CN101642107B - Insect-killing composition containing pymetrozine and etofenprox - Google Patents

Insect-killing composition containing pymetrozine and etofenprox Download PDF

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Publication number
CN101642107B
CN101642107B CN2009100233532A CN200910023353A CN101642107B CN 101642107 B CN101642107 B CN 101642107B CN 2009100233532 A CN2009100233532 A CN 2009100233532A CN 200910023353 A CN200910023353 A CN 200910023353A CN 101642107 B CN101642107 B CN 101642107B
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chrysanthemum ester
ether
pyrrole aphid
ketone
agent
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CN101642107A (en
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郑敬敏
何爱华
冯建雄
时晓磊
张武
张崇斌
孙瑞
赵海军
梅红玉
乌小瑜
段莹
苏蓓
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Shaanxi Sunger Road Bio Science Co Ltd
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Shaanxi Sunger Road Bio Science Co Ltd
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Abstract

The invention discloses an insect-killing composition containing pymetrozine and etofenprox, comprising the effective active components of the pymetrozine and the etofenprox, wherein the weight ratio of the pymetrozine to the etofenprox is 1:2-3:1. The invention has reasonable components, good insect-destroying effect, low application cost, high quick-acting property, long lasting period and good safety without pollution on crops, little residual quantity of a preparation and obvious synergistic action, delays the generation of resistibility, and conforms to the safety requirement of a pesticide preparation; and the activity and the insect-killing effect of the invention are not the simple superposition of the activity of the components. The invention has the preventing effect of 84.24-96.22% to paddy rice planthopper after being applied 14 days.

Description

A kind of Pesticidal combination that contains pyrrole aphid ketone and ether chrysanthemum ester
Technical field
The present invention relates to a kind of Pesticidal combination, particularly Pesticidal combination and the application thereof be made up of pyrrole aphid ketone and ether chrysanthemum ester of effective active composition belongs to technical field of compounded pesticide.
Background technology
Pyrrole aphid ketone (english common name pymetrozine, chemical molecular formula C 10H 11N 5O) mechanism of action is adult with after nymph contacts, and produces the lancet blocking effect, stops to get food and causes harm, hungry causing death.The characteristics of control are that speed of action is slower; Lasting period is long, does not have cross resistance with its existing numerous insecticides, can prevent and treat most of homoptera pest; Especially aphid section, Aleyrodidae, Cicadellidae and Delphacidae insect insect are applicable to vegetables, paddy rice, cotton, fruit tree and multiple field crop.But in actual application, use pyrrole aphid ketone list agent quick-acting relatively poor separately, insect is prone to produce resistance.
Ether chrysanthemum ester (english common name etofenprox, chemical molecular formula C 25H 28O 3) be a kind of insecticide of similar pyrethroid, have that insecticidal spectrum is wide, insecticidal activity is high, the speed of knocking down is fast, the lasting period is long, less to natural enemy lethality such as paddy field spiders, to advantages such as crop safeties.Have and tag and stomach poison function, do not inhale conduction in insect is not had.Be widely used on paddy rice, vegetables, the cotton, various pests such as Lepidoptera, Semiptera, orthoptera, coleoptera, diptera and Isoptera are had efficiently.But in actual application, use the agent of ether chrysanthemum ester list separately, insect is prone to produce resistance, and use cost rises day by day.
At present, be that the pesticidal preparations of effective ingredient is main with 25% pyrrole aphid ketone wetting powder with pyrrole aphid ketone, in actual use, the lasting period is long; But quick-acting is relatively poor, and ether chrysanthemum ester quick-acting is better, to crop safety; The unexpected discovery of inventor is mixed two active components to use and can improves its quick-acting, is arranged, significantly synergistic effect the lasting period preferably again; Can reduce the pharmacy application amount, save cost, the generation that slows down pest resistance.
Summary of the invention
One of the object of the invention is to provide a kind of good disinsection effect, and drug cost is low, the Pesticidal combination that contains pyrrole aphid ketone and ether chrysanthemum ester that is difficult for developing immunity to drugs.
Another object of the present invention is to provide the purposes of above-mentioned composition.
In order to overcome the defective of existing single component formulations, technical scheme of the present invention is to solve like this:
A kind of Pesticidal combination that contains pyrrole aphid ketone and ether chrysanthemum ester comprises:
A) the first active component pyrrole aphid ketone;
B) the second active component ether chrysanthemum ester;
The weight ratio of first active component and second active component was at 1: 2~3: 1.The cumulant of pyrrole aphid ketone and ether chrysanthemum ester is 5%~90% of a said composition total weight, is preferably 10%~50%.
According to method known in those skilled in the art, the present composition can be mixed with water dispersible granules, wetting powder, suspending agent, oil-suspending agent, suspended emulsion, missible oil, microemulsion, aqueous emulsion, soluble concentrate.
For water dispersible granules, those skilled in the art are familiar with the use corresponding adjuvants and accomplish the present invention very much.In dispersant such as polycarboxylate, lignosulfonates, the alkylnaphthalene sulfonate one or more; In wetting agent such as alkyl sulfate, alkylsulfonate, the naphthalene sulfonate one or more; In disintegrant such as ammonium sulfate, urea, sucrose, the glucose one or more; In binding agent such as diatomite, corn starch, PEG6000, carboxymethyl (ethyl) cellulose family one or more; Filler such as kaolin, white carbon, fine particle calcium carbonate, talcum powder, attapulgite, potter's clay, diatomite one or more.
