CN116784338A - Composition containing flucyclofen or KII-9396 and application thereof - Google Patents

Composition containing flucyclofen or KII-9396 and application thereof Download PDF

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Publication number
CN116784338A
CN116784338A CN202210249245.2A CN202210249245A CN116784338A CN 116784338 A CN116784338 A CN 116784338A CN 202210249245 A CN202210249245 A CN 202210249245A CN 116784338 A CN116784338 A CN 116784338A
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Prior art keywords
compound
composition
percent
agent
kii
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迟会伟
吴建挺
刘莹
徐龙祥
刘立龙
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SHANDONG UNITED PESTICIDE INDUSTRY CO LTD
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SHANDONG UNITED PESTICIDE INDUSTRY CO LTD
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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
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
    • A01N43/80—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,2
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01G—HORTICULTURE; CULTIVATION OF VEGETABLES, FLOWERS, RICE, FRUIT, VINES, HOPS OR SEAWEED; FORESTRY; WATERING
    • A01G13/00—Protecting plants
    • 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
    • A01N41/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a sulfur atom bound to a hetero atom
    • A01N41/02—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a sulfur atom bound to a hetero atom containing a sulfur-to-oxygen double bond
    • A01N41/10—Sulfones; Sulfoxides

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

Abstract

The present invention relates to compositions containing a biologically effective amount of compound I and flucyclofen or KII-9396, and methods for their use in controlling pests in agronomic and non-agronomic environments. The compound I and the flucyclofen or the KII-9396 have a synergistic effect, so that the pest control effect can be improved, the application amount can be reduced, the use times can be reduced, and the use cost can be reduced.

Description

Composition containing flucyclofen or KII-9396 and application thereof
Technical Field
The invention belongs to the technical field of pesticide compounding, and relates to a composition containing a biologically effective amount of a compound I and flucyclofen or KII-9396, and a method for preventing and controlling insect pests in agronomic and non-agronomic environments by using the same.
Background
In recent years, the occurrence of insect pests of various crops tends to be serious year by year, the occurrence area is increased year by year, and huge harm is brought to the crops, so that the problems of crop yield reduction, agricultural production cost increase and the like are caused. The farmers increase the dosage or mix the medicines at will in order to improve the control effect on pests, and the unscientific dosage can not achieve the synergistic effect, but can cause the problems of pesticide waste, exceeding residue, environmental pollution, pest resistance to pesticides and the like. Therefore, development of a synergistic composition for pests is needed to achieve the effects of expanding the range of control objects, reducing the dosage and delaying the generation of resistance.
In the actual process of agricultural production, the same medicament is continuously and singly used for a long time, pests can quickly generate drug resistance, the prevention effect is reduced, the pesticide use amount is increased, and the damage of pesticide residues and ecological environment of agricultural products is aggravated. The compound of the pesticide varieties with completely different action mechanisms is an effective way for delaying the generation of drug resistance of pests, expanding the insecticidal spectrum, prolonging the service life and reducing the using amount of pesticides. However, how to compound the medicines makes the medicines generate synergy rather than antagonism is a great difficulty.
Patent document CN 111909143A discloses a compound I having broad-spectrum insecticidal activity, and particularly having excellent control effects on pests such as Lepidoptera (Lepidoptera), hemiptera (Hemiptera), coleoptera (Coleoptera), thysanoptera (Thysanoptera), diptera, mites, and the like. However, how to compound the medicine with other medicines to achieve the aim of synergism is not disclosed.
The structural formula of the compound I is shown as follows,
disclosure of Invention
In order to ameliorate the deficiencies of the prior art, the present invention first provides a composition comprising compound I and compound II, said compound II being flucyclofen, KII-9396 or a combination thereof,
the structure of the compound I is shown as follows,
the KII-9396 is (RS) - [5- [ 4-chloro-2-fluoro-5- [ (2, 2-trifluoroethyl) sulfinyl ] phenoxy ] pentanyl ] trifluoromethyl sulfide (CAS: 1472050-04-6).
According to an embodiment of the present invention, said compound I is prepared by the method of example 1 in patent document CN 111909143A, which is incorporated herein by reference in its entirety.
