxicity coefficient is 181.83.Result of the test shows; Ethyl pleocidin, two kinds of medicaments of azoles insect amide all have higher activity to beet armyworm under indoor conditions; The result of the test of different proportion proportioning shows, in active ingredient ratio ethyl pleocidin: the azoles insect amide all shows stronger synergistic effect when diluting respectively; Wherein with ethyl pleocidin: the azoles insect amide is 4: 8 o'clock, and synergistic effect is best.Suggestion is carried out further field control effectiveness test to the mixture preparation of 4: 8 left and right sides scopes of suitable proportion, to estimate its field practical application effect.
Experimental example 2, same former medicine and target are provided with different component and whether have synergistic effect with checking, and experimental technique is also roughly the same.
Result and analysis:
Table 4 ethyl pleocidin, azoles insect amide are to the indoor measurement result of diamond-back moth
Figure BDA0000110118840000111
Can find out that from table in being mixed of different proportion, its co-toxicity coefficient shows certain synergistic effect, wherein ethyl pleocidin all greater than 120: the azoles insect amide is that 15: 35 synergistic effect is the most obvious, and co-toxicity coefficient is 188.77.
Determination of activity instance 3:
(1) experiment supplies the reagent agent
The former medicine of 81.2% ethyl pleocidin, The Dow Agrosciences, LLC., 95% fipronil bisamide, Bayer crop science Co., Ltd.
(2) test target
The indoor apple olethreutid of for many generations raising, indoor conditions: temperature (26 ± 2) ℃, relative moisture 70% ± 5%, periodicity of illumination 16/8h (L/D).
Experimental technique is with determination of activity instance 1
(3) toxicity test result and analysis:
Table 5 ethyl pleocidin, fipronil bisamide are to the indoor measurement result of apple olethreutid
Figure BDA0000110118840000112
Figure BDA0000110118840000121
Can find out that from table in being mixed of different proportion, its co-toxicity coefficient shows certain synergistic effect, wherein ethyl pleocidin all greater than 120: fipronil bisamide is that 5: 11 synergistic effect is the most obvious, and co-toxicity coefficient is 181.36.Result of the test shows; Ethyl pleocidin, two kinds of medicaments of fipronil bisamide all have higher activity to the apple olethreutid under indoor conditions, and the result of the test of different proportionings shows, by the active ingredient ethyl pleocidin: fipronil bisamide is when diluting respectively; All show stronger synergistic effect; Wherein with ethyl pleocidin: fipronil bisamide is 5: 11 o'clock, and synergistic effect is best, is ethyl pleocidin secondly: fipronil bisamide 7: 9; Suggestion is to suitable proportion 5: 11-7: the mixture preparation of 9 left and right sides scopes carries out further field control effectiveness test, to estimate its field practical application effect.
Experimental example 2, same former medicine and target are provided with different component and whether have synergistic effect with checking, and experimental technique is also roughly the same.
Result and analysis:
Table 6 ethyl pleocidin, fipronil bisamide are to the indoor measurement result of apple olethreutid
Can find out that from table in being mixed of different proportion, its co-toxicity coefficient shows certain synergistic effect, wherein ethyl pleocidin all greater than 120: fipronil bisamide is that 24: 26 synergistic effect is the most obvious, and co-toxicity coefficient is 174.51.
Determination of activity instance 4:
(1) experiment supplies the reagent agent
The former medicine of 81.2% ethyl pleocidin, The Dow Agrosciences, LLC., 96% flonicamid, Japanese Ishihara Sangyo Kaisha, Ltd..
(2) test target
Apple aphid is taken from apple orchard, Yantai City, Shandong Province, and it is consistent to get size, and it is subsequent use not execute the young aphid of any agricultural chemicals.
Experimental technique is with determination of activity instance 1
(3) toxicity test result and analysis:
Table 7 ethyl pleocidin, flonicamid are to the indoor measurement result of apple aphid
Figure BDA0000110118840000123
Figure BDA0000110118840000131
Can find out that from table in being mixed of different proportion, its co-toxicity coefficient shows certain synergistic effect, wherein ethyl pleocidin all greater than 120: flonicamid is that 5: 8 synergistic effect is the most obvious, and co-toxicity coefficient is 193.99.Result of the test shows; Ethyl pleocidin, two kinds of medicaments of flonicamid all have higher activity to apple aphid under indoor conditions; The result of the test of different proportionings shows, by the active ingredient ethyl pleocidin: when flonicamid dilutes respectively, all show stronger synergistic effect; Wherein with ethyl pleocidin: flonicamid is 5: 8 o'clock, and synergistic effect is best.Suggestion is carried out further field control effectiveness test to the mixture preparation of 5: 8 left and right sides scopes of suitable proportion, to estimate its field practical application effect.
Experimental example 2, same former medicine and target are provided with different component and whether have synergistic effect with checking, and experimental technique is also roughly the same.
Result and analysis:
Table 8 ethyl pleocidin, flonicamid are to the indoor measurement result of apple aphid
Figure BDA0000110118840000132
Can find out that from table in being mixed of different proportion, its co-toxicity coefficient shows certain synergistic effect, wherein ethyl pleocidin all greater than 120: flonicamid is that synergistic effect in 25: 25 o'clock is the most obvious, and co-toxicity coefficient is 165.25.
Test Example 1 field experiment control beet armyworm
(1) test method