To wetting powder, spendable auxiliary agent has: in dispersant such as polycarboxylate, lignosulfonates, the alkylnaphthalene sulfonate one or more; In wetting agent such as alkyl sulfate, alkylsulfonate, the naphthalene sulfonate one or more; Filler such as ammonium sulfate, urea, sucrose, glucose, diatomite, kaolin, white carbon, fine particle calcium carbonate, talcum powder, attapulgite, potter's clay one or more.
To suspending agent, spendable auxiliary agent has: among dispersant such as polycarboxylate, lignosulfonates, alkylnaphthalene sulfonate (dispersing agent NNO), the TERSPERSE 2425 (U.S. Huntsman Corporation produces, the alkyl naphthalene sulfonic acid salt) one or more; Alkyl phenol formaldehyde resin polyoxyethylene ether), farming breast 2201, this dish-60# (common name: Span60), Tween-60 # (common name: the polyoxyethylene sorbitan stearate), agricultural newborn 1601# (common name: triphen ethyl-phenol polyoxyethylene polyoxypropylene block polymer), among the TERSPERSE 4894 (U.S. Huntsman Corporation product) one or more emulsifier such as Nongru-700 # (common name:; Among wetting agent such as alkylphenol-polyethenoxy base ether formaldehyde condensation products sulphate, alkylphenol-polyethenoxy base ether phosphate, phenethyl phenol polyethenoxy base ether phosphate, alkyl sulfate, alkylsulfonate, naphthalene sulfonate, the TERSPERSE 2500 (U.S. Huntsman Corporation product) one or more; In thickener such as xanthans, polyvinyl alcohol, bentonite, the aluminium-magnesium silicate one or more; In preservative such as formaldehyde, benzoic acid, the Sodium Benzoate one or more; In stabilizing agent such as epoxidized soybean oil, epoxychloropropane, the triphenyl phosphate one or more; Antifoaming agent such as organic silicon defoamer; In antifreezing agent such as ethylene glycol, propane diols, glycerine, urea, inorganic salts such as the sodium chloride one or more.
To oil-suspending agent, spendable auxiliary agent has: among dispersant such as polycarboxylate, lignosulfonates, alkylnaphthalene sulfonate (dispersing agent NNO), the TERSPERSE 2425 (U.S. Huntsman Corporation produces, the alkyl naphthalene sulfonic acid salt) one or more; Alkyl phenol formaldehyde resin polyoxyethylene ether), farming breast 2201, this dish-60# (common name: Span60), Tween-60 # (common name: the polyoxyethylene sorbitan stearate), agricultural newborn 1601# (common name: triphen ethyl-phenol polyoxyethylene polyoxypropylene block polymer), among the TERSPERSE 4894 (U.S. Huntsman Corporation product) one or more emulsifier such as Nongru-700 # (common name:; Among wetting agent such as alkylphenol-polyethenoxy base ether formaldehyde condensation products sulphate, APES phosphate, phenethyl phenol polyethenoxy base ether phosphate, alkyl sulfate, alkylsulfonate, naphthalene sulfonate, the TERSPERSE 2500 (U.S. Huntsman Corporation product) one or more; In thickener such as white carbon, polyvinyl alcohol, bentonite, the aluminium-magnesium silicate one or more; In antifreezing agent such as ethylene glycol, propane diols, glycerine, urea, inorganic salts such as the sodium chloride one or more; In preservative such as formaldehyde, benzoic acid, the Sodium Benzoate one or more; In stabilizing agent such as epoxidized soybean oil, epoxychloropropane, the triphenyl phosphate one or more; Antifoaming agent such as organic silicon defoamer; In dispersion medium such as soybean oil, rapeseed oil, corn oil, methyl oleate, diesel oil, machine oil, the mineral oil one or more.
To suspended emulsion, spendable auxiliary agent has: among dispersant such as polycarboxylate, lignosulfonates, alkylnaphthalene sulfonate (dispersing agent NNO), the TERSPERSE 2425 (U.S. Huntsman Corporation produces, the alkyl naphthalene sulfonic acid salt) one or more; Alkyl phenol formaldehyde resin polyoxyethylene ether), farming breast 2201, this dish-60# (common name: Span60), Tween-60 # (common name: the polyoxyethylene sorbitan stearate), agricultural newborn 1601# (common name: triphen ethyl-phenol polyoxyethylene polyoxypropylene block polymer), in the triphen ethyl phenol polyoxyethylene groups ether phosphate, TERSPERSE 4894 (U.S. Huntsman Corporation product) one or more emulsifier such as Nongru-700 # (common name:; Among wetting agent such as alkylphenol-polyethenoxy base ether formaldehyde condensation products sulphate, alkylphenol-polyethenoxy base ether phosphate, phenethyl phenol polyethenoxy base ether phosphate, alkyl sulfate, alkylsulfonate, naphthalene sulfonate, the TERSPERSE 2500 (U.S. Huntsman Corporation product) one or more; Solvent: one or more in xylol, toluene, cyclohexanone, the solvent naphtha (S-150, S-180, S-200); In thickener such as xanthans, polyvinyl alcohol, bentonite, the aluminium-magnesium silicate one or more; In preservative such as formaldehyde, benzoic acid, the Sodium Benzoate one or more; Antifoaming agent such as organic silicon defoamer; In antifreezing agent such as ethylene glycol, propane diols, glycerine, urea, inorganic salts such as the sodium chloride one or more; In stabilizing agent such as triphenyl phosphite, epoxychloropropane, the aceticanhydride one or more; Water is deionized water.