According to an embodiment of the invention, the mass ratio of compound I to compound II is 80-1:1-80, preferably 50-1:1-50, more preferably 10-1:1-10, for example 50:1, 40:1, 30:1, 20:1, 10:1, 5:1, 4:1, 3:1, 2:1, 1:1, 1:2, 1:3, 1:4, 1:5, 1:10, 1:20, 1:30, 1:40 or 1:50.
According to embodiments of the present invention, the composition may be prepared as a liquid formulation or a solid formulation.
According to the embodiment of the invention, the content range of the effective active ingredient in the preparation is different according to different preparation types, and generally, the liquid preparation contains 1 to 60 percent of the effective active ingredient by weight, preferably 5 to 50 percent; the solid preparation contains 5-80% by weight of effective active ingredient, preferably 10-70%.
According to an embodiment of the present invention, at least one of deionized water, an organic solvent, an emulsifier, a dispersant, a wetting agent, a thickener, an antifoaming agent, a stabilizer, a binder, a disintegrant, an antifreeze agent, an anticaking agent, a suspending agent, a film former, a preservative, a colorant, a polymeric wall material, a pH adjuster, a filler, or the like is further included in the composition.
According to an embodiment of the invention, the sum of the masses of compound I and compound II in the composition is 1 to 80%, preferably 2 to 70%, or 5 to 65%, based on 100% of the total weight of the composition; 10-60%, for example 1%, 5%,10%, 15%, 20%, 25%, 30%, 35%, 40%, 45% or 50%.
According to embodiments of the present invention, the composition may be diluted by the user prior to use or used directly. The preparation can be prepared by a processing method known to a person skilled in the art, namely, the effective active ingredients (namely the compound I and the compound II) are mixed with one or more of deionized water, an organic solvent, an emulsifying agent, a dispersing agent, a wetting agent, a thickening agent, a defoaming agent, a stabilizing agent, a binding agent, a disintegrating agent, an antifreeze agent, an anticaking agent, a suspending agent, a film forming agent, a preservative, a coloring agent, a polymer capsule wall material, a pH regulator or a filler and the like to prepare the composition.
According to embodiments of the present invention, the composition may be formulated into various dosage forms, preferably, the dosage forms include wettable powders, water dispersible granules, suspension concentrates, aqueous emulsions, suspension seed coatings, microcapsule suspensions, microcapsule suspension-suspensions, emulsifiable concentrates, microemulsions, dispersible solutions, or granules.
According to an embodiment of the invention, the composition is prepared into wettable powder and comprises the following components in percentage by weight: 1-80% of compound I, 1-80% of compound II, 0-10% of dispersing agent, 0-8% of wetting agent and the balance of filler.
Preferably, the compound I in the composition is 2% -70%, 5% -65%, 10% -60%, 15% -50% and the like;
2-70%, 5-65%, 10-60%, 15-50% and the like of the compound II;
1-8% of dispersing agent, 2-7% of dispersing agent, 3-6% or 4-5% of dispersing agent;
the wetting agent is 1 to 8 percent, 2 to 7 percent, 3 to 6 percent or 4 to 5 percent. According to the embodiment of the invention, the composition comprises the following components in percentage by weight when being prepared into water dispersible granules: 1-80% of compound I, 1-80% of compound II, 0-10% of dispersing agent, 0-16% of wetting agent, 0-20% of disintegrating agent and the balance of filler.
Preferably, the compound I in the composition is 2% -70%, 5% -65%, 10% -60%, 15% -50% and the like;
2-70%, 5-65%, 10-60%, 15-50% and the like of the compound II;
1-8% of dispersing agent, 2-7% of dispersing agent, 3-6% or 4-5% of dispersing agent;
1-8% of wetting agent, 2-7% of wetting agent, 3-6% or 4-5% of wetting agent;
1 to 18 percent of disintegrating agent, 2 to 16 percent of disintegrating agent, 3 to 15 percent, 4 to 12 percent, 5 to 10 percent or 6 to 8 percent.
According to an embodiment of the invention, the composition is prepared into a suspending agent and comprises the following components in percentage by weight: 1-50% of compound I, 1-50% of compound II, 0-5% of dispersing agent, 0-8% of wetting agent, 0-0.3% of thickening agent, 0-5% of antifreeze agent and the balance of deionized water.
