CN102487955A - Spinetoram compounded insecticidal composition - Google Patents

Spinetoram compounded insecticidal composition Download PDF

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CN102487955A
CN102487955A CN2011103834872A CN201110383487A CN102487955A CN 102487955 A CN102487955 A CN 102487955A CN 2011103834872 A CN2011103834872 A CN 2011103834872A CN 201110383487 A CN201110383487 A CN 201110383487A CN 102487955 A CN102487955 A CN 102487955A
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ethyl pleocidin
active ingredient
spinetoram
pesticidal combination
urea
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葛大鹏
杜秀斌
杨波涛
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JIANGXI HAIKE RUITE CROP SCIENCE CO Ltd
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JIANGXI HAIKE RUITE CROP SCIENCE CO Ltd
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Abstract

The invention relates to a spinetoram compounded insecticidal composition and belongs to the field of pesticide compounding. Active components of the spinetoram compounded insecticidal composition comprise spinetoram and chitin synthesis inhibitor compounds. A weight percentage of the spinetoram to the chitin synthesis inhibitor compounds is (1 to 90): (90 to 1), and preferably, the weight percentage is (1 to 45): (60 to 3). The spinetoram compounded insecticidal composition comprises 1 to 90% by mass of the active components, and preferably, comprises 3 to 7% by mass of the active components and the balance auxiliary ingredients which can be used in pesticides and are acceptable. The spinetoram compounded insecticidal composition can be processed into emulsion in water, microemulsion, missible oil, a suspending agent, wettable powder and water dispersible granules by known methods. The spinetoram compounded insecticidal composition has the advantage that through the active components of spinetoram and the chitin synthesis inhibitor compounds, control of lepidopterous, thysanopterous and homopterous pests such as cnaphalocrocis medinalis guenee, diamondback moth, prodenia litura, cotton bollworm, beet armyworm and thrip is realized.

Description

A kind of and the composite Pesticidal combination of ethyl pleocidin
Technical field
The present invention relates to the agriculture chemical compounding technical field, being specifically related to a kind of is that active ingredient is carried out two yuan of Pesticidal combinations that are mixed with ethyl pleocidin and chitin synthesis inhibitor compounds.
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 BDA0000113105040000011
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.
Described chitin synthesis inhibitor compound is that Buprofezin, Acarus tritici urea, butyl ether urea, fluorine bell urea, fluorine uride, pyrrole worm are grand.
Buprofezin has another name called buprofezin, english common name buprofezin, chemical name 2-Te-Ding imido grpup-3-isopropyl-5-phenyl-3,4,5,6-tetrahydrochysene-2H-1,3,5-thiadiazine-4-ketone, molecular formula: C 16H 23N 3OS.Structural formula is:
Figure BDA0000113105040000021
Buprofezin is a kind of selective insecticide that insect growth is grown that suppresses, and action of contace poison is strong, and stomach poison function is also arranged.Mechanism of action is synthetic and disturb metabolism for suppressing insect chitin, causes nymph cast off a skin deformity or wing deformity and slowly dead.Double wing purpose plant hopper, leafhopper, aleyrodid and scale insect class pest have good control efficiency, and the drug effect phase is longer, and is safer to natural enemy.Shortcoming is not obvious to homoptera pest adult control efficiency; In addition; Resistance (monitoring for resistance of brown planthopper parathiazine ketone, rice in China science, 2008 that insect parathiazine ketone such as rice fulgorid has produced low-medium level have been found at present; Increased more than one times when 22 (2)), the dosage of field control is than initial the application.
The Acarus tritici urea, chemical name: RS)-and 1-[2,5-two chloro-4-(1,1,2,3,3,3-hexafluoro propoxyl group) phenyl]-3-(2, the 6-difluoro benzoyl) urea, molecular formula: C 17H 8C 12F 8N 2O 3, act on insect larvae, stop the decortication process and kill off the insect pests, especially food leaf caterpillars such as fruit tree there is outstanding preventive effect, thrips, rust mite, trialeurodes vaporariorum there are unique mechanism of killing, be suitable for control to pyrethroid and organophosphorous pesticide generation resistant insect.