For missible oil, those skilled in the art are familiar with the use corresponding adjuvants and accomplish the present invention very much.Emulsifier such as calcium dodecyl benzene sulfonate (agricultural newborn 500#); Nongru-700 # (common name: alkyl phenol formaldehyde resin polyoxyethylene ether); The newborn 2201# of farming; This dish-60# (common name: Span60); Tween-60 # (common name: the polyoxyethylene sorbitan stearate); TX-10 (common name: octyl phenol polyoxy ethene (10) ether); The newborn 1601# of farming (common name: triphen ethyl-phenol polyoxyethylene polyoxypropylene block polymer); The newborn 600# of farming; The farming newborn 400# in one or more; In solvent such as xylol, toluene, solvent naphtha (S-150, S-180, S-200), toluene, methyl alcohol, dimethyl formamide, N-Methyl pyrrolidone, cyclohexanone, acetone, the dimethyl sulfoxide (DMSO) one or more; In stabilizing agent such as triphenyl phosphite, the epoxychloropropane one or more.
To microemulsion, spendable auxiliary agent has: emulsifier such as calcium dodecyl benzene sulfonate (agricultural newborn 500#), Nongru-700 # (common name: alkyl phenol formaldehyde resin polyoxyethylene ether), agricultural newborn 2201#, this dish-60# (common name: Span60), Tween-60 # (common name: the polyoxyethylene sorbitan stearate), TX-10 (common name: octyl phenol polyoxy ethene (10) ether), farming breast 1601 (common name: triphen ethyl-phenol polyoxyethylene polyoxypropylene block polymer), among the agricultural newborn 600#, agricultural newborn 400# one or more; In assistant for emulsifying agent such as methyl alcohol, isopropyl alcohol, n-butanol, the ethanol one or more; Solvent such as cyclohexanone, N-Methyl pyrrolidone, xylol, toluene, solvent naphtha (trade mark: S-150, S-180, S-200) one or more; In stabilizing agent such as triphenyl phosphite, the epoxychloropropane one or more; Water is deionized water.
To aqueous emulsion, spendable auxiliary agent has: emulsifier such as Nonyl pheno (EO=10) ether phosphate, triphen ethyl-phenol polyoxyethylene ether phosphate, Nongru-700 # (common name: alkyl phenol formaldehyde resin polyoxyethylene ether), agricultural newborn 2201#, this dish-60# (common name: Span60), Tween-60 # (common name: the polyoxyethylene sorbitan stearate), TX-10 (common name: octyl phenol polyoxy ethene (10) ether), farming breast 1601 (common name: triphen ethyl-phenol polyoxyethylene polyoxypropylene block polymer), among the agricultural newborn 600#, agricultural newborn 400# one or more; Solvent such as xylol, toluene, cyclohexanone, solvent naphtha (trade mark: S-150, S-180, S-200) one or more; In stabilizing agent such as triphenyl phosphite, epoxychloropropane, the epoxidized soybean oil one or more; Antifreezing agent: in ethylene glycol, propane diols, glycerine, urea, inorganic salts such as the sodium chloride one or more; In thickener such as xanthans, polyvinyl alcohol, bentonite, the aluminium-magnesium silicate one or more; In preservative such as formaldehyde, benzoic acid, the Sodium Benzoate one or more, water is deionized water.
To soluble concentrate, spendable auxiliary agent has: emulsifier such as Nongru-700 # (common name: alkyl phenol formaldehyde resin polyoxyethylene ether), agricultural newborn 2201#, this dish-60# (common name: Span60), Tween-60 # (common name: the polyoxyethylene sorbitan stearate), TX-10 (common name: octyl phenol polyoxy ethene (10) ether), agricultural newborn 1601# (common name: triphen ethyl-phenol polyoxyethylene polyoxypropylene block polymer), among the agricultural newborn 600#, agricultural newborn 400# one or more; In solvent such as methyl alcohol, ethanol, acetone, cyclohexanone, dimethyl formamide, dimethyl sulfoxide (DMSO), N-Methyl pyrrolidone, cyclohexanone, the isophorone one or more; In stabilizing agent such as triphenyl phosphite, triphenyl phosphate, the epoxychloropropane one or more.
Component of the present invention is reasonable, good disinsection effect, and drug cost is low; And its activity and insecticidal effect are not the simple superposition of each composition activity, but significant synergistic effect is arranged, and quick-acting is high, lasting effect is long; Slow down the generation of resistance, the preparation less residue, pollution-free to crop; Safety is good, meets the security requirement of pesticidal preparations.The present invention to the rice hoppers medicine after 14d have 84.24%~96.22% control efficiency.
Embodiment
Below in conjunction with embodiment content of the present invention is described further.