Preferably, the compound I in the composition is 2% -45%, 5% -40%, 10% -35%, 15% -30%, 20% -25% and the like;
2 to 45 percent of compound II, 5 to 40 percent, 10 to 35 percent and 15 to 30 percent; 20% -25% and the like;
the dispersant is 1 to 4 percent or 2 to 3 percent;
1-8% of wetting agent, 2-7% of wetting agent, 3-6% or 4-5% of wetting agent;
the thickener is 0.1 to 0.25 percent;
1 to 4 percent or 2 to 3 percent of antifreeze agent. According to the embodiment of the invention, the composition is prepared into an aqueous emulsion and comprises the following components in parts by weight: 1 to 50 percent of compound I, 1 to 50 percent of compound II, 0 to 95 percent of organic solvent, 0 to 10 percent of emulsifier, 0 to 5 percent of antifreeze agent, 0 to 0.2 percent of defoamer, 0 to 0.5 percent of thickener and the balance of deionized water.
Preferably, the compound I in the composition is 2% -45%, 5% -40%, 10% -35%, 15% -30%, 20% -25% and the like;
2 to 45 percent of compound II, 5 to 40 percent, 10 to 35 percent and 15 to 30 percent; 20% -25% and the like;
the organic solvent is 1 to 90 percent, 2 to 80 percent, 5 to 70 percent, 10 to 60 percent and 15 to 50 percent; 20% -50%, 30% -40% and the like;
1-8% of emulsifying agent, 2-7% of emulsifying agent, 3-6% or 4-5% of emulsifying agent;
1 to 4 percent or 2 to 3 percent of antifreeze agent;
0.05 to 0.1 percent of defoaming agent, or
The thickener accounts for 0.1 to 0.4 percent and 0.2 to 0.3 percent. According to the embodiment of the invention, the composition is prepared into a suspended seed coating agent and comprises the following components in parts by weight: 1 to 50 percent of compound I, 1 to 50 percent of compound II, 1 to 12 percent of dispersing agent, 1 to 10 percent of wetting agent, 1 to 10 percent of antifreeze agent, 0.1 to 10 percent of anticaking agent, 0.1 to 5 percent of suspending agent, 1 to 10 percent of film forming agent, 0.1 to 5 percent of preservative, 1 to 30 percent of colorant, 0.1 to 5 percent of pH regulator, 0.1 to 8 percent of thickening agent and the balance of deionized water.
Preferably, the compound I in the composition is 2% -45%, 5% -40%, 10% -35%, 15% -30%, 20% -25% and the like;
2 to 45 percent of compound II, 5 to 40 percent, 10 to 35 percent and 15 to 30 percent; 20% -25% and the like;
2 to 10 percent of dispersing agent, 3 to 8 percent, 4 to 7 percent, or 5 to 6 percent;
1-8% of wetting agent, 2-7% of wetting agent, 3-6% or 4-5% of wetting agent;
1-8% of antifreeze agent, 2-7% of antifreeze agent, 3-6% or 4-5% of antifreeze agent;
the anticaking agent is 0.5 to 9 percent, 1 to 8 percent, 2 to 7 percent, 3 to 6 percent or 4 to 5 percent;
the suspending agent is 0.2-4%, 0.5-3.5%, 1-3%, 1.5-2.5%, or 1.8-2%;
2 to 9 percent of film forming agent, 3 to 8 percent, 4 to 7 percent or 5 to 6 percent;
0.2 to 4 percent of preservative, 0.5 to 3.5 percent, 1 to 3 percent, 1.5 to 2.5 percent or 1.8 to 2 percent;
the colorant is 2-25%, 3-20%, 5-15%, 8-12%, or 9-10%;
0.1 to 5 percent of pH regulator, 0.2 to 4 percent of pH regulator, 0.5 to 3.5 percent of pH regulator, 1 to 3 percent of pH regulator, 1.5 to 2.5 percent of pH regulator, or 1.8 to 2 percent of pH regulator;
the thickener is 0.5-7, 1-6, 2-5, or 3-4%.