Test that the suburb truck garden carries out in Kaiping City, Guangdong Province on October 9th, 2010 to October 19.Tested on October 9th, 2010 and carry out routine to water spray by each processing design concentration.Spraying equipment is a WF-16 type knapsack hand sprayer, and shower nozzle is single fan nozzle, and operating pressure is 0.2-0.4Mpa, and spray amount is 0.36-0.48L/min, carries out the routine spraying, makes every effort to evenly thoughtful during the spray medicine.The field beet armyworm is 1~2 instar larvae peak period during dispenser, every 667m 2To the water yield is 70kg.
Duration of test weather is good, and daily mean temperature is 18.5~27.9 ℃.Dispenser was fine the same day.
(2) control time and method
Before dispenser in every sub-district by 5 samplings of diagonal. every wild cabbage 8~12 strain of choosing beet armyworm ovum and larva (look insect density and decide).Statistics is demarcated beet exigua larvae head number in the strain. with this as dispenser before the insect population radix.In after the dispenser the 3rd, 7,10d investigates the beet exigua larvae number of deciding residual survival in the strain respectively. go down rate as control efficiency to proofread and correct insect population.
(3) drug effect computational methods
Figure BDA0000110118840000141
Figure BDA0000110118840000142
(4) poisoning investigation method
Duration of test is observed and is respectively handled sub-district wild cabbage well-grown, and all not finding has the poisoning phenomenon to take place.
(5) field control effectiveness test result of the test
Table 9 is handled chemical control wild cabbage beet armyworm field control effectiveness test result
Can find out that from table 9 Mixed Pharmacy of different proportion carries out field experiment by different consumptions; Its control efficiency to the wild cabbage beet armyworm all is superior to contrasting medicament behind the medicine; 5% ethyl pleocidin+11% fipronil bisamide control beet armyworm quick-acting is fast, and efficiency time is long, and control efficiency is good.7 days insecticidal effect reaches 94.34%, 93.79%, 92.26% insecticidal effect respectively and increases progressively along with the increase of consumption behind medicine.According to experimental observation, each medication is handled does not all have poisoning to wild cabbage, finds that it also has the better prevention effect to insects such as diamond-back moths simultaneously yet.Suggestion was grasped at beet exigua larvae before 3 ages in dispenser period, required even spraying during dispenser, the positive and negative of leaf even medicine, advise that the medicament different with other mechanisms of action is used alternatingly, to delay the generation of pest resistance to insecticide.
Test Example 2: field experiment control diamond-back moth
(1) test method
Test is sprayed medicine 1 time altogether, and the dispenser date is June 21.Wild cabbage this moment balling not as yet.The diamondback moth larvae major part was in for 2~3 length of times.Weather is cloudy calm during the spray medicine.With sharp agricultural board level pressure knapsack hand sprayer each is handled even spraying, leave dual sides all requires to be sprayed with the effect soup, and soup 2L is used in every sub-district.
(2) investigation method
Investigate the fixing 15 strain wild cabbages in each sub-district as the investigation strain, write down the larva quantity on whole blades.Investigation insect population radix before the spray medicine, 3,7 days and investigation in the 10 days borer population of living behind the spray medicine respectively, this test is investigated 4 times altogether.
(3) drug effect computational methods
Insect population borer population * the l00 that lives before rate (%)=(borer population of living after borer population one dispenser of living before the dispenser)/dispenser that goes down
Preventive effect (%)=(the treatment region insect population rate of going down-check plot insect population go down rate)/(100-according to district's insect population go down rate) * 100
(4) poisoning investigation method
Continuous 10d range estimation medicament does not have poisoning to produce the wild cabbage well-grown to crop after the dispenser.
(5) field control effectiveness test result of the test
Table 10 is handled chemical control diamond-back moth field control effectiveness test result
Figure BDA0000110118840000151
Can find out that from table 10 Mixed Pharmacy of different proportion carries out field experiment by different consumptions; Its control efficiency to the wild cabbage diamond-back moth all is superior to contrasting medicament behind the medicine; And the lasting period is long, 3% ethyl pleocidin+5% chlorine insect amide behind medicine 7 days, and insecticidal effect is respectively 92.41%, 94.37% and 96.35%; Insecticidal effect increases along with the increase of consumption, and difference reaches extremely remarkable between each consumption processing insecticidal effect.According to the field range estimation, in the test dose scope, plant growth is normal, and each is handled medicament and the poisoning phenomenon to wild cabbage all do not occur, explains that it is safe to wild cabbage.In process of the test, testing crew finds that it also has favorable effect to insects such as trialeurodes vaporariorums.Suggestion mixes with mechanism of action different insecticide to be used to delay the generation of pest resistance to insecticide.
To sum up result of the test checking several times; The present invention contains one or two yuan of any composite Pesticidal combination in ethyl pleocidin and four kinds of amides compound azoles insect amides, flonicamid, fipronil bisamide, the chlorine insect amide; Anti-eliminate aphis, Homoptera sucking pest such as leafhopper and during to lepidopterous insects such as diamond-back moth, beet armyworm, prodenia litura, cotton bollworm, mealybug classes preventive effect remarkable; To the target crop safety, to compare with single agent, Pesticidal combination of the present invention has mechanism of action uniqueness; Consumption is few, and quick-acting is good, the lasting period is long, the advantage of environmental protection.So, in research and development of the present invention and popularization the important social meaning is arranged, can produce very big economic benefit.

