A composition containing a bisamide insecticide and its use

Abstract

The present application relates to a kind of biamide-containing insecticide composition and its application.The compound I has synergistic effect with biamide-containing insecticide, can improve pest control effect, reduce application amount, reduce use frequency, reduce use cost.

Description

[0001] This application is a divisional application of application number 202210247899.1, filed on March 14, 2022, entitled "A composition containing a diamide insecticide and its application". Technical Field

[0002] This invention belongs to the field of pesticide compound technology, specifically relating to compositions containing biologically effective amounts of compound I and diamide insecticides, and methods for using them to control pests in agronomic and non-agronomic environments. Background Technology In recent years, the occurrence of various crop pests has shown a trend of increasing severity year by year, with the affected area growing annually, causing enormous damage to crops and leading to problems such as reduced crop yields and increased agricultural production costs. To improve pest control, farmers often increase pesticide dosage or arbitrarily mix pesticides. This unscientific use of pesticides not only fails to achieve synergistic effects but also leads to pesticide waste, excessive residues, environmental pollution, and the development of pesticide resistance in pests. Therefore, there is an urgent need to develop a synergistic combination for pests that can broaden the range of target pests, reduce pesticide dosage, and delay the development of resistance.

[0003] In actual agricultural production, the long-term, continuous use of the same pesticide quickly leads to pesticide resistance in pests, resulting in reduced efficacy, increased pesticide usage, and exacerbated pesticide residues in agricultural products and damage to the ecological environment. Combining insecticides with completely different mechanisms of action is an effective way to delay the development of pesticide resistance, broaden the pesticide spectrum, extend the pesticide's lifespan, and reduce pesticide usage. However, determining how to combine the pesticides to achieve synergistic rather than antagonistic effects remains a significant challenge.

[0004] Patent document CN 111909143 A discloses compound I, which has broad-spectrum insecticidal activity, especially effective against pests of the orders Lepidoptera, Hemiptera, Coleoptera, Thysanoptera, Diptera, and mites. However, it does not disclose how to combine it with other drugs to achieve synergistic effects.

[0005] The structural formula of compound I is shown below. .

[0006] I

[0007] Diamide insecticides have become a hot topic in insecticide research in recent years. They mainly act on the ryanodine receptors of insects and have the following characteristics: (1) Novel and efficient mechanism of action, no cross-resistance with traditional pesticides: Diamide insecticides have a very prominent effect on lepidopteran pests in the field. They are more effective when used during the egg stage and early larval stages, have a long duration of action, and have a significant effect on leaf protection; (2) Safe for non-target organisms and good environmental compatibility: Diamide insecticide products are highly safe for bees, fish, natural enemies, humans, livestock, birds, etc., but pose a certain risk to crustaceans; (3) Effective on both adults and larvae: They are mainly effective against larvae through stomach poisoning, and also have contact killing effect (the stomach poisoning effect is stronger than the contact killing effect, and its contact killing effect is no less than other contact insecticides); they are mainly effective against adults through contact killing. They have extremely high activity against early larvae, high activity against older larvae, and moderate activity against adults. They have extremely high egg / larval activity.

[0008] However, both of these compounds still exhibit resistance, and their insecticidal activity needs to be improved. Summary of the Invention

[0009] To overcome the shortcomings of the prior art, the present invention provides a composition comprising compound I and a diamide insecticide, wherein the diamide insecticide is selected from at least one of the following: chlorantraniliprole, flubendiamide, chlorfenapyr, bromonifen, tetrachlorfenapyr, cyclopropamide, tetrazolium, fluoxastrobin, thiamethoxam, thiophanate-methyl, and fluchlorfenapyr diamide. The structural formula of compound I is shown below.

[0010] I

[0011] According to an embodiment of the present invention, compound I is prepared by the method of Example 1 in patent document CN 111909143 A, the entire contents of which are incorporated herein by reference.

[0012] According to an embodiment of the present invention, the mass ratio of compound I to the diamide insecticide is 80~1:1~80.

[0013] According to an embodiment of the present invention, the mass ratio of compound I to the diamide insecticide is 50 to 1:1 to 50, 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.

[0014] According to a preferred embodiment of the present invention, the mass ratio of compound I to the diamide insecticide is 10~1:1~10.

[0015] According to an embodiment of the present invention, the total mass of the compound I and the diamide insecticide in the composition is 1-80%, preferably 2-70%, or 5-65%; 10-60%, for example 1%, 5%, 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45% or 50%, based on the total weight of the composition as 100%.

[0016] According to embodiments of the present invention, the composition can be prepared as a liquid formulation or a solid formulation.

[0017] According to embodiments of the present invention, the content range of the effective active ingredient in the formulation varies depending on the type of formulation. Generally, liquid formulations contain 1% to 60% of the effective active ingredient by weight, preferably 5% to 50%; solid formulations contain 5% to 80% of the effective active ingredient by weight, preferably 10% to 70%.

[0018] According to embodiments of the present invention, the composition further includes at least one of the following: deionized water, organic solvent, emulsifier, dispersant, wetting agent, thickener, defoamer, stabilizer, binder, disintegrant, antifreeze, anticaking agent, suspending agent, film-forming agent, preservative, colorant, polymeric capsule wall material, pH adjuster, or filler.