According to an embodiment of the invention, the composition is prepared into microcapsule suspending agent and comprises the following components in parts by weight: 1 to 50 percent of compound I, 1 to 50 percent of compound II, 1 to 30 percent of high molecular capsule wall material, 2 to 10 percent of dispersing agent, 1 to 50 percent of organic solvent, 1 to 7 percent of emulsifying agent, 0.1 to 5 percent of pH regulator, 0.01 to 2 percent of defoaming agent, 0.1 to 8 percent of thickening agent, 0.1 to 8 percent of antifreeze agent and the balance of deionized water.
Preferably, the compound I in the composition is 2% -45%, 5% -40%, 10% -35%, 15% -30%, 20% -25% and the like;
2 to 45 percent of compound II, 5 to 40 percent, 10 to 35 percent and 15 to 30 percent; 20% -25% and the like;
2-25% of macromolecular wall material, 5-20%, 6-18% or 10-15% and the like;
3 to 8 percent of dispersing agent, 4 to 7 percent or 5 to 6 percent;
the organic solvent is 2% -45%, 5% -40%, 10% -35% and 15% -30%; or 20% -25% and the like;
2 to 6 percent or 4 to 5 percent of emulsifying agent;
0.2 to 4 percent of pH regulator, 0.5 to 3.5 percent, 1 to 3 percent, 1.5 to 2.5 percent, or 1.8 to 2 percent;
0.05 to 1.8 percent of defoaming agent, 0.1 to 1.5 percent of defoaming agent, 0.5 to 1.3 percent of defoaming agent and 0.8 to 1.0 percent of defoaming agent;
the thickener is 0.2 to 7,0.5 to 6, 1 to 5, 1.5 to 4 or 2 to 3 percent;
0.5 to 7 percent of antifreeze agent, 1 to 6 percent, 2 to 5 percent or 3 to 4 percent.
According to an embodiment of the invention, the composition is prepared into a microcapsule suspension-suspension agent and comprises the following components in percentage by weight: 1-50% of compound I, 1-50% of compound II, 1-12% of high molecular capsule wall material, 1-12% of dispersing agent, 1-8% of wetting agent, 1-50% of organic solvent, 1-8% of emulsifying agent, 0.01-2% of defoaming agent, 0.1-8% of thickening agent, 0.1-5% of pH regulator, 0.1-8% of antifreeze agent and the balance of deionized water.
According to an embodiment of the invention, the composition is prepared into emulsifiable concentrates and comprises the following components in percentage by weight: 1-50% of compound I, 1-50% of compound II, 0-10% of emulsifying agent, 0-5% of antifreeze agent, 0-0.5% of stabilizing agent and the balance of organic solvent;
or 1-50% of compound I, 1-50% of compound II, 0-12% of emulsifying agent, 0-0.5% of stabilizing agent and the balance of organic solvent.
According to an embodiment of the invention, the composition is prepared into a microemulsion and comprises the following components in percentage by weight: 1 to 50 percent of compound I, 1 to 50 percent of compound II, 1 to 50 percent of organic solvent, 1 to 30 percent of emulsifier, 1 to 10 percent of antifreeze agent, 0.1 to 5 percent of stabilizer and the balance of deionized water.
According to an embodiment of the invention, the composition is formulated as a dispersible formulation comprising the following components and amounts: 1-50% of compound I, 1-50% of compound II, 1-30% of emulsifier, 1-10% of antifreeze agent, 0.1-5% of stabilizer and the balance of organic solvent.
According to an embodiment of the invention, the composition is prepared into granules and comprises the following components in percentage by weight: 0.1 to 10 percent of compound I, 0.1 to 10 percent of compound II, 0 to 5 percent of dispersing agent, 0 to 5 percent of wetting agent, 0 to 3 percent of adhesive and the balance of filler.
According to an embodiment of the present invention, the emulsifier may be at least one of the following: sodium lignin sulfonate, pesticide emulsion, phenyl phenol polyoxyethylene ether phosphate, triethanolamine salt of tristyrylphenol polyoxyethylene ether phosphate, benzyl dimethyl phenol polyoxyethylene ether, sorbitan fatty acid ester polyoxyethylene ether, sorbitan oleic acid ester (span-80), fatty alcohol polyoxyethylene ether, sodium alkyl naphthalene sulfonate, sodium isooctyl succinate sulfonate, nonylphenol polyoxyethylene ether phosphate, castor oil polyoxyethylene ether phosphate.