FORMULATION EXAMPLE 1
Take by weighing 15% pyrrole aphid ketone, 10% ether chrysanthemum ester, 3%TERSPERSE 4894 (U.S. Huntsman Corporation product), 1%TERSPERSE 2500 (U.S. Huntsman Corporation product), 2% dispersing agent NNO, 0.3% xanthans, 5% propane diols, 0.5% benzoic acid, 0.5% silicone defoaming agent (trade name: s-29 Nanjing "four news" (new ideas applied chemistry article company produces), 1% epoxychloropropane, deionized water adds to 100% weight portion.Above-mentioned raw materials is through mixing, and high speed shear is disperseed 30min, with the pyrrole aphid ether ketone chrysanthemum ester suspending agent that makes 25% behind the sand mill sand milling.
The part by weight of pyrrole aphid ketone and ether chrysanthemum ester can be 1 in the present embodiment: 2-3: change between 1, both total weight items still are 25%, form new embodiment.
FORMULATION EXAMPLE 2
Take by weighing 10% pyrrole aphid ketone, 10% ether chrysanthemum ester, 4%TERSPERSE 4894 (U.S. Huntsman Corporation product), 1.5%TERSPERSE 2500 (U.S. Huntsman Corporation product), 2%TERSPERSE2425 (U.S. Huntsman Corporation product), 0.2% aluminium-magnesium silicate, 5% ethylene glycol, 0.5% formaldehyde, 0.5% silicone defoaming agent (trade name: s-29 Nanjing "four news" (new ideas applied chemistry article company produces), 2% triphenyl phosphate, deionized water adds to 100% weight portion.Above-mentioned raw materials is through mixing, and high speed shear is disperseed 30min, with the pyrrole aphid ether ketone chrysanthemum ester suspending agent that makes 20% behind the sand mill sand milling.
The part by weight of pyrrole aphid ketone and ether chrysanthemum ester can be 1 in the present embodiment: 2-3: change between 1, both total weight items still are 20%, form new embodiment.
FORMULATION EXAMPLE 3
Take by weighing 30% pyrrole aphid ketone, 10% ether chrysanthemum ester, 5%TERSPERSE 4894 (U.S. Huntsman Corporation product), 2%TERSPERSE 2500 (U.S. Huntsman Corporation product), 3%TERSPERSE2425 (U.S. Huntsman Corporation product), 0.2% xanthans, 5% propane diols, 0.5% benzoic acid, 0.5% silicone defoaming agent (trade name: s-29 Nanjing "four news" (new ideas applied chemistry article company produces), 1% epoxychloropropane, deionized water adds to 100% weight portion.Above-mentioned raw materials is through mixing, and high speed shear is disperseed 30min, with the pyrrole aphid ether ketone chrysanthemum ester suspending agent that makes 40% behind the sand mill sand milling.
The part by weight of pyrrole aphid ketone and ether chrysanthemum ester can be 1 in the present embodiment: 2-3: change between 1, both total weight items still are 24%, form new embodiment.
FORMULATION EXAMPLE 4
Take by weighing 15% pyrrole aphid ketone, 30% ether chrysanthemum ester, 3% dispersing agent NNO, 3% Nongru-700 #, 2%TERSPERSE 2500 (U.S. Huntsman Corporation product), 0.3% xanthans, 5% propane diols, 0.5% benzoic acid, 0.5% silicone defoaming agent (trade name: s-29 Nanjing "four news" (new ideas applied chemistry article company produces), 1% epoxychloropropane, deionized water adds to 100% weight portion.Above-mentioned raw materials is through mixing, and high speed shear is disperseed 30min, with the pyrrole aphid ether ketone chrysanthemum ester suspending agent that makes 36% behind the sand mill sand milling.
The part by weight of pyrrole aphid ketone and ether chrysanthemum ester can be 1 in the present embodiment: 2-3: change between 1, both total weight items still are 45%, form new embodiment.
FORMULATION EXAMPLE 5
Take by weighing 24% pyrrole aphid ketone, 8% ether chrysanthemum ester, 3%TERSPERSE 2425 (U.S. Huntsman Corporation product), 2% this dish-60#, 2% Tween-60 #, 1%TERSPERSE 2500 (U.S. Huntsman Corporation product), 0.5% white carbon, 5% propane diols, 0.5% benzoic acid, 0.5% silicone defoaming agent (trade name: s-29 Nanjing "four news" (new ideas applied chemistry article company produces), 1% epoxychloropropane, methyl oleate adds to 100% weight portion.Above-mentioned raw materials is through mixing, and high speed shear is disperseed 30min, with the pyrrole aphid ether ketone chrysanthemum ester oil suspending agent that makes 32% behind the sand mill sand milling.
The part by weight of pyrrole aphid ketone and ether chrysanthemum ester can be 1 in the present embodiment: 2-3: change between 1, both total weight items still are 32%, form new embodiment.