[0019] According to embodiments of the present invention, the composition can be diluted or used directly by the user before use. Its formulation can be prepared by processing methods known to those skilled in the art, i.e., by mixing the active ingredient with one or more of the following: deionized water, organic solvents, emulsifiers, dispersants, wetting agents, thickeners, defoamers, stabilizers, binders, disintegrants, antifreeze agents, anti-caking agents, suspending agents, film-forming agents, preservatives, colorants, polymeric capsule wall materials, pH adjusters, or fillers, to prepare the composition.

[0020] According to embodiments of the present invention, the composition can be formulated into various dosage forms, preferably including wettable powders, water-dispersible granules, suspensions, water-emulsions, suspension seed coatings, microcapsule suspensions, microcapsule suspension-suspension agents, emulsifiable concentrates, microemulsions, dispersible liquids, and granules.

[0021] According to an embodiment of the present invention, when the composition is formulated into a wettable powder, it comprises the following components and contents: compound I 1%~80%, diamide insecticide 1%~80%, dispersant 0%~10%, wetting agent 0%~8%, and the balance being filler.

[0022] Preferably, the compound I in the composition is 2%~70%, 5%~65%, 10%~60%, 15%~50%, etc.; Diamide insecticides are available in concentrations of 2%–70%, 5%–65%, 10%–60%, and 15%–50%, etc. The dispersant concentration is 1%~8%, 2%~7%, 3-6%, or 4%~5%; The wetting agent is 1%~8%, 2%~7%, 3-6%, or 4%~5%.

[0023] According to an embodiment of the present invention, when the composition is formulated into water-dispersible granules, it comprises the following components and contents: compound I 1%~80%, diamide insecticide 1%~80%, dispersant 0%~10%, wetting agent 0%~16%, disintegrant 0%~20%, and the balance being filler.

[0024] Preferably, the compound I in the composition is 2%~70%, 5%~65%, 10%~60%, 15%~50%, etc.; Diamide insecticides are available in concentrations of 2%–70%, 5%–65%, 10%–60%, and 15%–50%, etc. The dispersant concentration is 1%~8%, 2%~7%, 3-6%, or 4%~5%; The wetting agent is 1%~8%, 2%~7%, 3-6% or 4%~5%; The disintegrant is 1%~18%, 2%~16%, 3-15%, 4%~12%, 5%~10%, or 6-8%.

[0025] According to an embodiment of the present invention, when the composition is made into a suspension, it comprises the following components and contents: compound I 1%~50%, diamide insecticide 1%~50%, dispersant 0%~5%, wetting agent 0%~8%, thickener 0%~0.3%, antifreeze agent 0%~5%, and the balance being deionized water.

[0026] Preferably, compound I in the composition is 2%~45%, 5%~40%, 10%~35%, 15%~30%, 20%~25%, etc.; Diamide insecticides are available in concentrations of 2%–45%, 5%–40%, 10%–35%, 15%–30%, and 20%–25%, etc. The dispersant is 1%~4% or 2%~3%; The wetting agent is 1%~8%, 2%~7%, 3-6% or 4%~5%; The thickener content is 0.1%~0.25%; Antifreeze 1%~4% or 2%~3%.

[0027] According to an embodiment of the present invention, when the composition is formulated into an aqueous emulsion, it comprises the following components and contents: compound I 1%~50%, diamide insecticide 1%~50%, organic solvent 0%~95%, emulsifier 0%~10%, antifreeze 0%~5%, defoamer 0%~0.2%, thickener 0%~0.5%, and the balance being deionized water.

[0028] Preferably, compound I in the composition is 2%~45%, 5%~40%, 10%~35%, 15%~30%, 20%~25%, etc.; Diamide insecticides are available in concentrations of 2%–45%, 5%–40%, 10%–35%, 15%–30%, and 20%–25%, etc. The organic solvents are 1%~90%, 2%~80%, 5%~70%, 10%~60%, 15%~50%, 20%~50%, 30%~40%, etc. Emulsifiers: 1%~8%, 2%~7%, 3-6%, or 4%~5%; Antifreeze 1%~4% or 2%~3%; Defoamer 0.05%~0.1%, or The thickener is 0.1%~0.4% or 0.2%~0.3%.

[0029] According to an embodiment of the present invention, when the composition is formulated into a suspension seed coating agent, it comprises the following components and contents: compound I 1%~50%, diamide insecticide 1%~50%, dispersant 1%~12%, wetting agent 1%~10%, antifreeze agent 1%~10%, anticaking agent 0.1%~10%, suspending agent 0.1%~5%, film-forming agent 1%~10%, preservative 0.1%~5%, colorant 1%~30%, pH adjuster 0.1%~5%, thickener 0.1%~8%, and the balance being deionized water.

