CN108077303A - A kind of Pesticidal combination of brominated worm fluorobenzene bisamide and indoxacarb - Google Patents

A kind of Pesticidal combination of brominated worm fluorobenzene bisamide and indoxacarb Download PDF

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Publication number
CN108077303A
CN108077303A CN201810121195.3A CN201810121195A CN108077303A CN 108077303 A CN108077303 A CN 108077303A CN 201810121195 A CN201810121195 A CN 201810121195A CN 108077303 A CN108077303 A CN 108077303A
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China
Prior art keywords
indoxacarb
fluorobenzene bisamide
worm fluorobenzene
pesticidal combination
bromine worm
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CN201810121195.3A
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Inventor
赵立荣
黄瑛
张小敏
吕伟民
何焯荣
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Hunan Zefeng Agrochemical Co Ltd
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Hunan Zefeng Agrochemical Co Ltd
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Priority to CN201810121195.3A priority Critical patent/CN108077303A/en
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    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
    • A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
    • A01N47/38—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< where at least one nitrogen atom is part of a heterocyclic ring; Thio analogues thereof
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/44—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a nitrogen atom attached to the same carbon skeleton by a single or double bond, this nitrogen atom not being a member of a derivative or of a thio analogue of a carboxylic group, e.g. amino-carboxylic acids
    • A01N37/46—N-acyl derivatives

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  • Life Sciences & Earth Sciences (AREA)
  • Agronomy & Crop Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Plant Pathology (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Dentistry (AREA)
  • General Health & Medical Sciences (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The present invention relates to pesticide fields, disclose a kind of Pesticidal combination, and active ingredient is bromine worm fluorobenzene bisamide and indoxacarb, and the mass ratio of the two is 10:1~1:20, preferably than for 2:1~1:5.Pesticidal combination of the present invention can be made into wettable powder, water dispersible granules, suspending agent, suspension emulsion, aqueous emulsion, microemulsion.There is apparent synergistic effect after two groups of active ingredients compounding of the present invention, dosage can be reduced, expand insecticidal spectrum, improve pest lethal speed, extend the duration of desinsection, delaying drug resistance, to crop safety, Environmental security.

Description

A kind of Pesticidal combination of brominated worm fluorobenzene bisamide and indoxacarb
Technical field
The invention belongs to technical field of pesticide, it is related to the Pesticidal combination of a kind of brominated worm fluorobenzene bisamide and indoxacarb, For preventing crops class pest.
Background technology
Bromine worm fluorobenzene bisamide：English name：Broflanilide, molecular formula：C25H14BrF11N2O2。
Structural formula：
Bromine worm fluorobenzene bisamide as a kind of novel pesticide, is cooperated by Mitsui Agrichimie and BASF Exploitation.It is mainly used for preventing and kill off Lepidoptera, coleoptera, termite and mosquito on the crops such as green vegetable, perennial crop and cereal The pests such as fly.
Indoxacarb：English name：Indoxacarb, chemical name：Chloro- 2,3,4a, the 5- tetrahydrochysenes -2- [methoxycarbonyls of 7- （4- Trifluoromethoxyphen-ls）Carbamoyl] indeno [1,2-e] [1,3,4] oxadiazine -4a- methyl formates.Molecular formula： C22H17ClF3N3O7。
Structural formula：
Indoxacarb is du pont company（E.I.du Pont de Nemours and Company）Kai Fa oxadiazine classes are new Type efficient pesticides.Trade name Anda.Indoxacarb has unique mechanism of action, mainly blocks in pest nerve cell Sodium channel causes target pest paralysis, final death.With tagging and stomach poison function.Medicament is by tagging and ingesting into worm Body, the behavior of pest change rapidly, and pest is caused to terminate rapidly and is ingested, so as to which fabulous protects Target crops.Indoxacarb is fitted Crop has vegetables such as wild cabbage, cabbage mustard, cauliflower, tomato, eggplant, capsicum；Melon such as cucumber, lettuce；Fruit tree such as apple Tree, peach, apricot, grape etc.；Crop such as cotton, corn, potato.Prevent object from having lepidoptera pest such as bollworm, dish Blue or green worm, oriental tobacco budworm, diamondback moth, beet armyworm, prodenia litura, cabbage looper, leaf rollers, leafhopper, grape-berry moth, grape Long hair leaf roller, spark, cotton leafroller etc..
The long-time service of single insecticide so that resistance enhances, and dosage is continuously increased, and environmental pollution aggravates.Two kinds of medicines The compounding of agent can effectively solve the problem that this problem.Inventor is had found by the research of a large amount of indoor biometrics and field control effectiveness test Bromine worm fluorobenzene bisamide and indoxacarb are combined application, and synergistic effect is apparent, can reduce dosage, delaying drug resistance, to ring Border safety.
The content of the invention
It is an object of the present invention to propose that a kind of synergistic effect is apparent, it being capable of delaying drug resistance, the desinsection group of reduction usage amount Close object.
To solve the above-mentioned problems, the technical solution adopted in the present invention is：
The Pesticidal combination of a kind of brominated worm fluorobenzene bisamide and indoxacarb proposed by the present invention, it is characterised in that：The desinsection Composition contains active ingredient bromine worm fluorobenzene bisamide and active ingredient indoxacarb.