FORMULATION EXAMPLE 6
Take by weighing 11% pyrrole aphid ketone; 22% ether chrysanthemum ester; 3%TERSPERSE 2425 (U.S. Huntsman Corporation product); 3% triphen ethyl-phenol polyoxyethylene ether phosphate; 2% agricultural newborn 2201#; 1%TERSPERSE2500 (U.S. Huntsman Corporation product); 10% xylol; 0.3% xanthans; 5% propane diols; 0.5% benzoic acid; 0.5% silicone defoaming agent (trade name: s-29 Nanjing "four news" (new ideas applied chemistry article company produces); 1% epoxychloropropane; Deionized water adds to 100% weight portion.Ether chrysanthemum ester in the above-mentioned raw materials, triphen ethyl-phenol polyoxyethylene ether phosphate, agricultural newborn 2201#, xylol, epoxychloropropane mixed dissolution evenly after; In the mixing mutually of input by pyrrole aphid ketone, TERSPERSE 2425, TERSPERSE 2500, xanthans, propane diols, benzoic acid, silicone defoaming agent, deionized water; High speed shear is disperseed 30min, with the pyrrole aphid ether ketone chrysanthemum ester suspended emulsion that makes 33% behind the sand mill sand milling.
The part by weight of pyrrole aphid ketone and ether chrysanthemum ester can be 1 in the present embodiment: 2-3: change between 1, both total weight items still are 33%, form new embodiment.
FORMULATION EXAMPLE 7
Take by weighing 60% pyrrole aphid ketone, 20% ether chrysanthemum ester, 6% calcium lignosulfonate, 3% alkylnaphthalene sulfonate formaldehyde condensation products (dispersing agent NNO), 1% lauryl sodium sulfate, 3% white carbon, kaolin and fill up weight portion to 100%.Above-mentioned raw materials is prepared into 80% pyrrole aphid ether ketone chrysanthemum ester wetting powder through mixing, ultra micro comminution by gas stream, hybrid technique step.
The part by weight of pyrrole aphid ketone and ether chrysanthemum ester can be 1 in the present embodiment: 2-3: change between 1, both total weight items still are 80%, form new embodiment.
FORMULATION EXAMPLE 8
Take by weighing 20% pyrrole aphid ketone, 40% ether chrysanthemum ester, 6% calcium lignosulfonate, 4% alkylnaphthalene sulfonate formaldehyde condensation products (dispersing agent NNO), 1.5% lauryl sodium sulfate, 10% white carbon, fine particle calcium carbonate and fill up weight portion to 100%.Above-mentioned raw materials is prepared into 60% pyrrole aphid ether ketone chrysanthemum ester wetting powder through mixing, ultra micro comminution by gas stream, hybrid technique step.
The part by weight of pyrrole aphid ketone and ether chrysanthemum ester can be 1 in the present embodiment: 2-3: change between 1, both total weight items still are 60%, form new embodiment.
FORMULATION EXAMPLE 9
Take by weighing 15% pyrrole aphid ketone, 10% ether chrysanthemum ester, 4% calcium lignosulfonate, 4%TERSPERSE 2425 (U.S. Huntsman Corporation produces, the alkyl naphthalene sulfonic acid salt), 2% lauryl sodium sulfate, 5% white carbon, kaolin fills up the weight portion to 100%.Above-mentioned raw materials is prepared into 25% pyrrole aphid ether ketone chrysanthemum ester wetting powder through mixing, ultra micro comminution by gas stream, hybrid technique step.
The part by weight of pyrrole aphid ketone and ether chrysanthemum ester can be 1 in the present embodiment: 2-3: change between 1, both total weight items still are 25%, form new embodiment.
FORMULATION EXAMPLE 10
Take by weighing 30% pyrrole aphid ketone, 30% ether chrysanthemum ester, 3%TERSPERSE 2700 (polycarboxylate, U.S. Huntsman Corporation produces), 2% dispersing agent NNO (alkylnaphthalene sulfonate formaldehyde condensation products), 3% Nekal BX (nekal), 2%K-12 (lauryl sodium sulfate), 2%PEG6000,8% sulphur ammonium, kaolin adds to 100% weight portion.The method of the frequent regulation of above-mentioned raw materials water intaking dispersible granule is promptly mixed, ultra micro comminution by gas stream, mixing, granulation step are produced 60% pyrrole aphid ether ketone chrysanthemum ester water dispersible granules.
The part by weight of pyrrole aphid ketone and ether chrysanthemum ester can be 1 in the present embodiment: 2-3: change between 1, both total weight items still are 60%, form new embodiment.
FORMULATION EXAMPLE 11
Take by weighing 30% pyrrole aphid ketone, 10% ether chrysanthemum ester, 5%TERSPERSE 2700 (polycarboxylate, U.S. Huntsman Corporation produces), 3% dispersing agent NNO (alkylnaphthalene sulfonate formaldehyde condensation products), 3% Nekal BX (nekal), 2%K-12 (lauryl sodium sulfate), 10% glucose, 10% sulphur ammonium, kaolin adds to 100% weight portion.The method of the frequent regulation of above-mentioned raw materials water intaking dispersible granule is promptly mixed, ultra micro comminution by gas stream, mixing, granulation step are produced 40% pyrrole aphid ether ketone chrysanthemum ester water dispersible granules.