[0030] Preferably, compound I in the composition is 2%~45%, 5%~40%, 10%~35%, 15%~30%, 20%~25%, etc.; Diamide insecticides are available in concentrations of 2%–45%, 5%–40%, 10%–35%, 15%–30%, and 20%–25%, etc. The dispersant concentration is 2%~10%, 3%~8%, 4%~7%, or 5%~6%; The wetting agent is 1%~8%, 2%~7%, 3-6% or 4%~5%; Antifreeze is 1%~8%, 2%~7%, 3-6%, or 4%~5%; Anti-caking agents are available at concentrations of 0.5%–9%, ​​1%–8%, 2%–7%, 3–6%, or 4%–5%. The suspending agent is 0.2%~4%, 0.5%~3.5%, 1%~3%, 1.5%~2.5%, or 1.8%~2%; The film-forming agent is 2%~9%, 3%~8%, 4%~7%, or 5%~6%; The preservative content is 0.2%~4%, 0.5%~3.5%, 1%~3%, 1.5%~2.5%, or 1.8%~2%; The colorant is 2%~25%, 3%~20%, 5%~15%, 8%~12%, or 9%~10%; pH adjuster: 0.1%~5%, 0.2%~4%, 0.5%~3.5%, 1%~3%, 1.5%~2.5%, or 1.8%~2%; The thickener is 0.5%~7%, 1%~6%, 2%~5%, or 3%~4%.

[0031] According to an embodiment of the present invention, when the composition is formulated into a microcapsule suspension, it comprises the following components and contents: compound I 1%~50%, diamide insecticide 1%~50%, polymeric capsule wall material 1%~30%, dispersant 2%~10%, organic solvent 1%~50%, emulsifier 1%~7%, pH adjuster 0.1%~5%, defoamer 0.01%~2%, thickener 0.1%~8%, antifreeze agent 0.1%~8%, and the balance being deionized water.

[0032] Preferably, compound I in the composition is 2%~45%, 5%~40%, 10%~35%, 15%~30%, 20%~25%, etc.; Diamide insecticides are available in concentrations of 2%–45%, 5%–40%, 10%–35%, 15%–30%, and 20%–25%, etc. Polymer capsule wall material 2~25%, 5~20%, 6~18%, or 10~15%, etc.; The dispersant concentration is 3%~8%, 4%~7%, or 5%~6%; The organic solvents are 2%~45%, 5%~40%, 10%~35%, 15%~30%; or 20%~25%, etc. The emulsifier is 2%~6% or 4%~5%; pH adjuster: 0.2-4%, 0.5%-3.5%, 1%-3%, 1.5%-2.5%, or 1.8%-2%; The defoamer concentrations are 0.05~1.8%, 0.1%~1.5%, 0.5%~1.3%, and 0.8%~1.0%. The thickener is 0.2%~7%, 0.5%~6%, 1%~5%, 1.5%~4%, or 2%~3%; The antifreeze is 0.5%~7%, 1%~6%, 2%~5%, or 3%~4%.

[0033] According to an embodiment of the present invention, when the composition is formulated into a microcapsule suspension, it comprises the following components and contents: compound I 1%~50%, diamide insecticide 1%~50%, polymeric capsule wall material 1%~12%, dispersant 1%~12%, wetting agent 1%~8%, organic solvent 1%~50%, emulsifier 1%~8%, defoamer 0.01%~2%, thickener 0.1%~8%, pH adjuster 0.1%~5%, antifreeze agent 0.1%~8%, and the balance being deionized water.

[0034] According to an embodiment of the present invention, when the composition is prepared into an emulsifiable concentrate, it comprises the following components and contents: compound I 1%~50%, diamide insecticide 1%~50%, emulsifier 0~10%, antifreeze 0%~5%, stabilizer 0%~0.5%, and the balance being organic solvent; Alternatively, the composition may be: 1%–50% compound I, 1%–50% diamide insecticide, 0–12% emulsifier, 0%–0.5% stabilizer, with the remainder being organic solvent.

[0035] According to an embodiment of the present invention, when the composition is prepared into a microemulsion, it comprises the following components and contents: compound I 1%~50%, diamide insecticide 1%~50%, organic solvent 1%~50%, emulsifier 1%~30%, antifreeze 1%~10%, stabilizer 0.1%~5%, and the balance being deionized water.

[0036] According to an embodiment of the present invention, when the composition is prepared into a dispersible liquid, it comprises the following components and contents: compound I 1%~50%, diamide insecticide 1%~50%, emulsifier 1%~30%, antifreeze 1%~10%, stabilizer 0.1%~5%, and the balance being organic solvent.

[0037] According to an embodiment of the present invention, when the composition is made into granules, it comprises the following components and contents: compound I 0.1%~10%, diamide insecticide 0.1%~10%, dispersant 0%~5%, wetting agent 0%~5%, binder 0%~3%, and the balance being filler.

[0038] According to an embodiment of the present invention, the emulsifier may be selected from at least one of the following: sodium lignosulfonate, agricultural emulsion, phenylphenol polyoxyethylene ether phosphate, tristyrylphenol polyoxyethylene ether phosphate triethanolamine salt, benzyl dimethylphenol polyoxyethylene ether, sorbitan fatty acid ester polyoxyethylene ether, sorbitan anhydride oleate (Span-80), fatty alcohol polyoxyethylene ether, sodium alkyl naphthalene sulfonate, sodium isooctanol succinate sulfonate, nonylphenol polyoxyethylene ether phosphate, and castor oil polyoxyethylene ether phosphate.