The Pesticidal combination contains active ingredient bromine worm fluorobenzene bisamide and active ingredient indoxacarb, the mass ratio of the two For 10:1~1:20, the quality of the two is preferably than for 2:1~1:5.
The Pesticidal combination, it is characterised in that：The gross mass percentage composition of active ingredient in the Pesticidal combination For 5% ~ 80%, preferably 10% ~ 60%.According to different preparation types, active constituent content scope is different.It is in general, solid The gross mass of body preparation active ingredient is 5% ~ 70%, is preferably 10% ~ 60%；The gross mass of liquid preparation active ingredient for 10% ~ 50%, it is preferably 10% ~ 40%.
The Pesticidal combination can be processed into the arbitrary dosage form agriculturally allowed, wherein more preferably dosage form have it is wettable Property pulvis, water dispersible granules, suspending agent, suspension emulsion, aqueous emulsion, microemulsion.
When above-described Pesticidal combination is wettable powder, following component is included in preparation：Bromine worm fluorobenzene bisamide 1% ~ 50%, indoxacarb 1% ~ 50%, dispersant 2% ~ 10%, wetting agent 2% ~ 8%, filler supplement surplus.
When above-described Pesticidal combination is water dispersible granules, following component is included in preparation：Bromine worm fluorobenzene bisamide 1% ~ 50%, indoxacarb 1% ~ 50%, dispersant 3% ~ 9%, wetting agent 1% ~ 8%, disintegrant 1% ~ 10%, filler supplement surplus.
When above-described Pesticidal combination is suspending agent, following component is included in preparation：Bromine worm fluorobenzene bisamide 0.1% ~ 40%th, indoxacarb 0.1% ~ 40%, dispersant 2% ~ 10%, wetting agent 2% ~ 10%, antifoaming agent 0.1% ~ 1%, thickener 0.1% ~ 2%, antifreeze Agent 0.1% ~ 8%, deionized water add to 100%.
When above-described Pesticidal combination is suspension emulsion, following component is included in preparation：Bromine worm fluorobenzene bisamide 0.1% ~ 40%th, indoxacarb 0.1% ~ 40%, emulsifier 2% ~ 12%, dispersant 2% ~ 10%, antifoaming agent 0.1% ~ 2%, thickener 0.1% ~ 2%, antifreeze Agent 0.1% ~ 8%, preservative 0.05% ~ 3%, deionized water add to 100%.
When above-described Pesticidal combination is aqueous emulsion, following component is included in preparation：Bromine worm fluorobenzene bisamide 0.1% ~ 50%th, indoxacarb 0.1% ~ 50%, solvent 1% ~ 30%, emulsifier 1% ~ 15%, antifreezing agent 0.1% ~ 10%, thickener 0.1% ~ 2%, defoaming Agent 0.01% ~ 2%, deionized water add to 100%.
When above-described Pesticidal combination is microemulsion, following component is included in preparation：Bromine worm fluorobenzene bisamide 0.1% ~ 50%th, indoxacarb 0.1% ~ 50%, solvent 1% ~ 30%, emulsifier 3% ~ 20%, antifreezing agent 0.1% ~ 10%, thickener 0.1% ~ 2%, defoaming Agent 0.01% ~ 2%, preservative 0.05% ~ 4%, deionized water add to 100%.
Of the present invention dose can be prepared as the method well known to those skilled in the art.Wherein, more than preparation
Wetting agent, dispersant used in various preparations, disintegrant, antifoaming agent, thickener, antifreezing agent, preservative, solvent, emulsification Agent, filler are well known to those skilled in the art.
The dispersant is selected from：It is alkylnaphthalene sulfonate, double（Alkyl）Naphthalenesulfonate formaldehyde condensation compound, naphthalenesulfonateformaldehyde formaldehyde contracting Close object, aryl phenol polyoxyethylene succinate sulfonate, octylphenol polyethylene oxyethylene group ether sulfate, polycarboxylate, sulfomethylated lignin Hydrochlorate, to methoxyl group fatty acyl anilinesulfonic acid, APES formaldehyde condensation products sulfat, alkyl benzene calcium sulfonate Salt, naphthalene sulfonic acid-formaldehyde condensation product sodium salt, alkylphenol polyoxyethylene ether, aliphatic amine polyoxyethylene ether, polyoxyethylene carboxylate, ester One or more in polyoxyethylene ether.
The wetting agent is selected from：Lauryl sodium sulfate, neopelex, pull open powder X, wetting and penetrating agent F, One or more in spaonin powder, silkworm excrement, spaonin powder.
The disintegrant is selected from：In bentonite, ammonium sulfate, citric acid, urea, aluminium chloride, succinic acid, sodium acid carbonate It is one or more.
The solvent is selected from：N,N-Dimethylformamide, cyclohexanone, methanol, ethyl alcohol, 3-methyl cyclohexanol ketenes, N- are pungent Base pyrrolidones, N- pyrrolidones, propyl alcohol, butanol, ethylene glycol, diethylene glycol, ethylene glycol monomethyl ether, butyl ether, ethyl acetate, plant One or more in oil, acetonitrile.
The emulsifier is selected from：Alkyl benzene sulfonate calcium salt, styrene polyoxyethylene ether ammonium sulfate salt, alkyl biphenyl ether two Sulfonic acid magnesium salts, triethanolamine salt, phenethyl phenol polyethenoxy ether, 506#, 600#, 700#, NP-10 phosphate, OP-10 phosphoric acid One or more in ester, castor oil polyoxyethylene ether, sorbester p17, Tween 80,602#.