The part by weight of pyrrole aphid ketone and ether chrysanthemum ester can be 1 in the present embodiment: 2-3: change between 1, both total weight items still are 40%, form new embodiment.FORMULATION EXAMPLE 12:
Take by weighing 5% pyrrole aphid ketone, 10% ether chrysanthemum ester, 4% agricultural newborn 500#, 2% agricultural newborn 600#, 3% agricultural newborn 2201#, 3% triphenyl phosphite, 20% dimethyl sulfoxide (DMSO), solvent naphtha S-180 add to 100% weight portion.Above-mentioned raw materials makes 15% pyrrole aphid ether ketone chrysanthemum emulsifiable concentrate after mix, stirring and dissolving is complete.
The part by weight of pyrrole aphid ketone and ether chrysanthemum ester can be 1 in the present embodiment: 2-3: change between 1, both total weight items still are 15%, form new embodiment.
FORMULATION EXAMPLE 13:
Take by weighing 10% pyrrole aphid ketone, 12% ether chrysanthemum ester, 5% agricultural newborn 500#, 2% agricultural newborn 400#, 3% Nongru-700 #, 3% epoxychloropropane, 20%N-methyl pyrrolidone, 10% cyclohexanone, xylol add to 100% weight portion.Above-mentioned raw materials makes 22% pyrrole aphid ether ketone chrysanthemum emulsifiable concentrate after mix, stirring and dissolving is complete.
The part by weight of pyrrole aphid ketone and ether chrysanthemum ester can be 1 in the present embodiment: 2-3: change between 1, both total weight items still are 22%, form new embodiment.
FORMULATION EXAMPLE 14:
Take by weighing 4% pyrrole aphid ketone, 8% ether chrysanthemum ester, 3% agricultural newborn 2201#, 2% Nonyl pheno (EO=10) ether phosphate, 2% triphen ethyl-phenol polyoxyethylene ether phosphate, 2% this dish-60#, 1% epoxychloropropane, 5% ethylene glycol; 20% xylol, 15% cyclohexanone, 0.2% xanthans, 0.5% benzoic acid, deionized water adds to 100% weight portion.Above-mentioned raw materials is through mixing, and high speed shear emulsification makes 12% pyrrole aphid ether ketone chrysanthemum ester aqueous emulsion.
The part by weight of pyrrole aphid ketone and ether chrysanthemum ester can be 1 in the present embodiment: 2-3: change between 1, both total weight items still are 12%, form new embodiment.
FORMULATION EXAMPLE 15
Take by weighing 20% pyrrole aphid ketone, 10% ether chrysanthemum ester, 4%TX-10,2% agricultural newborn 1601#, 1% epoxychloropropane, 30% dimethyl formamide, methyl alcohol and add to 100% weight portion.Above-mentioned raw materials makes 30% pyrrole aphid ether ketone chrysanthemum ester soluble concentrate after mix, stirring and dissolving is complete.
The part by weight of pyrrole aphid ketone and ether chrysanthemum ester can be 1 among the embodiment: 2-3: change between 1, both total weight items still are 30%, form new embodiment.
FORMULATION EXAMPLE 16
Take by weighing 15% pyrrole aphid ketone, 5% ether chrysanthemum ester, 4%TX-10,5% Nongru-700 #, 6% agricultural newborn 500#, 4% agricultural newborn 1601#, 30% cyclohexanone, 10%N-methyl pyrrolidone, 5% n-butanol, 1% epoxychloropropane, fully and mix through dissolving; Deionized water adds to 100% weight portion, makes 20% pyrrole aphid ether ketone chrysanthemum ester microemulsion after the stirring.
The part by weight of pyrrole aphid ketone and ether chrysanthemum ester can be 1 among the embodiment: 2-3: change between 1, both total weight items still are 20%, form new embodiment.
Biological Examples 1: prevent and treat the rice hoppers field trial
The Shishou county carried out 20% pyrrole aphid ether ketone chrysanthemum ester (10% pyrrole aphid ketone+10% ether chrysanthemum ester) suspending agent and has prevented and treated the field control effectiveness test of rice hoppers the inventor in Hubei Province on July 20th, 2008, had verified that this medicament is to the control efficiency of rice fulgorid, effective dose and to the safety of paddy rice.Trial crops is a paddy rice, controlling object brown planthopper (Panonychus citri Me Gregor).Test medicine and dosage are 20% pyrrole aphid ether ketone chrysanthemum ester suspending agent 20ml/ mu, 30ml/ mu, 40ml/ mu, 10% ether chrysanthemum ester suspending agent 90ml/ mu, and 25% pymetrozine suspension agent 30ml/ mu adopts conventional spray-on process.Respectively at respectively carrying out once residual borer population investigation before the medicine, behind the medicine in 2 days, 7 days, 14 days.Take the random sampling of balance great-jump-forward, every sub-district 10 points, 2 clumps every (totally 20 clumps), with basin bat method record rice fulgorid (brown planthopper) borer population, by before every clump of medicine, the borer population calculation correction preventive effect (hereinafter to be referred as preventive effect) behind the medicine, and carry out the significance of difference and measure.While is 2,7,14 days observation paddy growth situation behind medicine, and the visual test medicament has or not poisoning to produce to paddy rice.