Butyl ether urea (Diafenthiuron), C 23H 32N 2OS is a kind of novel Thiourea efficient insecticide, miticide, have tag, stomach toxicity, interior suction and fumigation action, low toxicity, but to fish, the high poison of honeybee.Under ultraviolet light, change material into, have stronger activity having produced serious drug-fast insect on the vegetables with insecticidal activity.Can prevent and treat aphid, aleyrodid, leafhopper, noctuidae pests and evil mite on various crop and the ornamental plants.
Fluorine bell urea, and 1-[3,5-two chloro-4-(1,1; 2,2-tetrafluoro ethyoxyl) phenyl]-3-(2, the 6-difluoro benzoyl) urea, these article belong to the benzoyl urea insecticide; Be chitin synthesis inhibitor, have very high desinsection and ovicidal activity, and quick-acting, especially prevent and treat cotton bollworm.Be used for cotton, potato and fruit tree and prevent and treat multiple coleoptera, diptera, Homoptera insect.
The fluorine uride has the compound of stomach toxicity and action of contace poison simultaneously concurrently, has the insecticidal activity of wide spectrum, and is not only effective to lepidoptera pest, and plant hopper and other class pests are also had activity; Activity to sea ash wing moth 3 instar larvaes at night is suitable with UC 62644 10, is 10 times of Teflubenzuron 11, and B.tabaci ovum and larva are all had good active.
The grand pyridine tick urine that has another name called of pyrrole worm; The fluorine pearl is grand, fluorine pyridine tick urine, chemical name: 1-[4-chloro-3-(3-chloro-5-trifluoromethyl)-2-pyridine oxygen base phenyl)]-3-[2; The 6-difluoro benzoyl] urea; White is to the off-white powder crystallization, and the pyrrole worm is grand to be a kind of parasite growth regulator, and multiple animal body epizoas such as ox, sheep, rabbit are had good killing effect.
Several kinds of chitin synthesis inhibitor compounds recited above, the desinsection selectivity ratios of self is higher, and insecticidal spectrum is narrower, and quick-acting is undesirable, and the lasting period is short.And after using for a long time continuously, insect is easy to generate pesticide resistance, has caused in agricultural production amount ratio bigger, and use cost has also increased the weight of environmental pollution simultaneously than higher.In order to solve the above problem that runs into; Improve the quick-acting and the lasting effect of medicine; Reduce the use cost of agricultural chemicals, we have filtered out ethyl pleocidin and chitin synthesis inhibitor compound and have carried out two yuan of composite composition medicaments on the basis of indoor biometrics experiment screening and field test effect checking; Ethyl pleocidin is the biological species agricultural chemicals; High-efficiency environment friendly has obvious synergistic effect with the chitin compounds is composite, and does not up to now find relevant both composite relevant reports as yet.
Summary of the invention
Based on above technical background; On the basis of the long-time lot of experiments of the research staff of our company; A kind of new insecticides has been proposed, Pesticidal combination promptly of the present invention, said composition contains A, two kinds of effective active compositions of B; Effective constituents A is selected from ethyl pleocidin, and active ingredient B is selected from that chitin synthesis inhibitor compounds Buprofezin, pyrrole worm are grand, one of any in the butyl ether urea, fluorine bell urea, fluorine uride, Acarus tritici urea.Have the notable synergistic effect with these two kinds of composite Pesticidal combinations of active ingredient, have efficient, two outstanding advantages of environmental protection.
Wherein of the present invention with two yuan of composite Pesticidal combinations of effective constituents A (ethyl pleocidin) and active ingredient B one of (Buprofezin, pyrrole worm are grand, any in the butyl ether urea, fluorine bell urea, fluorine uride, Acarus tritici urea); Composite between two kinds of active ingredient is one of key character of the present invention; Has compatibility preferably between ethyl pleocidin and the above-mentioned several kinds of chitin synthesis inhibitor compounds; Can be prepared into some common formulations in the agricultural chemicals, and have obvious synergistic effect between the active ingredient.