The antifreezing agent is selected from：One or more in ethylene glycol, propylene glycol, glycerine, polyethylene glycol.
The preservative is selected from：Sodium benzoate, sodium propionate, butyl p-hydroxybenzoate, dimethyl fumarate, sorbic acid One or more in potassium, sodium Diacetate.
The antifoaming agent is selected from：C8~10Aliphatic alcohols, C10~20Saturated fat acids（Such as capric acid）And amide, silicone oil, have One or more in machine silicone compound.
The thickener is selected from：Xanthans, hydroxymethyl cellulose, hydroxyethyl cellulose, methylcellulose, magnesium silicate One or more in aluminium, polyvinyl alcohol.
The filler is selected from：In kaolin, diatomite, bentonite, attapulgite, white carbon, starch, precipitated calcium carbonate One or more.
The Pesticidal combination for preventing and kill off lepidoptera pest, is especially changed rice/rice leaf roller, rice/bis- Snout moth's larva, the prevention of wild cabbage/beet armyworm.
The advantage of the invention is that：The two compounds, and shows significant synergistic effect within the specific limits, can reduce use Dose reduces cost；It being capable of delaying drug resistance；It is safe, environmentally friendly environmental protection.
Specific embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, present invention specific examples below It illustrates, but the present invention is limited to absolutely not this.Percentage in embodiment is weight percentage.
Implementation of an application example one：Bromine worm fluorobenzene bisamide and indoxacarb compound product example of formulations（Following content is folding Hundred percentage compositions）, but the present invention is not limited to the proportion in following embodiment.
Wettable powder（Example of formulations 1 ~ 3）
The specific procedure of processing of Pesticidal combination wettable powder is：According to formula by active ingredient bromine worm fluorobenzene bisamide, work Property ingredient indoxacarb, dispersant, wetting agent, filler mixing, be uniformly mixed in mixed cylinder, mixed again after airslide disintegrating mill crushes It closes uniform, you can wettable powder of the present invention is made.
1 45% bromine worm fluorobenzene bisamide indoxacarb wettable powder of example of formulations
Bromine worm fluorobenzene bisamide 30%, indoxacarb 15%, ester APEO（Dispersant）7%th, lauryl sodium sulfate（Wetting agent） 7%th, starch adds to 100%, and 45% bromine worm fluorobenzene bisamide indoxacarb wettable powder is made.
2 50% bromine worm fluorobenzene bisamide indoxacarb wettable powder of example of formulations
Bromine worm fluorobenzene bisamide 10%, indoxacarb 40%, alkylnaphthalene sulfonate（Dispersant）9%th, spaonin powder（Wetting agent）6%th, it is high Ridge soil adds to 100%, and 50% bromine worm fluorobenzene bisamide indoxacarb wettable powder is made.
3 30% bromine worm fluorobenzene bisamide indoxacarb wettable powder of example of formulations
Bromine worm fluorobenzene bisamide 25%, indoxacarb 5%, octylphenol polyethylene oxyethylene group ether sulfate（Dispersant）5%th, pull open powder X（Profit Humectant）4%th, bentonite adds to 100%, and 30% bromine worm fluorobenzene bisamide indoxacarb wettable powder is made.
Water dispersible granules（Example of formulations 4 ~ 6）
The specific procedure of processing of Pesticidal combination water dispersible granules is：According to formula by active ingredient bromine worm fluorobenzene bisamide, will Active ingredient indoxacarb, dispersant, wetting agent, disintegrant, filler are uniformly mixed, and are crushed with micro jet, through mediating, Then add in fluidized-bed granulation dryer after being granulated, drying, sieve, you can water-dispersible grain of the present invention is made Agent.
4 40% bromine worm fluorobenzene bisamide indoxacarb water dispersible granule of example of formulations
Bromine worm fluorobenzene bisamide 20%, indoxacarb 20%, lignosulfonates（Dispersant）6%th, wetting and penetrating agent F（Wetting agent）6%、 Citric acid（Disintegrant）7%th, attapulgite adds to 100%, and 40% bromine worm fluorobenzene bisamide indoxacarb water dispersible granule is made.
5 60% bromine worm fluorobenzene bisamide indoxacarb water dispersible granule of example of formulations
Bromine worm fluorobenzene bisamide 15%, indoxacarb 45%, alkylphenol polyoxyethylene ether（Dispersant）8%th, spaonin powder（Wetting agent）7%、 Succinic acid（Disintegrant）9%th, precipitated calcium carbonate adds to 100%, and 60% bromine worm fluorobenzene bisamide indoxacarb water dispersible granule is made.
6 33% bromine worm fluorobenzene bisamide indoxacarb water dispersible granule of example of formulations
Bromine worm fluorobenzene bisamide 30%, indoxacarb 3%, alkyl benzene sulfonate calcium salt（Dispersant）5%th, silkworm excrement（Wetting agent）4%th, bentonite （Disintegrant）5%th, white carbon adds to 100%, and 33% bromine worm fluorobenzene bisamide indoxacarb water dispersible granule is made.