Computational methods:
Figure G2009100233532D00121
In the formula: Pt 0Before-----treatment region medicine; Pt 1Behind-----treatment region medicine
CK 0Before the medicine of-----check plot; CK 1Behind the medicine of-----check plot
Table 1 20% pyrrole aphid ether ketone chrysanthemum ester suspending agent is prevented and treated the rice hoppers result of the test
Figure G2009100233532D00122
To behind the medicine the 14th day the time each sub-district preventive effect carry out biostatistics analysis (seeing table 1), analysis result shows: handle differences and reach extremely outstanding level, district's group difference is not remarkable.Significance of difference comparative result shows: on 0.05 level with 0.01 level on the significance of difference consistent; 20% pyrrole aphid ether ketone chrysanthemum ester suspending agent 40ml/ mu and 30ml/ mu 2 are handled differences and are all reached utmost point significance level; 2 handle all with its 20ml/ mu and contrast medicament 10% ether chrysanthemum ester suspending agent 90ml/ mu, 25% pymetrozine suspension agent 30ml/ mu and handle differences and all reach utmost point significance level, test medicine 20% pyrrole aphid ether ketone chrysanthemum ester suspending agent 20ml/ with contrast medicament 10% ether chrysanthemum ester suspending agent 90ml/ mu, 3 processing of 25% pymetrozine suspension agent 30ml/ mu differences is all not remarkable.
Field test results shows (seeing table 1): 20% pyrrole aphid ether ketone chrysanthemum ester suspending agent has remarkable prevention effect to rice hoppers, has after ether chrysanthemum ester and pyrrole aphid ketone are mixed that dosage is few, the control efficiency advantages of higher; Solve the problem of pyrrole aphid ketone quick-acting difference, practiced thrift drug cost and dosage, and good to rice safety property, therefore have wide practical use in the production.
Biological Examples 2: prevent and treat the rice hoppers field trial
The fairy house county carried out 25% pyrrole aphid ether ketone chrysanthemum ester (15% pyrrole aphid ketone+10% ether chrysanthemum ester) suspending agent and has prevented and treated the field control effectiveness test of rice hoppers the inventor in Zhejiang Province on July 26th, 2008, had verified that this medicament is to the control efficiency of rice fulgorid, effective dose and to the safety of paddy rice.Trial crops is a paddy rice, controlling object brown planthopper (Panonychus citri Me Gregor).Test medicine and dosage are 25% pyrrole aphid ether ketone chrysanthemum ester suspending agent 10ml/ mu, 20ml/ mu, 30ml/ mu, 10% ether chrysanthemum ester suspending agent 80ml/ mu, and 25% pymetrozine suspension agent 30ml/ mu adopts conventional spray-on process.Respectively at respectively carrying out once residual borer population investigation before the medicine, behind the medicine in 2 days, 7 days, 14 days.Take the random sampling of balance great-jump-forward, 10 every 2 clumps of every sub-districts (totally 20 clumps), with basin bat method record rice fulgorid (brown planthopper) borer population, by before every clump of medicine, the borer population calculation correction preventive effect (hereinafter to be referred as preventive effect) behind the medicine, and carry out the significance of difference and measure.While is 2,7,14 days observation paddy growth situation behind medicine, and the visual test medicament has or not poisoning to produce to paddy rice.
Computational methods:
Figure G2009100233532D00141
In the formula: Pt 0Before-----treatment region medicine; Pt 1Behind-----treatment region medicine
CK 0Before the medicine of-----check plot; CK 1Behind the medicine of-----check plot
Table 2 25% pyrrole aphid ether ketone chrysanthemum ester suspending agent is prevented and treated the rice hoppers result of the test
Figure G2009100233532D00142
To behind the medicine the 14th day the time each sub-district preventive effect carry out biostatistics analysis (seeing table 2), analysis result shows: handle differences and reach extremely outstanding level, district's group difference is not remarkable.Significance of difference comparative result shows: on 0.05 level with 0.01 level on the significance of difference consistent; 25% pyrrole aphid ether ketone chrysanthemum ester suspending agent 30ml/ mu and 20ml/ mu 2 are handled differences and are all reached utmost point significance level; 2 handle all with its 10ml/ mu and contrast medicament 10% ether chrysanthemum ester suspending agent 80ml/ mu, 25% pymetrozine suspension agent 30ml/ mu processing differences all reaches utmost point significance level; Contrast medicament 25% pymetrozine suspension agent 30ml/ mu and 10% ether chrysanthemum ester suspending agent 80ml/ mu and test medicine 25% pyrrole aphid ether ketone chrysanthemum ester suspending agent 10ml/ mu processing differences and reach utmost point significance level, and test medicine 25% pyrrole aphid ether ketone chrysanthemum ester suspending agent 10ml/ mu is not remarkable with contrast medicament 10% ether chrysanthemum ester suspending agent 80ml/ mu processing differences.
Field test results shows (seeing table 2): 25% pyrrole aphid ether ketone chrysanthemum ester suspending agent has remarkable prevention effect to rice hoppers, has after ether chrysanthemum ester and pyrrole aphid ketone are mixed that dosage is few, the control efficiency advantages of higher; Solve the problem of pyrrole aphid ketone quick-acting difference, practiced thrift drug cost and dosage, and good to rice safety property, therefore have wide practical use in the production.