The mass percent of two kinds of effective constituents A and B is 1~90: 90~1 in Pesticidal combination of the present invention in addition.Two kinds of compounds composite all shows certain synergistic effect in this scope.In the later stage of experimental study; We again emphasis done the specific aim proportioning screening test in some small scale scopes; 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, 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 3%-70%; 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.
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.
Pesticidal combination of the present invention has obvious synergistic effect; Can reduce effective ingredient consumption, reduce drug cost, delay the generation of pest resistance to insecticide; Effectively reduce environmental pollution and residue of pesticide; Homoptera suckings pest such as lepidopterous insects such as control diamond-back moth, beet armyworm, prodenia litura, cotton bollworm, striped rice borer, mealybug class and plant hopper, aphid, aleyrodid, leafhopper, during insect aspects such as cotton fleahopper, two spotted spider mite, excellent preventive effect is arranged.Especially when the insect of control paddy field, compare existing medicament, the phase price ratio is higher.
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 of ethyl pleocidin and buprofezin suspension agent and embodiment
Ethyl pleocidin 2g, Buprofezin 30g, sodium lignin sulfonate 9g, ethylene glycol 3g; Xanthans 8g, silicone oil 2g, water surplus complements to 100g; Other auxiliary agents are mixed, mix, add ethyl pleocidin and Buprofezin 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 Buprofezin of the present invention.
Ethyl pleocidin 5g, Buprofezin 18g, sodium lignin sulfonate 7g, ethylene glycol 3g; Xanthans 6g, silicone oil 1g, water surplus complements to 100g; Other auxiliary agents are mixed, mix, add ethyl pleocidin and Buprofezin 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 Buprofezin of the present invention.
Ethyl pleocidin 25g, Buprofezin 5g, sodium lignin sulfonate 8g, ethylene glycol 2g; Xanthans 6g, silicone oil 1g, water surplus complements to 100g; Other auxiliary agents are mixed, mix, add ethyl pleocidin and Buprofezin 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 Buprofezin of the present invention.
Embodiment 2: the processing and the embodiment of ethyl pleocidin and butyl ether urea aqueous emulsion
Ethyl pleocidin 4g, butyl ether urea 14g, polyoxyethylene aliphatic alcohol ether 6g, carrene 7g, sodium citrate 3g, ethylene glycol 4g, silicone oil 1g, xanthans 7g, water complements to 100g.Former medicine ethyl pleocidin added with butyl ether urea, 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 butyl ether urea.
Embodiment 3: the processing of ethyl pleocidin and hexaflumuron water dispersible granule and embodiment
Ethyl pleocidin 3g, fluorine bell urea 30g, sodium lignin sulfonate 7g, spaonin powder 8g, citric acid 3g, white carbon 49g.Ethyl pleocidin, fluorine bell urea 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 fluorine bell urea of the present invention.
Ethyl pleocidin 2g, fluorine bell urea 10g, sodium lignin sulfonate 4g, spaonin powder 6g, citric acid 3g, white carbon 75g.Ethyl pleocidin, fluorine bell urea 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 fluorine bell urea of the present invention.
Ethyl pleocidin 30g, fluorine bell urea 3g, sodium lignin sulfonate 9g, spaonin powder 8g, citric acid 5g, white carbon 45g.Ethyl pleocidin, fluorine bell urea 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 fluorine bell urea of the present invention.
Embodiment 4: the processing and the embodiment of ethyl pleocidin and pyrrole worm mamaplasty oil
Ethyl pleocidin 3g, the pyrrole worm is swelled 8g, calcium dodecyl benzene sulfonate 5g, aliphatic acid polyethenoxy ether 4g, toluene, xylol are supplied 100g.With the ethyl pleocidin of capacity with the pyrrole worm is grand is dissolved in the solvent, add surfactant (using after the heating for dissolving in case of necessity) and other components according to formula rate, mix and promptly make the said composition cream preparation.