Suspending agent（Example of formulations 7 ~ 9）
The specific procedure of processing of Pesticidal combination suspending agent is：According to formula by dispersant, wetting agent, antifoaming agent, thickener, anti- Freeze agent to be uniformly mixed by high speed shear, active ingredient bromine worm fluorobenzene bisamide, active ingredient indoxacarb are added, in ball mill When middle ball milling 2 ~ 3 is small, make diameter of particle all below 5 μm, you can suspending agent of the present invention is made.
7 15% bromine worm fluorobenzene bisamide indoxacarb suspending agent of example of formulations
It is bromine worm fluorobenzene bisamide 12%, indoxacarb 3%, double（Alkyl）Naphthalenesulfonate formaldehyde condensation compound（Dispersant）5%th, dodecyl Benzene sulfonic acid sodium salt（Wetting agent）4%、C8~10Aliphatic alcohols（Antifoaming agent）0.4%th, polyvinyl alcohol（Thickener）0.5%th, ethylene glycol（It is antifreeze Agent）0.6%th, deionized water supplies surplus, and 15% bromine worm fluorobenzene bisamide indoxacarb suspending agent is made.
8 12% bromine worm fluorobenzene bisamide indoxacarb suspending agent of example of formulations
Bromine worm fluorobenzene bisamide 4%, indoxacarb 8%, aryl phenol polyoxyethylene succinate sulfonate（Dispersant）3%th, silkworm excrement（Profit Humectant）3%th, silicone oil（Antifoaming agent）0.2%th, hydroxyethyl cellulose（Thickener）0.3%th, glycerine（Antifreezing agent）0.4%th, deionized water Surplus is supplied, 12% bromine worm fluorobenzene bisamide indoxacarb suspending agent is made.
9 18% bromine worm fluorobenzene bisamide indoxacarb suspending agent of example of formulations
Bromine worm fluorobenzene bisamide 3%, indoxacarb 15%, APES formaldehyde condensation products sulfat（Dispersant）6%th, draw Open powder X（Wetting agent）5%th, silicone oil（Antifoaming agent）0.5%th, xanthans（Thickener）0.7%th, polyethylene glycol（Antifreezing agent）0.9%th, go from Sub- water supplies surplus, and 18% bromine worm fluorobenzene bisamide indoxacarb suspending agent is made.
Suspension emulsion（Example of formulations 10 ~ 12）
The specific procedure of processing of Pesticidal combination suspension emulsion is：Dispersant, antifoaming agent, thickener, antifreezing agent are passed through according to formula It crosses high speed shear-mixed and is uniformly added into active ingredient bromine worm fluorobenzene bisamide, when ball milling 2 ~ 3 is small in the ball mill, make diameter of particle All below 5 μm, bromine worm fluorobenzene bisamide suspension agent is made, then by active ingredient indoxacarb, emulsifier and various auxiliary agents It is directly emulsified with high speed agitator in suspending agent, you can suspension emulsion of the present invention is made.
10 33% bromine worm fluorobenzene bisamide indoxacarb suspending agent of example of formulations
Bromine worm fluorobenzene bisamide 3%, indoxacarb 30%, alkyl benzene sulfonate calcium salt（Emulsifier）7%th, to methoxyl group fatty acyl amido benzene Sulfonic acid（Dispersant）8%、C10~20Saturated fat acids（Antifoaming agent）1%th, hydroxymethyl cellulose（Thickener）1%th, propylene glycol（It is antifreeze Agent）1.5%th, sodium Diacetate（Preservative）0.9%th, deionized water adds to 100%, and 33% bromine worm fluorobenzene bisamide indoxacarb is made and hangs Emulsion.
11 20% bromine worm fluorobenzene bisamide indoxacarb suspending agent of example of formulations
Bromine worm fluorobenzene bisamide 10%, indoxacarb 10%, phenethyl phenol polyethenoxy ether（Emulsifier）6%th, naphthalene sulfonic acid-formaldehyde condensation product Sodium salt（Dispersant）5%th, organic silicone（Antifoaming agent）0.6%th, methylcellulose（Thickener）0.9%th, ethylene glycol（Antifreezing agent） 0.9%th, sodium propionate（Preservative）0.6%th, deionized water adds to 100%, and 20% bromine worm fluorobenzene bisamide indoxacarb suspending agent is made.
12 10% bromine worm fluorobenzene bisamide indoxacarb suspending agent of example of formulations
Bromine worm fluorobenzene bisamide 8%, indoxacarb 2%, alkyl biphenyl ether disulfonic acid magnesium salts（Emulsifier）4%th, polyoxyethylene carboxylate （Dispersant）4%th, silicone oil（Antifoaming agent）0.3%th, hydroxymethyl cellulose（Thickener）0.4%th, glycerine（Antifreezing agent）0.7%th, rich horse Dimethyl phthalate（Preservative）0.3%th, deionized water adds to 100%, and 10% bromine worm fluorobenzene bisamide indoxacarb suspending agent is made.
Aqueous emulsion（Example of formulations 13 ~ 15）
The specific procedure of processing of Pesticidal combination aqueous emulsion is：According to formula by active ingredient bromine worm fluorobenzene bisamide, activity into Indoxacarb, solvent, emulsifier is divided to be added together, makes to be dissolved into homogeneous oil phase；Part water, antifreezing agent, antifoaming agent are blended in one It rises into uniform water phase；In a kettle while high-speed stirred by oil phase add in water phase, add in thickener, slowly plus water until Reach special phase point, open cutter and carry out high speed shear, and add in remaining water, shearing about half an hour, form oil-in-water type Aqueous emulsion.Aqueous emulsion as of the present invention.