[0039] According to an embodiment of the present invention, the dispersant may be selected from at least one of the following: glycerol fatty acid polyoxyethylene ether, polyoxyethylene alkyl aryl ether, sodium lignosulfonate, naphthalene sulfonate formaldehyde condensate, fatty alcohol polyoxyethylene ether sulfate, naphthalene sulfonate formaldehyde condensate, sodium naphthalene sulfonate formaldehyde condensate, nonylphenol polyoxyethylene ether, polyoxyethylene lanolin alcohol, alkylphenol polyoxyethylene ether formaldehyde condensate, fatty alcohol polyoxyethylene ether, fatty alcohol polyoxyethylene ether phosphate, polyoxyethylene sorbitan fatty acid ester, and phosphate ester.

[0040] According to an embodiment of the present invention, the wetting agent may be selected from at least one of the following: trisiloxane polyoxyethylene ether, sodium N-lauroyl glutamate, sodium dodecyl sulfate, sodium lauroyl sarcosinate, sodium methylnaphthalene sulfonate formaldehyde condensate, castor oil polyoxyethylene ether, triphenylethylphenol polyoxyethylene ether, sodium dodecylbenzene sulfonate, sodium alkylnaphthalene sulfonate, sodium isooctanol succinate sulfonate, polyoxyethylene alkyl aryl ether, fatty alcohol polyether glycerol fatty acid polyoxyethylene ether, and fatty alcohol polyoxyethylene ether.

[0041] According to an embodiment of the present invention, the adhesive may be selected from at least one of xanthan gum, starch, urea-formaldehyde resin, gelatin, gum arabic, carboxymethyl cellulose, carboxyethyl cellulose, and polyvinyl alcohol.

[0042] According to an embodiment of the present invention, the disintegrant may be selected from at least one of sodium bicarbonate, ammonium sulfate, sodium sulfate, calcium sulfate, and magnesium chloride.

[0043] According to an embodiment of the present invention, the thickener may be selected from at least one of magnesium aluminum silicate, polyvinyl acetate, xanthan gum, gelatin, gum arabic, and polyvinyl alcohol.

[0044] According to an embodiment of the present invention, the defoamer may be selected from at least one of the following: silicone oil, n-octanol, silicone, butyl phosphate, isobutyl phosphate, etc.

[0045] According to an embodiment of the present invention, the antifreeze agent may be selected from at least one of propylene glycol, ethylene glycol, glycerol, etc.

[0046] According to an embodiment of the present invention, the stabilizer may be selected from at least one of the following: triethanolamine, epichlorohydrin, butyl glycidyl ether, triphenyl phosphite, N-soybean oil-based trimethylenediamine, dialkyl succinate acesulfonate, etc.

[0047] According to an embodiment of the present invention, the filler includes solid filler and liquid filler, wherein the solid filler may be selected from at least one of the following: kaolin, attapulgite, diatomaceous earth, silica, bentonite, montmorillonite, calcium carbonate, and talc. The liquid filler may be selected from at least one of soybean oil, castor oil, and mineral oil.

[0048] According to an embodiment of the present invention, the organic solvent may be selected from at least one of the following: ethyl acetate, acetone, isopropanol, 2,2,2-trifluoroethanol, propylene carbonate, benzene, toluene, xylene, dimethylformamide, dimethyl sulfoxide, dichloromethane, cyclohexane, cyclohexanone, N-methylpyrrolidone, and solvent oil (such as 150# solvent oil).

[0049] The present invention also provides the use of the above composition for the prevention and control of pests in agriculture and non-agriculture.

[0050] According to an embodiment of the present invention, the pests are insects of the orders Lepidoptera, Hemiptera, Coleoptera, Thysanoptera, Diptera, mites, etc.

[0051] As one implementation scheme, the pests are selected from the following: corn armyworm, cabbage cutworm, and cabbage diamondback moth.

[0052] The present invention also provides a method for controlling agricultural or non-agricultural pests, comprising applying the above composition to plants infested with pests.

[0053] The compositions of this invention can be provided as finished formulations or as single agents. They are mixed directly before use, then diluted with water to achieve the desired concentration. They can be applied to crops in any manner, such as spraying, root irrigation, or application. In specific applications, they can also be mixed with other agents such as growth regulators, soil conditioners, herbicides, and nematicides.

[0054] The present invention also provides a composition for controlling invertebrate pests, comprising a biologically effective amount of compound I, a diamide insecticide, and at least one other component selected from surfactants, solid diluents, and liquid diluents, wherein the composition optionally further contains an effective amount of at least one other biologically active compound or agent, wherein the diamide insecticide is selected from at least one of the following: chlorantraniliprole, flubendiamide, chlorfenapyr, bromonitrile cyanamide, tetrachlorantraniliprole, cyclopropamide, tetrazole acetamiprid, fluoxastrobin, thiamethoxam, thiophanate-methyl, and fluchlorfenapyr diamide.