Claims (5)

1. agricultural insecticidal composite; It is characterized in that: this Pesticidal combination contains two kinds of active ingredients; Wherein effective constituents A is an ethyl pleocidin, and active ingredient B is one of any in azoles insect amide, flonicamid, fipronil bisamide, the chlorine insect amide, and all the other compositions are the complementary component of agricultural chemicals when preparing with relevant auxiliary agent and formulation; The mass percent of effective constituents A in this Pesticidal combination and active ingredient B is 1~90: 90~1, and synergistic effect is all arranged in this proportion.
2. Pesticidal combination according to claim 1 is characterized in that: on the basis of further specific aim prescription screening experiment checking, the mass percent of active ingredient ethyl pleocidin and active ingredient B can further be preferably 1~45: 60~3.
3. according to claim 1 and 2 described Pesticidal combinations, it is characterized in that: this Pesticidal combination can be prepared into the agricultural chemicals common dosage forms, and the gross mass of two kinds of active ingredient ethyl pleocidins and active ingredient B accounts for the 1%-90% of total formulation gross mass in the preparation.
4. Pesticidal combination according to claim 3 is characterized in that: the percentage that the gross mass of active ingredient ethyl pleocidin and active ingredient B accounts for the total formulation gross mass in the preparation of this Pesticidal combination preparation is preferably 5%-60%.
5. according to the described Pesticidal combination of claim 1 to 4, it is characterized in that: the pesticidal preparations formulation that Pesticidal combination of the present invention can be prepared into is aqueous emulsion, microemulsion, missible oil, suspending agent, wetting powder, microcapsule suspending agent, water dispersible granules.
CN2011103689421A 2011-11-18 2011-11-18 Insecticidal composition containing spinetoram and amide pesticides Pending CN102362591A (en)

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Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102726397A (en) * 2012-06-09 2012-10-17 广东中迅农科股份有限公司 Insecticidal composition containing flonicamid and ethyl spinosad
CN102939970A (en) * 2012-10-18 2013-02-27 上海沪联生物药业(夏邑)股份有限公司 Microcapsule suspending agent containing spinosad and cyantraniliprole, and preparation method thereof
CN104106591A (en) * 2013-04-22 2014-10-22 陕西美邦农药有限公司 High-efficiency insecticidal composition containing flubendiamide
CN104663669A (en) * 2013-11-29 2015-06-03 南京华洲药业有限公司 Compound insecticidal composition containing tolfenpxrad and spinetoram and application of compound insecticidal composition
CN108077264A (en) * 2018-02-08 2018-05-29 广东绿银生物科技有限公司 A kind of Pesticidal combination containing ethyl pleocidin and bromine worm fluorobenzene bisamide
CN113907080A (en) * 2021-10-28 2022-01-11 溧阳中南化工有限公司 Insecticide
CN114901074A (en) * 2019-12-31 2022-08-12 阿达玛马克西姆有限公司 Insecticide mixtures

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102726397A (en) * 2012-06-09 2012-10-17 广东中迅农科股份有限公司 Insecticidal composition containing flonicamid and ethyl spinosad
CN102939970A (en) * 2012-10-18 2013-02-27 上海沪联生物药业(夏邑)股份有限公司 Microcapsule suspending agent containing spinosad and cyantraniliprole, and preparation method thereof
CN104106591A (en) * 2013-04-22 2014-10-22 陕西美邦农药有限公司 High-efficiency insecticidal composition containing flubendiamide
CN104663669A (en) * 2013-11-29 2015-06-03 南京华洲药业有限公司 Compound insecticidal composition containing tolfenpxrad and spinetoram and application of compound insecticidal composition
CN108077264A (en) * 2018-02-08 2018-05-29 广东绿银生物科技有限公司 A kind of Pesticidal combination containing ethyl pleocidin and bromine worm fluorobenzene bisamide
CN114901074A (en) * 2019-12-31 2022-08-12 阿达玛马克西姆有限公司 Insecticide mixtures
CN113907080A (en) * 2021-10-28 2022-01-11 溧阳中南化工有限公司 Insecticide

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