13 22% bromine worm fluorobenzene bisamide indoxacarb aqueous emulsion of example of formulations
Bromine worm fluorobenzene bisamide 20%, indoxacarb 2%, cyclohexanone（Solvent）8%th, OP-10 phosphates（Emulsifier）6%th, polyethylene glycol （Antifreezing agent）1.5%th, aluminium-magnesium silicate（Thickener）0.6%th, organic silicone（Antifoaming agent）0.5%th, deionized water adds to 100%, is made 22% bromine worm fluorobenzene bisamide indoxacarb aqueous emulsion.
14 12% bromine worm fluorobenzene bisamide indoxacarb aqueous emulsion of example of formulations
Bromine worm fluorobenzene bisamide 9%, indoxacarb 3%, N- pyrrolidones（Solvent）4%th, styrene polyoxyethylene ether ammonium sulfate salt（Breast Agent）3%th, polyethylene glycol（Antifreezing agent）0.7%th, methylcellulose（Thickener）0.3%、C8~10Aliphatic alcohols（Antifoaming agent）0.2%、 Deionized water adds to 100%, and 12% bromine worm fluorobenzene bisamide indoxacarb aqueous emulsion is made.
15 30% bromine worm fluorobenzene bisamide indoxacarb aqueous emulsion of example of formulations
Bromine worm fluorobenzene bisamide 5%, indoxacarb 25%, ethylene glycol（Solvent）10%th, castor oil polyoxyethylene ether（Emulsifier）9%th, third Glycol（Antifreezing agent）2%th, hydroxyethyl cellulose（Thickener）0.8%th, silicone oil（Antifoaming agent）0.9%th, deionized water adds to 100%, system Obtain 30% bromine worm fluorobenzene bisamide indoxacarb aqueous emulsion.
Microemulsion（Example of formulations 16 ~ 18）
The specific procedure of processing of Pesticidal combination microemulsion is：According to formula by active ingredient bromine worm fluorobenzene bisamide, activity into Indoxacarb is divided to be dissolved in the homogenizer equipped with solvent and cosolvent, emulsifier, antifreezing agent and water are added to equipped with above-mentioned molten It in the homogenizer of liquid, mixes and homogenizes strongly, the transparent microemulsion of clear appearance is finally made, it is as of the present invention Microemulsion.
16 21% bromine worm fluorobenzene bisamide indoxacarb microemulsion of example of formulations
Bromine worm fluorobenzene bisamide 1%, indoxacarb 20%, 3-methyl cyclohexanol ketenes（Solvent）8%th, Tween 80（Emulsifier）9%th, poly- second two Alcohol（Antifreezing agent）1%th, xanthans（Thickener）0.7%th, organic silicone（Antifoaming agent）0.6%th, butyl p-hydroxybenzoate（Preservative） 0.5%th, deionized water adds to 100%, and 21% bromine worm fluorobenzene bisamide indoxacarb microemulsion is made.
17 15% bromine worm fluorobenzene bisamide indoxacarb microemulsion of example of formulations
Bromine worm fluorobenzene bisamide 10%, indoxacarb 5%, n,N-Dimethylformamide（Solvent）3%th, triethanolamine salt（Emulsifier）6%、 Ethylene glycol（Antifreezing agent）0.4%th, hydroxyethyl cellulose（Thickener）0.3%、C8~10Aliphatic alcohols（Antifoaming agent）0.3%th, sodium benzoate （Preservative）0.2%th, deionized water adds to 100%, and 15% bromine worm fluorobenzene bisamide indoxacarb microemulsion is made.
18 24% bromine worm fluorobenzene bisamide indoxacarb microemulsion of example of formulations
Bromine worm fluorobenzene bisamide 4%, indoxacarb 20%, ethyl acetate（Solvent）9%th, alkyl benzene sulfonate calcium salt（Emulsifier）10%th, third Glycol（Antifreezing agent）1.5%th, methylcellulose（Thickener）0.9%、C10~20Saturated fat acids（Antifoaming agent）0.7%th, potassium sorbate （Preservative）0.6%th, deionized water adds to 100%, and 24% bromine worm fluorobenzene bisamide indoxacarb microemulsion is made.
Implementation of an application example two：The Toxicity Determination experiment of bromine worm fluorobenzene bisamide and indoxacarb compounding
1 bromine worm fluorobenzene bisamide of toxicity test embodiment and indoxacarb test the Toxicity Determination of rice/rice leaf roller
Subjects：Rice/rice leaf roller
Test method：Standard method NY/T 1154.6-2006 are surveyed with reference to raw, using dip method.
Medicament is directly diluted with water to dissolving, then it is dilute with the aqueous solution containing proper amount of surfactant such as 0.1% Tween 80 It releases.According to agent activity, 5-7 series mass concentration are set according to method of ratio or equal difference is waited.Per mass concentration liquid volume No less than 50mL.After target insect is soaked into the liquid 5s-10s, extra liquid is absorbed with filter paper, test worm is transferred to normal item It is raised under part.4 repetitions are often handled, leaching worm 10-20 is often repeated, and sets the processing without medicament as blank control.