[0055] The present invention also provides a method for controlling invertebrate pests, comprising contacting the invertebrate pest or its environment with a biologically effective amount of the composition of the present invention as described above.

[0056] The present invention also provides a spray composition comprising the composition and propellant of the present invention as described above.

[0057] The present invention also provides a bait composition comprising the composition of the present invention as described above; one or more food materials; optional insect attractant; and optional wetting agent.

[0058] The beneficial effects of this invention are: The synergistic composition of the present invention has the following advantages: 1) It has a synergistic effect, which can improve the pest control effect; 2) It broadens the insecticidal spectrum, and since pests often occur in the field in a mixed manner, it has a stronger effect on pests; 3) The two active ingredients have different mechanisms of action, and their mixed use can delay the development of pesticide resistance in pests; 4) It reduces the amount of pesticide applied, the number of applications, and the cost of use. Detailed Implementation

[0059] The present invention will be further described in detail below with reference to specific embodiments. It should be understood that the following embodiments are merely illustrative and explanatory of the present invention and should not be construed as limiting the scope of protection of the present invention. All technologies implemented based on the above content of the present invention are covered within the scope of protection intended by the present invention.

[0060] Unless otherwise specified, the experimental methods used in the following examples are conventional methods; unless otherwise specified, the reagents and materials used in the following examples are commercially available.

[0061] This invention employs a combination of indoor bioassays and field trials to test the insecticidal efficacy of the composition. It should be noted that any modifications, equivalent substitutions, and improvements made within the spirit and principles of this invention should be included within the scope of protection of this invention.

[0062] Compound I used in the following examples was prepared by the method described in Example 1 of patent document CN 111909143 A.

[0063] Unless otherwise specified, all percentages in the preparations and examples below refer to mass percentages of each component.

[0064] I. Example of formulation preparation: Preparation Example 1: Wettable Powder Compound I 1~80% Diamide insecticides: 1-80% Sodium dodecylbenzenesulfonate (wetting agent) 0~8% Sodium lignosulfonate (dispersant) 0~10% Talc (filler) 0~5% Silica (filler) 0~5% Attapulgite (fill material) replenished to 100%. The above materials are coarsely pulverized in proportion and then mixed evenly in a mixer. After being pulverized by airflow, the finished product is obtained.

[0065] Preparation Example 2: Water-dispersible granules Compound I 1~80% Diamide insecticides: 1-80% Sodium alkylnaphthalene sulfonate (wetting agent) 0~8% Sodium lignosulfonate (dispersant) 0~10% Sodium dodecyl sulfate (wetting agent) 0~8% Ammonium sulfate (disintegrant) 0~20% Kaolin (fill material) replenished to 100%. The active ingredients and various additives are mixed evenly according to the formula, and then the powder is obtained by air jet milling. A certain amount of water is added, the mixture is extruded and granulated, and then dried and sieved to obtain the finished product.

[0066] Preparation Example 3: Suspension Compound I 1~50% Diamide insecticides 1-50% Sodium methylnaphthalenesulfonate formaldehyde condensate (wetting agent) 0~8% Xanthan gum (thickener) 0~0.3% Sodium salt of naphthalenesulfonic acid formaldehyde condensate (dispersant) 0~5% Propylene glycol (antifreeze) 0~5% Replenish deionized water to 100%. The active ingredients and various additives are mixed evenly according to the formula, and then the mixture is subjected to high-speed shearing and sand milling to obtain the finished product.

[0067] Preparation Example 4: Emulsifiable Oil Compound I 1~50% Diamide insecticides 1-50% Tristyrene-phenylphenol polyoxyethylene ether phosphate triethanolamine salt (emulsifier) ​​0~7% Fatty alcohol polyvinyl ether (emulsifier) ​​0~3% Propylene glycol (antifreeze) 0~5% Triethanolamine (stabilizer) 0~0.5% Solvent oil (organic solvent) replenished to 100%. The above raw materials are mixed in proportion to dissolve them into a homogeneous oil phase; after passing inspection, they are metered and packaged to obtain the finished product.

[0068] Preparation Example 5: Water-based emulsion Compound I 1~50% Diamide insecticides 1-50% 2,2,2-Trifluoroethanol (organic solvent) 0~35% Propylene carbonate (organic solvent) 0~30% 150# Solvent Oil (Organic Solvent) 0~30% Span-80 (emulsifier) ​​0~10% Ethylene glycol (antifreeze) 0~5% Silicone oil (defoamer) 0~0.2% Polyvinyl alcohol (thickener) 0~0.5% Replenish deionized water to 100%. According to the formula requirements, the above raw materials are added to the mixing tank and mixed evenly by a high-speed shearing machine to make a water-emulsion. After passing the inspection, it is metered and packaged to become the finished product.

[0069] Preparation Example 6: Emulsifiable Oil Compound I 1~50% Diamide insecticides 1-50% Tristyrene-phenylphenol polyoxyethylene ether phosphate triethanolamine salt (emulsifier) ​​0~6% Fatty alcohol polyvinyl ether (emulsifier) ​​0~6% Triethanolamine (stabilizer) 0~0.5% Solvent oil (organic solvent) replenished to 100%. The above raw materials are mixed in proportion to dissolve them into a homogeneous oil phase; after passing inspection, they are metered and packaged to obtain the finished product.