Embodiment 5: the processing and the embodiment of ethyl pleocidin and Acarus tritici urea missible oil
Ethyl pleocidin 2g, Acarus tritici urea 28g, calcium dodecyl benzene sulfonate 8g, aliphatic acid polyethenoxy ether 7g, toluene, xylol are supplied 100g.Be dissolved in the solvent according to the ethyl pleocidin and the Acarus tritici urea 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.
Ethyl pleocidin 3g, Acarus tritici urea 7g, calcium dodecyl benzene sulfonate 5g, aliphatic acid polyethenoxy ether 5g, toluene, xylol are supplied 100g.Be dissolved in the solvent according to the ethyl pleocidin and the Acarus tritici urea 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.
Ethyl pleocidin 20g, Acarus tritici urea 3g, calcium dodecyl benzene sulfonate 7g, aliphatic acid polyethenoxy ether 8g, toluene, xylol are supplied 100g.Be dissolved in the solvent according to the ethyl pleocidin and the Acarus tritici urea 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 6: the processing and the embodiment of ethyl pleocidin and lice fluorine uride missible oil
Ethyl pleocidin 3g, fluorine uride 32g, calcium dodecyl benzene sulfonate 9g, aliphatic acid polyethenoxy ether 6g, toluene, xylol are supplied 100g.Be dissolved in the solvent according to the ethyl pleocidin and the fluorine uride 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.
Ethyl pleocidin 3g, fluorine uride 7g, calcium dodecyl benzene sulfonate 4g, aliphatic acid polyethenoxy ether 5g, toluene, xylol are supplied 100g.Be dissolved in the solvent according to the ethyl pleocidin and the fluorine uride 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.
Ethyl pleocidin 25g, fluorine uride 4g, calcium dodecyl benzene sulfonate 9g, aliphatic acid polyethenoxy ether 5g, toluene, xylol are supplied 100g.Be dissolved in the solvent according to the ethyl pleocidin and the fluorine uride 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 7: the processing and the embodiment of ethyl pleocidin and Buprofezin wetting powder
Ethyl pleocidin 3g, Buprofezin 47g, sodium lignin sulfonate 13g; Lauryl sodium sulfate 7g; White carbon 24g, evenly stirs in stirred tank ethyl pleocidin and Buprofezin 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.
Ethyl pleocidin 3g, Buprofezin 17g, sodium lignin sulfonate 7g; Lauryl sodium sulfate 6g; White carbon 67g, evenly stirs in stirred tank ethyl pleocidin and Buprofezin 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.
Ethyl pleocidin 17g, Buprofezin 8g, sodium lignin sulfonate 6g; Lauryl sodium sulfate 5g; White carbon 64g, evenly stirs in stirred tank ethyl pleocidin and Buprofezin 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 8: the processing and the embodiment of ethyl pleocidin and Acarus tritici urea microemulsion
Ethyl pleocidin 4g, Acarus tritici urea 11g, aliphatic acid polyethenoxy ether 6g, ethylene glycol 3g, sodium citrate 2g, conventional solvent cosolvent 18g.Former medicine ethyl pleocidin, Acarus tritici urea 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.
Above formulation embodiment is illustrating of preparation just; These can not simply be interpreted as; For example ethyl pleocidin all can be prepared into suspending agent with six kinds of chitin synthesis inhibitor compounds mentioning, and active constituent content is looked crop and the pest control of concrete location mostly and decided.The real protection scope of patent of the present invention should be as the criterion with protection of the formulation in the appended claims and scope.
Indoor biometrics screening and field experiment:
The method that the present invention adopts indoor bioassay and field trial to combine.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% fluorine bell urea, Shandong Tian Feng bio tech ltd.
(2) test target
The indoor cotton bollworm of for many generations raising, indoor conditions: temperature (26 ± 2) ℃.Relative moisture 70% ± 5%, periodicity of illumination 16/8h (L/D).