Test worm death condition is checked after processing for 24 hours, records total borer population and death toll respectively.It is special according to test requirements document and medicament Point can shorten or extend control time.
According to survey data, the corrected mortality of each processing is calculated, and the co-toxicity coefficient of mixture is calculated according to the abundant methods of Sun Yun （CTC values）.Use statistical analysis system（SAS）, data handling system（DPS）Softwares is waited to be analyzed, calculate the LC of each medicament50、 LC90, b values（Standard error）Equivalent and its 95% confidence limit.
The death rate（%）=death borer population（Head）The total borer population of/processing（Head）×100%
Corrected mortality=（Handle the death rate-blank control death rate）/（The 1- blank control death rates）×100%
Survey toxicity index (ATI)=(standard agent LC50/ reagent agent LC50)×100
Mixture theoretical toxicity index (TTI)=medicament A toxicity indexes × A medicaments percentage (%)+medicament B shared in mixture Toxicity index × B medicaments percentage (%) shared in mixture
Co-toxicity coefficient (CTC)=[mixture actual measurement toxicity index (ATI)/mixture theoretical toxicity index (TTI)] × 100
Co-toxicity coefficient CTC >=120 of complex preparation show as synergistic effect, and 80 ＜ CTC ＜ 120 show as summation action, and CTC≤ 80 show as antagonism.Toxicity Determination result of the test refers to table 1.
The above test results show that active ingredient bromine worm fluorobenzene bisamide and active ingredient indoxacarb compounding prevention rice/ Rice leaf roller is matched 10:1~1:When between 20, co-toxicity coefficient has synergistic effect all more than 120；And 2:1~1:5 Between when, co-toxicity coefficient is above 170, and synergistic effect becomes apparent from.
2 bromine worm fluorobenzene bisamide of toxicity test embodiment and indoxacarb test the Toxicity Determination of rice/striped rice borer
Subjects：Rice/striped rice borer
Test method：Standard method NY/T 1154.1-2006 are surveyed with reference to raw, using drop method.Age neat one is chosen with writing brush The test worm of cause（CO can be used as needed2Or etherization）It is placed in spare in culture dish.Test worm in culture dish is carried out by head Drop processing, lepidopterous larvae drop is on polypide pronotary, every 0.5 μ L-1.0 μ L of drop medicament.By the test worm after drop It is transferred under normal condition and raises respectively.4 repetitions are often handled, often repeat no less than 10 test worms, and set the phase without medicament The processing for the organic solvent answered is as control.
Test worm death condition is checked after processing for 24 hours, records total borer population and death toll respectively.It is special according to test requirements document and medicament Point can shorten or extend control time.
According to survey data, the corrected mortality of each processing is calculated, and the co-toxicity coefficient of mixture is calculated according to the abundant methods of Sun Yun （CTC values）.Use statistical analysis system（SAS）, data handling system（DPS）Softwares is waited to be analyzed, calculate the LC of each medicament50、 LC90, b values（Standard error）Equivalent and its 95% confidence limit.
The death rate（%）=death borer population（Head）The total borer population of/processing（Head）×100%
Corrected mortality=（Handle the death rate-blank control death rate）/（The 1- blank control death rates）×100%
Survey toxicity index (ATI)=(standard agent LC50/ reagent agent LC50)×100
Mixture theoretical toxicity index (TTI)=medicament A toxicity indexes × A medicaments percentage (%)+medicament B shared in mixture Toxicity index × B medicaments percentage (%) shared in mixture
Co-toxicity coefficient (CTC)=[mixture actual measurement toxicity index (ATI)/mixture theoretical toxicity index (TTI)] × 100
Co-toxicity coefficient CTC >=120 of complex preparation show as synergistic effect, and 80 ＜ CTC ＜ 120 show as summation action, and CTC≤ 80 show as antagonism.Toxicity Determination result of the test refers to table 2.
The above test results show that active ingredient bromine worm fluorobenzene bisamide and active ingredient indoxacarb compounding prevention rice/ Striped rice borer is matched 10:1~1:When between 20, co-toxicity coefficient has synergistic effect all more than 120；And 2:1~1:Between 5 When, co-toxicity coefficient is above 170, and synergistic effect becomes apparent from.
3 bromine worm fluorobenzene bisamide of toxicity test embodiment and indoxacarb try the Toxicity Determination of wild cabbage/beet armyworm It tests
Subjects：Wild cabbage/beet armyworm
Test method：Standard method NY/T 1154.14-2008 are surveyed with reference to raw, using leaf dipping method.It will be fresh, open and flat with card punch Host's blade break into leaf dish, beat when taking and to avoid choosing the big and thick position of vein as far as possible.Leaf dish is invaded into 10s in liquid to be measured Afterwards, taking-up is dried, and face of blade is laid in downward in the culture dish for having added good agar with tweezers, accesses test worm, is often repeated not Less than 10.Often processing is no less than 4 repetitions, and sets the processing without medicament as blank control.The test worm of processing is placed in Temperature is（25±1）DEG C, humidity 60%-80%, photoperiod L:D=（16:8）It raises and observes under h condition.
48h checks test worm death condition after processing, records total borer population and death toll respectively.It is special according to test requirements document and medicament Point can shorten or extend control time.