[0070] Preparation Example 7: Granules Compound I 0.1~10% Diamide insecticides: 0.1-10% Sodium lignosulfonate (dispersant) 0~5% Sodium dodecyl sulfate (wetting agent) 0~5% Polyvinyl alcohol (adhesive) 0~3% Silica (filler) 0~5% Diatomaceous earth (filler) should be replenished to 100%.

[0071] Mix all components thoroughly according to the formula ratio, crush them, moisten them with water, stir them thoroughly again, granulate them using a screw extruder, dry them, and then sieve them to obtain the finished product.

[0072] The diamide insecticides described in the above preparation examples are selected from at least one of the following: chlorantraniliprole, flubendiamide, chlorfenapyramide, bromonitrile cyanamide, tetrachlorantraniliprole, cyclopropamide, tetrazolium amide, fluoxetine amide, thiamethoxam, thiophanate-methyl, and fluchlorfenapyr diamide.

[0073] II. Examples of Indoor Toxicity Testing (1) Tested pest: Diamondback moth ( Plutella xylostella ), corn armyworm ( Mythimna separate Walker), beet armyworm ( Spodoptera exigua ).

[0074] (2) Measurement method: Methods for determining the toxicity of pests The toxicity of pests was determined using pests such as diamondback moth, corn armyworm, and beet armyworm as test materials. The toxicity of compound I, diamide insecticides, and their mixtures was determined by leaf immersion method.

[0075] Referring to the People's Republic of China Agricultural Industry Standard NY / T 1154.14-2008 "Guidelines for Indoor Bioassay Testing of Pesticides," Part 14: Leaf Dipping Method for Insecticides, the test agents (including Compound I and diamide insecticides) were first prepared into five concentration gradients using suitable solvents (the types of solvents, such as acetone, methanol, N,N-dimethylformamide, and dimethyl sulfoxide, etc., selected according to their solubility in the sample). 50 (The concentration gradient is set according to the ratio or arithmetic progression), and the compound I and the diamide insecticide to be mixed are respectively calculated according to their LC values. 50 The values ​​are set according to a series of proportions by mass, and the final mass concentration (referring to the total mass of compound I and diamide insecticide) is prepared by different ratios.

[0076] Immerse leaf discs or leaf segments in the test solution for 10 seconds (the immersion time can be appropriately extended or shortened depending on the characteristics of the pesticide). After immersion, remove and air dry the leaf segments. Place them in a petri dish containing 1% water agar or moisturizing filter paper, and inoculate with test insects. Each replicate should contain at least 10 insects. Each treatment should be replicated at least 4 times, and a blank control should be provided for a treatment without pesticides (containing all organic solvents and emulsifiers).

[0077] According to Sun Yunpei's method, the co-toxicity coefficient (CTC) of two drugs with different ratios is calculated. A CTC ≥ 120 indicates a synergistic effect, a CTC ≤ 80 indicates an antagonistic effect, and 80 < CTC < 120 indicates an additive effect. The CTC of the mixture is calculated according to formulas (1), (2), and (3): (1) In the formula: ATI – Actual Measured Toxicity Index of Mixtures; S – LC50 of standard insecticides 50 The unit is milligrams per liter (mg / L); M – LC of the mixture 50The unit is milligrams per liter (mg / L). (2) In the formula: TTI – Theoretical Co-toxicity Index of Mixtures; TI A —A. Toxicity index of drug A; P A —The percentage content of drug A in the mixture, expressed as a percentage (%). TI B —Toxicity index of drug B; P B —Percentage content of agent B in the mixture, expressed as percentage (%).

[0078] (3) In the formula: CTC – Cotoxicity Coefficient; ATI – Actual Toxicity Index of Mixtures; TTI – Theoretical Toxicity Index of Mixtures.

[0079] When different pesticides are mixed, they typically exhibit three types of effects: additive, synergistic, and antagonistic. However, the specific type of effect cannot be predicted. The composition described in this invention uses compound I and a diamide insecticide as the active ingredients, and bioassay examples are used to illustrate this.

[0080] Indoor pesticide activity assay for diamondback moth in cabbage This experiment used the leaf-dipping method to conduct an indoor activity test of the compounds against the diamondback moth of cabbage, in order to determine the activity of the insecticidal compositions of Examples 1-4 against the diamondback moth of cabbage.

[0081] Example 1: To verify the effects of different ratios of Compound I and chlorantraniliprole on the diamondback moth of cabbage, indoor toxicity tests were conducted on different ratios of Compound I and chlorantraniliprole against the diamondback moth. The corresponding concentrations were prepared according to the mass ratios in the table, and indoor insecticidal experiments were performed. The results are as follows: Table 1. Results of toxicity assays of Compound I and chlorantraniliprole, alone and in mixtures, against diamondback moth in cabbage.

[0082] As shown in Table 1, different ratios of compound I and chlorantraniliprole in combination significantly enhanced the activity of diamondback moth on cabbage.