According to an embodiment of the present invention, the dispersant may be at least one of the following: glycerol fatty acid polyoxyethylene ether, polyoxyethylene alkylaryl ether, sodium lignin sulfonate, naphthalene sulfonate formaldehyde condensate, fatty alcohol polyoxyethylene ether sulfate, naphthalene sulfonate formaldehyde condensate sodium salt, nonylphenol polyoxyethylene ether, polyoxyethylene lanolin alcohol, alkylphenol polyoxyethylene ether formaldehyde condensate, fatty alcohol polyoxyethylene ether phosphate, polyoxyethylene sorbitan fatty acid ester, and phosphate.
According to an embodiment of the present invention, the wetting agent may be at least one selected from the group consisting of: trisiloxane polyoxyethylene ether, sodium N-lauroyl glutamate, sodium dodecyl sulfate, sodium lauroyl sarcosinate, sodium methyl naphthalene sulfonate formaldehyde condensate, castor oil polyoxyethylene ether, triphenyl ethylphenol polyoxyethylene ether, sodium dodecyl benzene sulfonate, sodium alkyl naphthalene sulfonate, sodium isooctyl succinate sulfonate, polyoxyethylene alkylaryl ether, fatty alcohol polyether glycerol fatty acid polyoxyethylene ether, and fatty alcohol polyoxyethylene ether.
According to an embodiment of the present invention, the binder may be at least one of the following: xanthan gum, starch, urea-formaldehyde resin, gelatin, acacia, carboxymethyl cellulose, carboxyethyl cellulose and polyvinyl alcohol.
According to an embodiment of the present invention, the disintegrant may be at least one of the following: sodium bicarbonate, ammonium sulfate, sodium sulfate, calcium sulfate, and magnesium chloride.
According to an embodiment of the present invention, the thickener may be at least one of the following: magnesium aluminum silicate, polyvinyl acetate, xanthan gum, gelatin, acacia, and polyvinyl alcohol.
According to an embodiment of the present invention, the antifoaming agent may be at least one of the following: silicone oil, n-octanol, silicone, butyl phosphate, isobutyl phosphate.
According to an embodiment of the invention, the antifreeze agent may be at least one of the following: propylene glycol, ethylene glycol, glycerol.
According to an embodiment of the present invention, the stabilizer may be at least one of the following: triethanolamine, epichlorohydrin, butyl glycidyl ether, triphenyl phosphite, N-soybean oil-based trimethylene diamine, and dialkyl succinic acid vinegar sulfonate.
According to an embodiment of the present invention, the filler includes a solid filler and a liquid filler, wherein the solid filler may be at least one of the following: kaolin, attapulgite, diatomite, white carbon black, bentonite, montmorillonite, calcium carbonate and talcum powder. The liquid filler can be one or more of soybean oil, castor oil and mineral oil.
According to an embodiment of the present invention, the organic solvent may be at least one of the following: ethyl acetate, acetone, isopropanol, 2-trifluoroethanol, propylene carbonate, benzene, toluene, xylene, dimethylformamide, dimethyl sulfoxide, methylene chloride, cyclohexane, cyclohexanone, N-methylpyrrolidone, and a mineral spirits (e.g., 150# mineral spirits).
The invention also provides the use of the above composition for controlling insect pests in agriculture or non-agriculture.
According to an embodiment of the invention, the pest is selected from Lepidoptera (Lepidoptera), hemiptera (Hemiptera), coleoptera (Coleoptera), thysanoptera (Thysanoptera), diptera, mites and the like.
As one embodiment, the pest is selected from the group consisting of spider mites.
The present invention also provides a method of controlling insect pests in agriculture or non-agriculture comprising applying a composition as described above to a plant in the presence of insect pests.
The composition of the invention can be provided in the form of a finished preparation or in the form of a single dose, and can be directly mixed before use, then mixed with water to prepare the required concentration, and can be applied to crops or plants in any way, such as spraying, root irrigation, smearing and the like. In particular application, the composition can also be mixed with other medicaments such as a growth regulator, a soil regulator, a herbicide, a nematicide and the like.