According to survey data, the corrected mortality of each processing is calculated, and the co-toxicity coefficient of mixture is calculated according to the abundant methods of Sun Yun （CTC values）.Use statistical analysis system（SAS）, data handling system（DPS）Softwares is waited to be analyzed, calculate the LC of each medicament50、 LC90, b values（Standard error）Equivalent and its 95% confidence limit.
The death rate（%）=death borer population（Head）The total borer population of/processing（Head）×100%
Corrected mortality=（Handle the death rate-blank control death rate）/（The 1- blank control death rates）×100%
Survey toxicity index (ATI)=(standard agent LC50/ reagent agent LC50)×100
Mixture theoretical toxicity index (TTI)=medicament A toxicity indexes × A medicaments percentage (%)+medicament B shared in mixture Toxicity index × B medicaments percentage (%) shared in mixture
Co-toxicity coefficient (CTC)=[mixture actual measurement toxicity index (ATI)/mixture theoretical toxicity index (TTI)] × 100
Co-toxicity coefficient CTC >=120 of complex preparation show as synergistic effect, and 80 ＜ CTC ＜ 120 show as summation action, and CTC≤ 80 show as antagonism.Toxicity Determination result of the test refers to table 3.
The above test results show that active ingredient bromine worm fluorobenzene bisamide and active ingredient indoxacarb compounding prevention wild cabbage/ Beet armyworm is matched 10:1~1:When between 20, co-toxicity coefficient has synergistic effect all more than 120；And 2:1~1:5 it Between when, co-toxicity coefficient is above 170, and synergistic effect becomes apparent from.
Implementation of an application example three：Bromine worm fluorobenzene bisamide and the field control effectiveness test of indoxacarb compounding
Field information embodiment 1 prevents the field control effectiveness test of rice/rice leaf roller
Reference《Pesticide field efficacy medicine test criterion（One）Insecticide control rice leaf roller GB/T 17980.2-2000》, experiment Medicament, comparison medicament and the processing of the cell of blank control are using random alignment, plot area 40m2, often handle 4 repetitions.
Investigation and statistical method：25 clumps of rice are looked into altogether per 5 points of samplings of cell, leaf roll rate are counted, with check plot leaf roll rate ratio Compared with calculating relative control effect, while investigate in leaf roll and have worm rate.Before processing carries out radix investigation.When blank control is aggrieved apparent or The present age cause harm sizing after carry out efficacy survey, i.e., after medicine 7,15 days investigation.
Leaf roll rate（%）=（Investigate leaf roll number/investigation total number of sheets）×100%；
Control effect（%）=（Leaf roll rate after leaf roll rate-chemicals treatment district medicine after blank district medicine）After/blank district medicine Leaf roll rate × 100%；
Vermins-proof effect（%）=（Borer population living after borer population-chemicals treatment district medicine living after blank district medicine）After/blank district medicine Borer population × 100% living.
As shown in Table 4,7 days after medicine, bromine worm fluorobenzene bisamide and indoxacarb complex preparation embodiment 1,3,4,6,7,8,9, 12nd, 14 preventive effect is 92.21% ~ 94.99%, and larva preventive effect is 93.34% ~ 97.01%.10% bromine worm fluorobenzene bisamide of comparison medicament Suspending agent preventive effect is 68.78%, and larva preventive effect is 78.34%.The preventive effect of 150 g/l of indoxacarb suspending agents of comparison medicament is 73.58%, larva preventive effect is 80.98%, higher than comparison medicament single dose, shows preferable quick-acting.15 days after medicine, all medicaments Preventive effect increases, wherein bromine worm fluorobenzene bisamide and indoxacarb complex preparation embodiment 1,3,4,6,7,8,9,12,14 Preventive effect is 95.03% ~ 97.06%, and larva preventive effect is 97.76% ~ 100%.10% bromine worm fluorobenzene bisamide suspension agent preventive effect of comparison medicament For 75.44%, larva preventive effect is 81.11%.The preventive effect of 150 g/l of indoxacarb suspending agents of comparison medicament is 79.55%, larva preventive effect For 82.49%, higher than comparison medicament single dose, preferable lasting effect is shown.During dispenser, poisoning generation is found no, to crop Safety.
Field information embodiment 2 prevents the field control effectiveness test of rice/striped rice borer
This experiment reference《Pesticide field efficacy medicine test criterion（One）Insecticide control rice Lepidoptera borer pest GB/ T17980.1-2000》, test medicine, comparison medicament and the processing of the cell of blank control are using random alignment, plot area 40m2, often handle 4 repetitions.
Investigation and statistical method：Parallel great-jump-forward sampling, 25-50 clumps of rice are investigated per cell, count withered heart rate or dead ears Number, striped rice borer investigation withered heart rate and the death rate.When the aggrieved shape of blank district is apparent or the present age cause harm sizing after investigated.
The withered heart（Dead ears）Rate（%）The withered heart of=investigation（Dead ears）Total spike number × 100 of rate/investigation；
Preventive effect（%）=[（The withered heart after blank district medicine（Dead ears）The withered heart after rate-chemicals treatment district medicine（Dead ears）Rate）/ blank control The withered heart after area's medicine（Dead ears）Rate] × 100%；
Vermins-proof effect（%）=（Borer population living after borer population-chemicals treatment district medicine living after blank district medicine）After/blank district medicine Borer population × 100% living.