(3) test method
The polypide immersion method is adopted in this test.At first the mother liquor with ethyl pleocidin, fluorine bell urea is diluted to 5 concentration, places beaker subsequent use respectively.Sweep lightly with the cotton bollworm larvae at writing brush 3 initial stages in age that physiological status is consistent and to soak in the worm device, will soak the worm device and immerse in the soup, take out after shaking 5s gently, wash dried polypide and unnecessary peripherally soup with blotting paper rapidly.It is 26 ℃ that larva after the processing places temperature, and relative moisture is in 70% the intelligent insectary.Every concentration repeats 3 times, and 20 larvas of every repetition are established blank simultaneously, and is doomed dead respectively at 48h inspection behind the medicine, calculates lethality, corrected mortality, obtains virulence regression equation and calculate LC 50The control group lethality is being efficiency test below 10%.
(4) data statistics and analysis
According to preliminary experiment both total active ingredient 12% is set, set ratio is that m (ethyl pleocidin): m (fluorine bell urea) was respectively 3: 9,4: 8, and 5: 7,7: 5,9: 3.
Adopt said method 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 ethyl pleocidin is the standard medicament, and its toxicity index is 100):
The LC of toxicity index (the TI)=ethyl pleocidin of fluorine bell urea 50The LC of/fluorine bell urea 50* 100
The LC of actual toxicity index (ATI)=ethyl pleocidin of M 50The LC of/M 50* 100
The TI of the TI of theoretical toxicity index (TTI)=ethyl pleocidin of M * P ethyl pleocidin+fluorine bell urea * P fluorine bell urea
TTI * 100 of the ATI/M of the co-toxicity coefficient of M (CTC)=M
In the formula:
M is a fluorine bell urea and the mixture of the different proportionings of ethyl pleocidin
P fluorine bell urea is fluorine bell urea shared ratio in mixture
The P ethyl pleocidin is ethyl pleocidin shared ratio in mixture
(5) toxicity test result and analysis
Table 1 ethyl pleocidin, fluorine bell urea are to the indoor measurement result of cotton bollworm
Figure BDA0000113105040000091
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: fluorine bell urea is that synergistic effect in 4: 8 o'clock is the most obvious, and co-toxicity coefficient is 179.38.Result of the test shows that fluorine bell urea, two kinds of medicaments of ethyl pleocidin all have higher activity to cotton bollworm under indoor conditions, and the result of the test of different proportion proportioning shows; In active ingredient ratio ethyl pleocidin: fluorine bell urea is 3: 9,4: 8, and 5: 7; 7: 5,, all show stronger synergistic effect at 9: 3 o'clock; Wherein with ethyl pleocidin: fluorine bell urea 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.
Determination of activity instance 2:
(1) experiment supplies the reagent agent
The former medicine of 81.2% ethyl pleocidin, The Dow Agrosciences, LLC., the former medicine of 97% Buprofezin, Jiangsu Anpon Electrochemical Co., Ltd..
According to preliminary experiment both total active ingredient 18% is set, set ratio is that m (ethyl pleocidin): m (Buprofezin) was respectively 3: 15; 5: 13; 7: 11; 9: 9; 11: 7.
(2) test target
The field population that Qingdao Agricultural University's experimental field of wheat picks up from wheat aphid system, the individual aptery one-tenth aphid of the same size of picking supplies examination during experiment.
Experimental technique is with determination of activity instance 1
(3) toxicity test result and analysis:
Table 2 ethyl pleocidin, Buprofezin are to the indoor measurement result of wheat aphid
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: Buprofezin is that synergistic effect in 5: 13 o'clock is the most obvious, and co-toxicity coefficient is 183.31.Result of the test shows that Buprofezin, two kinds of medicaments of ethyl pleocidin all have higher activity to wheat aphid under indoor conditions, and the result of the test of different proportion proportioning shows, in active ingredient ratio ethyl pleocidin: Buprofezin is 5: 15; 7: 13; 9: 11; 11: 9; When respectively diluting all show stronger synergistic effect at 13: 7, wherein with ethyl pleocidin: Buprofezin is 7: 13 o'clock, and synergistic effect is best.Suggestion is carried out further field control effectiveness test to the mixture preparation of 7: 13 left and right sides scopes of suitable proportion, to estimate its field practical application effect.