The present invention also provides a composition for controlling invertebrate pests comprising a biologically effective amount of a compound I, a compound II and at least one other component selected from the group consisting of a surfactant, a solid diluent and a liquid diluent, said composition optionally further comprising an effective amount of at least one other biologically active compound or agent, said compound II being selected from the group consisting of flucyclofen, KII-9396 or a combination thereof.
The present invention also provides a method for controlling an invertebrate pest comprising contacting the invertebrate pest or its environment with a biologically effective amount of a composition of the invention as described above.
The invention also provides a spray composition comprising a composition of the invention as described above and a propellant.
The present invention also provides a bait composition comprising the composition of the invention as described above; one or more food materials; optionally an insect attractant; and optionally a humectant.
The invention has the beneficial effects that:
the composition of the invention has the following advantages:
1) Has synergistic effect and can improve pest control effect; 2) The insecticidal spectrum is enlarged, multiple field insect pests are mixed, and the effect on the insect pests is stronger; 3) The two active ingredients have different action mechanisms, and the mixed use can delay the generation of drug resistance of pests; 4) The application amount is reduced, the use times are reduced, and the use cost is reduced.
Detailed Description
The technical scheme of the invention will be further described in detail below with reference to specific embodiments. It is to be understood that the following examples are illustrative only and are not to be construed as limiting the scope of the invention. All techniques implemented based on the above description of the invention are intended to be included within the scope of the invention.
Unless otherwise indicated, the starting materials and reagents used in the following examples were either commercially available or may be prepared by known methods.
The compound I employed in the following examples was prepared by the method of example 1 in reference CN 111909143A.
The% of each component in the preparations of the following examples refers to mass percent unless otherwise specified.
The invention adopts a method combining indoor bioassay and field test to perform performance test on the insecticidal effect of the composition. It should be noted that any modifications, equivalent substitutions and improvements made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
1. Preparation example:
preparation example 1: wettable powder
The materials are coarsely crushed according to the proportion, then are mixed uniformly in a mixer, and are crushed by air flow to obtain the finished product.
Preparation example 2: water dispersible granule
Uniformly mixing the effective active ingredients, various auxiliary agents and the like according to the proportion of the formula, obtaining powder after jet milling, adding a certain amount of water, mixing, extruding and granulating, and obtaining the finished product after drying and screening.
Preparation example 3: suspending agent
The effective active ingredients and various auxiliary agents are uniformly mixed according to the proportion of the formula, sheared at high speed and sanded to obtain the finished product.
Preparation example 4: emulsifiable concentrate
Mixing the raw materials in proportion to dissolve the raw materials into a uniform oil phase; and after the inspection is qualified, metering and split charging are carried out to obtain the finished product.
Preparation example 5: aqueous emulsion
According to the formula requirement, the raw materials are added into a batching kettle, uniformly mixed by a high-speed shearing machine to prepare aqueous emulsion, and after being checked to be qualified, the aqueous emulsion is metered and split-packed to obtain the finished product.
Preparation example 6: emulsifiable concentrate
Mixing the raw materials in proportion to dissolve the raw materials into a uniform oil phase; and after the inspection is qualified, metering and split charging are carried out to obtain the finished product.
Preparation example 7: granule preparation
The components are fully mixed according to the formula proportion, crushed, wetted by water, fully and uniformly stirred, granulated by a screw extrusion granulator, dried and sieved to obtain the finished product.
Compound II in the above preparation is flucyclofen or KII-9396.
2. Indoor toxicity measurement example
(1) Test pest: tetranychus urticae (Tetranychusurticae Koch).
(2) The measuring method comprises the following steps:
method for determining toxicity of pests
The toxicity measurement of the pests uses tetranychus urticae as a test material, and the toxicity measurement of the compound I, the compound II and the mixed preparation thereof is carried out.