As shown in Table 5, bromine worm fluorobenzene bisamide and indoxacarb complex preparation embodiment 2,3,5,8,10,11,13,15,16 Preventive effect for 92.57% ~ 95.19%, larva preventive effect is 96.41% ~ 98.77%.10% bromine worm fluorobenzene bisamide suspension agent of comparison medicament Preventive effect is 76.53%, and larva preventive effect is 86.17%；The preventive effect of 150 g/l of indoxacarb suspending agents of comparison medicament is 72.30%, larva Preventive effect is 82.61%, higher than comparison medicament single dose, shows preferable control effect.During dispenser, poisoning generation is found no, To crop safety.
Field information embodiment 3 prevents the field control effectiveness test of wild cabbage/beet armyworm
Reference《Pesticide field efficacy medicine test criterion（One）The lepidopterous larvae GB/T of insecticide control brassicaceous vegetable 17980.13-2000》, test medicine, comparison medicament and the processing of the cell of blank control are using random alignment, plot area 40m2, often handle 4 repetitions.
Investigation and statistical method：The work larva number that different larval instar on 10 plants of crops is no less than per cell is counted, investigation is whole A plant.Radix is investigated：Before processing.Second of investigation：1 ~ 3 day after processing.Third time is investigated:7 ~ 14 days after processing.
Revision insect recluced rate（%）=（Borer population after borer population-dispenser before dispenser）Borer population × 100 before/dispenser；
Control effect（%）=（（Chemicals treatment district Revision insect recluced rate-blank district Revision insect recluced rate）/（100-blank control Area's Revision insect recluced rate））×100.
As shown in Table 6,3 days after medicine, bromine worm fluorobenzene bisamide and indoxacarb complex preparation embodiment 1,5,6,8,9,10, 11st, 17,18 preventive effect is 92.41% ~ 95.65%, and 10% bromine worm fluorobenzene bisamide suspension agent preventive effect of comparison medicament is 84.79%, right Preventive effect according to 150 g/l of indoxacarb suspending agents of medicament is 82.56%, higher than comparison medicament single dose, shows preferable quick-acting. 7 days after medicine, bromine worm fluorobenzene bisamide and the preventive effect of indoxacarb complex preparation embodiment 1,5,6,8,9,10,11,17,18 are 95.73% ~ 98.46%, 10% bromine worm fluorobenzene bisamide suspension agent preventive effect of comparison medicament is 81.89%, 150 g/l of indenes of comparison medicament The preventive effect of worm prestige suspending agent is 79.47%, higher than comparison medicament single dose, shows preferable lasting effect.During dispenser, do not find There is poisoning generation, to crop safety.
In conclusion Pesticidal combination bromine worm fluorobenzene bisamide of the present invention is compounded with indoxacarb, rice/rice is indulged Leaf roll snout moth's larva, rice/striped rice borer, wild cabbage/beet armyworm have a significant synergistic effect, expand insecticidal spectrum, can delaying drug resistance, to making Object safety, can reduce dosage, environmentally safe.

Claims (5)

1. a kind of Pesticidal combination of brominated worm fluorobenzene bisamide and indoxacarb, it is characterised in that：The Pesticidal combination contains Active ingredient bromine worm fluorobenzene bisamide and active ingredient indoxacarb, the mass ratio of the two is 10:1~1:20.
2. Pesticidal combination according to claim 1, it is characterised in that：Active ingredient bromine worm fluorobenzene bisamide and activity into Point indoxacarb, the quality of the two is preferably than for 2:1~1:5.
3. Pesticidal combination according to any one of claim 1 to 2, it is characterised in that：It is living in the Pesticidal combination Property ingredient gross mass percentage composition be 5% ~ 80%.
4. Pesticidal combination according to any one of claim 1 to 3, it is characterised in that：It can be made into wettable powder, water Dispersible granule, suspending agent, suspension emulsion, aqueous emulsion, microemulsion.
5. Pesticidal combination according to claim 4, for preventing and kill off lepidoptera pest, especially to rice/cnaphalocrocis The prevention of snout moth's larva, rice/striped rice borer, wild cabbage/beet armyworm.
CN201810121195.3A 2018-02-07 2018-02-07 A kind of Pesticidal combination of brominated worm fluorobenzene bisamide and indoxacarb Pending CN108077303A (en)

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CN111789127A (en) * 2020-07-23 2020-10-20 京博农化科技有限公司 Insecticidal composition containing indoxacarb and cyclic bromoantraniliprole and application thereof
CN112292034A (en) * 2018-06-14 2021-01-29 三井化学Agro株式会社 Insecticide composition
EP3816150A4 (en) * 2018-06-26 2021-10-06 Cac Shanghai International Trading Co., Ltd. M-diamide compound and preparation method therefor and use thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112292034A (en) * 2018-06-14 2021-01-29 三井化学Agro株式会社 Insecticide composition
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EP3816150A4 (en) * 2018-06-26 2021-10-06 Cac Shanghai International Trading Co., Ltd. M-diamide compound and preparation method therefor and use thereof
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CN111789127A (en) * 2020-07-23 2020-10-20 京博农化科技有限公司 Insecticidal composition containing indoxacarb and cyclic bromoantraniliprole and application thereof

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Application publication date: 20180529