Biological Examples 3: prevent and treat the rice hoppers indoor virulence test
In order to prevent and treat the rice fulgorid in the agricultural production, the inventor has carried out mutual composite synergy research with ether chrysanthemum ester, pyrrole aphid ketone effective active composition.It is tested object that rice fulgorid is adopted in test, and concrete grammar is:
1) the former medicine of rice fulgorid (brown planthopper Nilaparvata lugens) test medicine ether chrysanthemum ester adopts the former medicine of Mitsui KCC production, the former medicine that the former medicine of pyrrole aphid ketone adopts Jiangsu Anpon Electrochemical Co., Ltd. to produce.By technology department of Shanggezhilu Biosciences Co., Ltd., Shaanxi former medicine is mixed with the test medicine that needs, test method is with reference to " the agricultural industry criteria NY/T1154.7-2006 of the People's Republic of China (PRC) ".At first single agent and each Mixed Pharmacy are provided with 5 variable concentrations gradient: 12.5g/ug, 25g/ug, 50g/ug, 100g/ug, 200g/ug.The examination worm be rice fulgorid (brown planthopper) pupa that picks up from the field, the water rice seedling raised for 3 generations in the greenhouse, select uniformity four age nymph; Be pressed into the culture dish of putting rice seedling (with the cotton ball processing of preserving moisture) diameter 12cm, every ware connects and anaesthetizes 30 of nymphs, and every processing connects 4 culture dishes; Spray under 50PSI pressure with the potter spray tower, spray a ware at every turn, every ware spraying liquid 3ml; After treating that insect revives; The culture dish of handling is put into the 12H/12H illumination box cultivate, checked dead borer population in 72 hours, calculate lethality.Blank spray equivalent clear water.Carry out statistical analysis with DPS data processor software, calculate the LC of each medicament 50Value is estimated the activity of confession reagent agent to the examination worm with this.
The co-toxicity coefficient of mixture (CTC value) calculates by following formula:
ATI = S M × 100
In the formula: ATI---mixture actual measurement toxicity index;
S---standard insecticide LC 50, unit is every liter (mg/L) of milligram;
The LC of M---mixture 50, unit is every liter (mg/L) of milligram;
TTI=TI A×P A+TI B×P B
In the formula: TTI---the theoretical toxicity index of mixture;
TI A---A medicament toxicity index;
P A---the percentage composition of A medicament in mixture, unit are percentage (%);
TI B---B medicament toxicity index;
P B---the percentage composition of B medicament in mixture, unit are percentage (%);
CTC = ATI TTI × 100
In the formula: CTC---co-toxicity coefficient;
ATI---mixture actual measurement toxicity index;
The theoretical toxicity index of TTI---mixture;
2) rice fulgorid mensuration result sees table 3 respectively.
Table 3 different disposal is to the toxicity test result of rice fulgorid
Handle Virulence regression equation LC50 (mg/L) Actual measurement toxicity index ATI Theoretical toxicity index TTI Co-toxicity coefficient (CTC)
Ether chrysanthemum ester (A) Y=2.6657+1.7205X 22.74 100 - -
Pyrrole aphid ketone (B) Y=2.0977+1.4899X 88.69 25.64 - -
A∶B=5∶15 Y=2.2516+1.7401X 37.97 59.89 44.23 135.40
A∶B=10∶10 Y=3.3441+1.3158X 18.14 125.25 62.82 199.38
A∶B=10∶15 Y=2.9022+1.7943X 14.76 153.93 55.38 277.95
A∶B=15∶10 Y=3.2389+1.4728X 15.69 144.93 70.26 206.28
A∶B=20∶10 Y=3.2081+1.4198X 18.29 124.33 75.54 164.59
Can find out that from table 3 ether chrysanthemum ester and Pyraphione compound have very high synergistic effect to rice fulgorid, each Mixed Pharmacy co-toxicity coefficient all reaches between 130~277.
In sum, composition of the present invention is to adopt two kinds of active component compound schemes, and its activity and insecticidal effect are not the simple superposition of each composition activity; Compare with existing single preparation, except that having significant insecticidal effect, and significant synergistic effect is arranged; Quick-acting is high, lasting effect is long, slows down the generation of resistance, the preparation less residue; Pollution-free to crop, safety is good, meets the security requirement of pesticidal preparations.

Claims (6)

1. Pesticidal combination that contains pyrrole aphid ketone and ether chrysanthemum ester is characterized in that comprising:
A) the first active component pyrrole aphid ketone;
B) the second active component ether chrysanthemum ester;
The weight ratio of first active component and second active component is 1: 2~3: 1.
2. Pesticidal combination according to claim 1 is characterized in that: the cumulant of pyrrole aphid ketone and ether chrysanthemum ester is 5%~90% of a said composition total weight.
3. Pesticidal combination according to claim 2 is characterized in that: the cumulant of pyrrole aphid ketone and ether chrysanthemum ester is 10%~50% of a said composition total weight.
4. according to one of any described Pesticidal combination of claim 1 to 3, it is characterized in that: said composition can be mixed with agricultural and go up any formulation that allows.
5. Pesticidal combination according to claim 4 is characterized in that: said composition can be mixed with water dispersible granules, wetting powder, suspending agent, oil-suspending agent, suspended emulsion, missible oil, microemulsion, aqueous emulsion, soluble concentrate formulation.
6. the said purposes of Pesticidal combination in preventing and kill off rice hoppers that contains pyrrole aphid ketone and ether chrysanthemum ester of claim 1.
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