Pesticide part 12 with reference to agricultural industry Standard NY/T1154.12-2008, pesticide indoor biological assay test criterion: the method comprises preparing test agent (including compound I and compound II) into 5 concentration gradients (according to LC of the compound to different pests) with appropriate solvent (such as acetone, methanol, N dimethylformamide, dimethyl sulfoxide, etc., and selected according to its dissolving capacity to sample) 50 Values, concentration gradients are set according to equal ratio or equal difference), and compound I and compound II for mixing are respectively mixed according to LC 50 The values are set into a series of proportions according to mass proportions, and the final mass concentration (refer to the total mass of the compound I and the compound II) is prepared according to different proportions.
Cutting double faced adhesive tape into 2cm length, attaching to one end of glass slide, selecting healthy female mites, adhering back of the mites to the double faced adhesive tape (note that mite feet, antennae and mouth parts are not adhered), placing 30 heads of each piece into a wet sponge container, covering a cover, and placing under the condition of (25+/-1) DEG C. And (3) after 2 hours of microscopic examination, dead and injured individuals are removed, and 30 pieces of the individuals are complemented. Immersing the slide in the liquid medicine, slightly shaking for 5s, taking out, sucking the excessive liquid medicine by using water absorbing paper, placing in a white porcelain tray filled with wet sponge, and covering with a plastic film with good light transmittance. Treatments without agent (containing organic solvent and emulsifier) were set as blank for each treatment for 4 replicates.
Calculating co-toxicity coefficients (CTC values) of the two medicaments in different proportions according to a grand Yunpei method, wherein the co-toxicity coefficient (CTC) of the compound medicament is more than or equal to 120 and shows synergistic effect, and the CTC is less than or equal to 80 and shows antagonistic effect; 80 < CTC < 120 shows additive effect. The co-toxicity coefficient (CTC) of the mixture is calculated according to the formula (1), the formula (2) and the formula (3):
wherein:
ati—actual measured virulence index of the mixture;
S-LC of Standard insecticide 50 Milligrams per liter (mg/L);
M-LC of the mixture 50 In milligrams per liter (mg/L)
TTI＝TI A ×P A +TI B ×P B (2)
Wherein:
TTI-the theoretical co-toxicity index of the mixture;
TI A -a medicament virulence index;
P A -the percentage of agent a in the mix, in percent (%);
TI B -B agent virulence index;
P B the percentage of the B medicament in the mixture is expressed as percentage (%).
Wherein:
ctc—co-toxicity coefficient;
ati—actual toxicity index of the mixture;
TTI-the theoretical toxicity index of the mixture.
After mixing different varieties of pesticides, three types of action are usually shown, namely additive action, synergistic action and antagonistic action, but the specific action cannot be predicted. The composition of the invention uses the compound I and the compound II as effective active ingredients, and is illustrated by using a bioassay example.
Test for measuring activity of indoor medicament of tetranychus urticae
In this test, an indoor activity measurement test of the compound against Tetranychus urticae was performed by using a mite slide dipping method to measure the activity of the insecticidal compositions of examples 1 to 2 against Tetranychus urticae.
Example 1: in order to verify the effect of different proportions of the compound I and the flucyclofen on the two-spotted spider mites, the indoor toxicity of the compound I and the flucyclofen on the two-spotted spider mites is measured, the corresponding concentrations are prepared according to the mass proportions in the table, and the indoor insecticidal test is carried out, wherein the test results are as follows:
TABLE 1 toxicity test results of Compound I and Fluomite Biether Single and its mixture on Tetranychus urticae
Active ingredient Proportioning of Regression equation LC 50 Co-toxicity coefficient Evaluation
Compound I — y＝3.8749+2.0618x 3.5131 — —
Fluomite diether — y＝5.4543+1.9871x 0.5907 — —
Compound I: fluomite diether 50：1 y＝4.5113+1.7684x 1.8896 169.4832 Synergistic effect
Compound I: fluomite diether 10：1 y＝5.1056+1.9491x 0.8827 274.5333 Synergistic effect
Compound I: fluomite diether 1：1 y＝5.8633+1.8421x 0.3399 297.5433 Synergistic effect
Compound I: fluomite diether 1：10 y＝5.9871+1.7382x 0.2704 236.3240 Synergistic effect
Compound I: fluomite diether 1：50 y＝5.7528+1.8988x 0.4014 149.5991 Synergistic effect
The results in Table 1 show that the compound I and the flucycloxaprid have obvious synergistic effect on the activity of the two-spotted spider mites when mixed in different proportions.