Determination of activity instance 3:
(1) experiment supplies the reagent agent
The former medicine of 81.2% ethyl pleocidin, The Dow Agrosciences, LLC., the former medicine of 95% Acarus tritici urea, Jiangsu Zhongqi Chemical Industry Co., Ltd.
According to preliminary experiment both total active ingredient 18% is set, set ratio is that m (ethyl pleocidin): m (Acarus tritici urea) was respectively 3: 15,5: 13, and 7: 11,9: 9,11: 7.
(2) test target
The indoor cotton bollworm of for many generations raising, indoor conditions: temperature (28 ± 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, Acarus tritici urea are to the indoor measurement result of cotton bollworm
Figure BDA0000113105040000111
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 Acarus tritici urea is that 3: 15 synergistic effect is the most obvious, and co-toxicity coefficient is 172.79.Result of the test shows that Acarus tritici urea, two kinds of medicaments of ethyl pleocidin all have higher activity to the cotton cotton bollworm under indoor conditions, and the result of the test of different proportion proportioning shows; In active ingredient ratio ethyl pleocidin: the Acarus tritici urea is 3: 15,5: 13, and 7: 11; 9: 9, when respectively diluting all show stronger synergistic effect at 11: 7; Wherein with ethyl pleocidin: the Acarus tritici urea is 3: 15 o'clock, and synergistic effect is best.Suggestion is carried out further field control effectiveness test to the mixture preparation of 3: 15 left and right sides scopes of suitable proportion, to estimate its field practical application effect.
Determination of activity instance 4:
(1) experiment supplies the reagent agent
The former medicine of 81.2% ethyl pleocidin, The Dow Agrosciences, LLC., the former medicine of 98.5% fluorine uride, Jiangsu Jiannong Agrochemical Co., Ltd..
According to preliminary experiment both total active ingredient 15% is set, set ratio is that m (ethyl pleocidin): m (fluorine uride) was respectively 3: 12,5: 10, and 7: 8,9: 6,11: 4.
(2) test target
Beet armyworm, the indoor beet armyworm 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 4 ethyl pleocidin, fluorine uride are to the indoor measurement result of beet armyworm
Figure BDA0000113105040000112
Figure BDA0000113105040000121
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 fluorine uride is that 5: 10 synergistic effect is the most obvious, and co-toxicity coefficient is 175.63.Result of the test shows that fluorine uride, two kinds of medicaments of ethyl pleocidin all have higher activity to beet armyworm under indoor conditions, and the result of the test of different proportion proportioning shows; In active ingredient ratio ethyl pleocidin: the fluorine uride is 3: 12,5: 10, and 7: 8; 9: 6, when respectively diluting all show stronger synergistic effect at 11: 4; Wherein with ethyl pleocidin: the fluorine uride is 5: 10 o'clock, and synergistic effect is best.Suggestion is carried out further field control effectiveness test to the mixture preparation of 5: 10 left and right sides scopes of suitable proportion, to estimate its field practical application effect.
Determination of activity instance 5:
(1) experiment supplies the reagent agent
The former medicine of 81.2% ethyl pleocidin, The Dow Agrosciences, LLC., 99% pyrrole worm is swelled former medicine, the auspicious and rich scientific & trading Co., Ltd. in Taiyuan City.
According to preliminary experiment both total active ingredient 17% is set, set ratio is that m (ethyl pleocidin): m (fluorine uride) was respectively 3: 14,5: 12, and 7: 10,9: 8,11: 6.
(2) test target
Diamond-back moth, the indoor diamond-back moth of for many generations raising, indoor conditions: temperature (25 ± 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, the grand indoor measurement result of pyrrole worm to diamond-back moth
Figure BDA0000113105040000122
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 pyrrole worm is grand to be that 5: 12 synergistic effect is the most obvious, and co-toxicity coefficient is 171.50.Result of the test shows, grand, the two kinds of medicaments of ethyl pleocidin of pyrrole worm all have higher activity to diamond-back moth under indoor conditions, and the result of the test of different proportion proportioning shows; In active ingredient ratio ethyl pleocidin: the pyrrole worm is grand to be 3: 14,5: 12, and 7: 10; 9: 8, when respectively diluting all show stronger synergistic effect at 11: 6; Wherein with ethyl pleocidin: the pyrrole worm is grand to be 5: 12 o'clock, and synergistic effect is best.Suggestion is carried out further field control effectiveness test to the mixture preparation of 5: 12 left and right sides scopes of suitable proportion, to estimate its field practical application effect.