[0083] Example 2: To verify the effects of different ratios of Compound I and chlorfenapyr on the diamondback moth, indoor toxicity tests were conducted on Compound I and chlorfenapyr at different ratios against the diamondback moth. The corresponding concentrations were prepared according to the mass ratios in the table, and indoor insecticidal experiments were performed. The results are as follows: Table 2. Results of toxicity assays of Compound I and chlorfenapyr monotherapy and its mixtures against diamondback moth in cabbage.

[0084] As shown in Table 2, different ratios of compound I and chlorfenapyr have a significant synergistic effect on the activity of diamondback moth in cabbage.

[0085] Example 3: To verify the effects of different ratios of Compound I and bromocyanamide on the diamondback moth, indoor toxicity tests were conducted on Compound I and bromocyanamide at different ratios against the diamondback moth. The corresponding concentrations were prepared according to the mass ratios in the table, and indoor insecticidal experiments were performed. The results are as follows: Table 3. Results of toxicity assays of Compound I and bromocyanamide, alone and in mixtures, against diamondback moth.

[0086] As shown in Table 3, different ratios of compound I and bromocyanamide significantly enhanced the activity of diamondback moth on cabbage.

[0087] Example 4: To verify the effects of different ratios of Compound I and fluchlorfenapyr on the diamondback moth, indoor toxicity tests were conducted on Compound I and fluchlorfenapyr at different ratios against the diamondback moth. The corresponding concentrations were prepared according to the mass ratios in the table, and indoor insecticidal experiments were performed. The results are as follows: Table 4. Results of toxicity assays of Compound I and fluchlorfenapyr alone and in mixtures against diamondback moth in cabbage.

[0088] As shown in Table 4, the combined effects of compound I and fluchlorfenapyr at different ratios on the activity of diamondback moth in cabbage were significantly enhanced.

[0089] Indoor pesticide activity assay for corn armyworm This experiment used the leaf dipping method to conduct an indoor activity test of the compounds against corn armyworm, in order to determine the activity of the insecticidal compositions of Examples 5-7 against corn armyworm.

[0090] Example 5: To verify the effects of different ratios of Compound I and tetrachlorantraniliprole on corn armyworm, indoor toxicity tests were conducted on different ratios of Compound I and tetrachlorantraniliprole against corn armyworm. The corresponding concentrations were prepared according to the mass ratios in the table, and indoor insecticidal experiments were performed. The results are as follows: Table 5. Results of toxicity assays of Compound I and tetrachlorantraniliprole, alone and in mixtures, against corn armyworm.

[0091] As shown in Table 5, different ratios of compound I and tetrachlorantraniliprole significantly enhanced the activity of corn armyworm.

[0092] Example 6: To verify the effects of different ratios of Compound I and cyclopropamide on corn armyworm, indoor toxicity tests were conducted on different ratios of Compound I and cyclopropamide against corn armyworm. The corresponding concentrations were prepared according to the mass ratios in the table, and indoor insecticidal experiments were performed. The results are as follows: Table 6. Results of toxicity assays of Compound I and cyclopropamide, alone and in mixtures, against corn armyworm.

[0093] As shown in Table 6, different ratios of compound I and cyclopropamide significantly enhanced the activity of corn armyworm.

[0094] Example 7: To verify the effects of different ratios of Compound I and tetrazolium acetamiprid on corn armyworm, indoor toxicity tests were conducted on different ratios of Compound I and tetrazolium acetamiprid against corn armyworm. The corresponding concentrations were prepared according to the mass ratios in the table, and indoor insecticidal experiments were performed. The results are as follows: Table 7. Results of toxicity assays of Compound I and tetrazolium acetamiprid, alone and in mixtures, against corn armyworm.

[0095] As shown in Table 7, different ratios of compound I and tetrazolium amide significantly enhanced the activity of compound I against corn armyworm.

[0096] Indoor pesticide activity assay for cabbage beet armyworm This experiment used the leaf-dipping method to conduct an indoor activity test of the compound against the cabbage beet armyworm, in order to determine the activity of the insecticidal compositions of Examples 8-11 against the cabbage beet armyworm.

[0097] Example 8: To verify the effects of different ratios of Compound I and flubendiamide on the cabbage looper, indoor toxicity tests were conducted on different ratios of Compound I and flubendiamide against the cabbage looper. The corresponding concentrations were prepared according to the mass ratios in the table, and indoor insecticidal experiments were performed. The results are as follows: Table 8. Results of toxicity assays of Compound I and flubendiamide, alone and in mixtures, against the cabbage looper.

[0098] As shown in Table 8, different ratios of compound I and flubendiamide significantly enhanced the activity of compound I against cabbage looper.

[0099] Example 9: To verify the effects of different ratios of Compound I and flufenoxuron on the cabbage looper, indoor toxicity tests were conducted on different ratios of Compound I and flufenoxuron against the cabbage looper. The corresponding concentrations were prepared according to the mass ratios in the table, and indoor insecticidal experiments were performed. The results are as follows: Table 9. Results of toxicity assays of Compound I and fluoxetine alone and in mixtures against the cabbage looper.

[0100] As shown in Table 9, different ratios of compound I and fluoxetine in combination significantly enhanced the activity of the cabbage beet armyworm.