Example 2: in order to verify the effect of different proportions of the compound I and the KII-9396 on the tetranychus urticae, the indoor toxicity of different mass proportions of the compound I and the KII-9396 on the tetranychus urticae is measured, the corresponding concentrations are prepared according to the mass proportions in the table, and the indoor insecticidal test is carried out, wherein the test results are as follows:
TABLE 2 toxicity determination results of Compounds I and KII-9396 alone and in combination on Tetranychus urticae
Active ingredient Proportioning of Regression equation LC 50 Co-toxicity coefficient Evaluation
Compound I — y＝3.8749+2.0618x 3.5131 — —
KII-9396 — y＝5.0877+1.6033x 0.8817 — —
Compound I: KII-9396 50：1 y＝4.4661+1.6635x 2.0939 158.5060 Synergistic effect
Compound I: KII-9396 10：1 y＝4.9666+1.3831x 1.0572 261.3904 Synergistic effect
Compound I: KII-9396 1：1 y＝5.5187+1.7244x 0.5003 281.7551 Synergistic effect
Compound I: KII-9396 1：10 y＝5.5105+1.6542x 0.4914 192.5352 Synergistic effect
Compound I: KII-9396 1：50 y＝5.4310+1.8889x 0.5913 151.3338 Synergistic effect
As shown in the results of Table 2, the compounds I and KII-9396 have obvious synergism on the activity of the Tetranychus urticae.
The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiment. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A composition comprising compound I and compound II, wherein compound II is flucyclofen, KII-9396 or a combination thereof,
the structure of the compound I is shown as follows,
the KII-9396 is (RS) - [5- [ 4-chloro-2-fluoro-5- [ (2, 2-trifluoroethyl) sulfinyl ] phenoxy ] pentanyl ] trifluoromethyl sulfide (CAS: 1472050-04-6).
2. The composition according to claim 1, wherein the mass ratio of the compound I to the compound II is 80-1:1-80.
3. The composition of claim 1 or 2, further comprising at least one of deionized water, an organic solvent, an emulsifier, a dispersant, a wetting agent, a thickener, an antifoaming agent, a stabilizer, a binder, a disintegrant, an antifreeze agent, an anticaking agent, a suspending agent, a film former, a preservative, a colorant, a polymeric wall material, a pH adjuster, or a filler.
4. The composition of claim 1, wherein the composition is formulated into a variety of dosage forms, including wettable powders, water dispersible granules, suspensions, emulsions in water, suspended seed coatings, microencapsulated suspensions, microencapsulated suspension-suspensions, emulsifiable concentrates, microemulsions, dispersible solutions, or granules.
5. Use of a composition according to any one of claims 1 to 4 for controlling insect pests in agriculture or non-agriculture.
6. The use according to claim 5, wherein the pest is selected from Lepidoptera (Lepidoptera), hemiptera (Hemiptera), coleoptera (Coleoptera), thysanoptera (Thysanoptera), diptera, mites.
7. A method of controlling insect pests in agriculture or non-agriculture comprising applying a composition according to any one of claims 1 to 4 to a plant in which the insect pest is present.
8. A composition for controlling invertebrate pests, characterized in that it comprises a biologically effective amount of a compound I, a compound II and at least one further component selected from the group consisting of surfactants, solid diluents and liquid diluents, said composition optionally further comprising an effective amount of at least one further biologically active compound or agent, said compound II being selected from the group consisting of flufenbisether, KII-9396 or a combination thereof.
9. A method for controlling an invertebrate pest comprising contacting the invertebrate pest or its environment with a biologically effective amount of the composition of any one of claims 1-4.
10. A spray composition comprising the composition of any one of claims 1-4 and a propellant; or alternatively, the process may be performed,
a bait composition comprising the composition of any one of claims 1-4; one or more food materials; optionally an insect attractant; and optionally a humectant.
CN202210249245.2A 2022-03-14 2022-03-14 Composition containing flucyclofen or KII-9396 and application thereof Pending CN116784338A (en)

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