Field experiment example 1: field experiment control cotton cotton bollworm
(1) test method
Test and carry out reagent spray on July 19th, 2010 and handle, the cotton bollworm generation investigation of beating period, Shuan Yao village cotton field makes an experiment in Yang Chengzhuan township, Jinghai County, Tianjin, and the cotton growing way is better, and the soil texture is a loam, middle fertility, pH value 6.9.Spraying equipment bodyguard WS one 16 type manual sprayers, cone nozzle spraying, operating pressure 0.2~0.4MPa, flow 0.65~0.88L/min.
(2) control time and method
(July 23) investigation insect population quantity before the medicine, dispenser on July 23,3,7,14 days remaining borer populations alive of investigation behind the medicine, each handles the investigation (looking into the remaining insect population number of 100 strains) and calculate control efficiency of taking to beat.
(3) drug effect computational methods
Insect population borer population * 100% of living before rate (%)=(borer population of living behind the borer population-medicine of living before the medicine)/medicine that goes down
Control efficiency (%)=(the CK insect population rate of going down-chemicals treatment insect population go down rate)/CK insect population rate * 100% that goes down
(4) poisoning investigation method
Behind medicine 3,7,14d observes the cotton plants growing state, the range estimation medicament does not all have poisoning to cotton.
(5) field control effectiveness test result of the test
Table 6 is handled chemical control cotton cotton bollworm field control effectiveness test result
Figure BDA0000113105040000131
Figure BDA0000113105040000141
Can find out from table 6; The Mixed Pharmacy of different proportion; Carry out field experiment by different consumptions, its control efficiency to the cotton cotton bollworm all is superior to contrasting medicament behind the medicine, and 4% Acarus tritici urea+14% ethyl pleocidin, insecticidal effect of 7 days behind medicine is respectively 92.85%, 94.14% and 95.21%; 10 days insecticidal effect is respectively 92.41%, 93.13% and 93.18% behind the medicine, and insecticidal effect increases progressively along with the increase of consumption.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 cotton all do not occur, explains that it is safe to cotton.In process of the test, testing crew finds that it also has favorable effect to insects such as cotton plant bugs, and suggestion mixes with mechanism of action different insecticide to be used to delay the generation of pest resistance to insecticide.
Field experiment example 2: field experiment control beet armyworm test
(1) test method
Test that the suburb truck garden carries out in Kaiping City, Guangdong Province on October 8th, 2010 to October 18.Tested on October 8th, 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 ℃, and dispenser was fine the same day.
(2) investigation method
Before dispenser, press 5 samplings of diagonal, every wild cabbage 2~3 strain of choosing beet armyworm ovum and larva (look insect density and decide) in every sub-district.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 BDA0000113105040000142
(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 7 is handled chemical control wild cabbage beet armyworm field control effectiveness test result
Figure BDA0000113105040000151
Can find out that from table 7 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; 10% fluorine uride+5% ethyl pleocidin control beet armyworm quick-acting is fast, and efficiency time is long, and control efficiency is good.7 days insecticidal effect reaches 93.84%, 95.07%, 96.16% respectively behind medicine, and 10 days insecticidal effect reaches 92.07%, 93.59%, 93.99% respectively behind medicine, and insecticidal effect increases progressively along with the increase of consumption.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, blade face, blade back even medicine, advise that the medicament different with other mechanisms of action is used alternatingly, to delay the generation of pest resistance to insecticide.

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 that Buprofezin, Acarus tritici urea, butyl ether urea, fluorine bell urea, fluorine uride, pyrrole worm are one of any in grand, 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 3%-70%.
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, water dispersible granules.
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