[0101] Example 10: To verify the effects of different ratios of Compound I and thiamethoxam on the cabbage looper, indoor toxicity tests were conducted on different ratios of Compound I and thiamethoxam against the cabbage looper. The corresponding concentrations were prepared according to the mass ratios in the table, and indoor insecticidal experiments were performed. The results are as follows: Table 10. Results of toxicity assays of Compound I and thiamethoxam, alone and in mixtures, against the cabbage looper.

[0102] As shown in Table 10, different ratios of compound I and thiamethoxam significantly enhanced the activity of compound I against the cabbage looper.

[0103] Example 11: To verify the effects of different ratios of Compound I and thiofenazate on the cabbage looper, indoor toxicity tests were conducted on different ratios of Compound I and thiofenazate against the cabbage looper. The corresponding concentrations were prepared according to the mass ratios in the table, and indoor insecticidal experiments were performed. The results are as follows: Table 11. Results of toxicity assays of Compound I and thiofenazate, alone and in mixtures, against the cabbage looper.

[0104] As shown in Table 11, different ratios of compound I and thiocyanate in combination significantly enhanced the activity of the cabbage beet armyworm.

[0105] III. Field Efficacy Examples To clarify the control efficacy of Compound I and diamide insecticides, both as single agents and mixtures, against diamondback moth, corn armyworm, and beet armyworm, multiple efficacy trials were conducted in different regions of China. All formulations used were prepared according to Preparation Examples 1-7. Taking the formulation in Table 12 as an example (other experimental formulations refer to the same formulation preparation examples), the specific preparation methods are as follows: Table 12 Preparation of Compound I·Bromofendiamide Suspension with Different Proportions

[0106] Field efficacy trials of pesticides on diamondback moth and beet armyworm in cabbage. Experimental method: The application method was specified in the National Standard of the People's Republic of China GB / T 17980.13-2000. The first application was carried out when there were a sufficient number of larvae (1-3 pre-third instar larvae per plant).

[0107] Survey Methods: Following the survey methods specified in the National Standard of the People's Republic of China GB / T 17980.13-2000, count the number of live larvae of different ages on at least 10 plants in each plot, surveying the entire plant. Insect population numbers were assessed before pesticide application, and the number of live insects was assessed 1-3 days and 7-14 days after treatment. The control efficacy (control effect) was calculated using the following formula:

[0108]

[0109] Field efficacy trial of corn armyworm Experimental method: The application method was specified in the National Standard of the People's Republic of China GB / T 17980.80-2004. The pesticide was applied when the larvae were in the 2nd or 3rd instar in the field.

[0110] Survey Methodology: Following the survey methods specified in the National Standard of the People's Republic of China GB / T 17980.80-2004, five sampling points were taken from each plot, with each point containing a 1m sample. 2 Investigate the number of live insects on the crop. Investigate the initial insect population before application, and then investigate again at 1, 3, and 7 days after application. The formula for calculating the control efficacy is:

[0111]

[0112] Table 13 Field efficacy tests of Compound I and chlorantraniliprole against diamondback moth in cabbage.

[0113] Note: Different letters after the data in the same column indicate that the differences are significant at the P<0.05 level according to Duncan's new multiple range test, and the same applies below.

[0114] In the table above, Example 12, 10% Compound I·chlorantraniliprole suspension (1:4), was prepared according to Preparation Example 3. Here, 10% refers to the total mass percentage of the active substances (Compound I and chlorantraniliprole), and 1:4 refers to the mass ratio of the two active ingredients, Compound I and chlorantraniliprole.

[0115] In Example 13, the 10% Compound I·chlorantraniliprole suspension (1:3) was prepared according to Preparation Example 3, where 10% refers to the total mass percentage of the active substances (Compound I and chlorantraniliprole), and 1:3 refers to the mass ratio of the two active ingredients, Compound I and chlorantraniliprole.

[0116] The 10% compound I suspension in Comparative Example 1 was also prepared according to Preparation Example 3, where 10% refers to the mass percentage of the active substance compound I.

[0117] The other embodiments and comparative examples below were also prepared in the same manner, and will not be described in detail here.

[0118] The results in the table show that, in controlling the diamondback moth in cabbage, the combination of compound I and chlorantraniliprole, compared with the single agent, at the same dosage of active ingredient (Comparative Examples 1 and 2 correspond to Examples 12-18), showed significantly higher 1-day, 3-day, and 7-day control efficacy against the diamondback moth in cabbage. The 7-day control efficacy still reached over 94.36%, indicating a longer duration of effectiveness.

[0119] Table 14 Field efficacy tests of Compound I and chlorantraniliprole against cabbage cutworm.

[0120] The results in the table show that, in controlling the cabbage looper, the combination of compound I and chlorantraniliprole, compared with the single agent, exhibited significantly higher control efficacy for cabbage looper at 1 day, 3 days, and 7 days under the same effective ingredient dosage (comparative examples 3 and 4 correspond to Examples 19-25). The 7-day control efficacy still reached over 94.23%, demonstrating a longer duration of effectiveness.

[0121] Table 15 Field efficacy test of compound I combined with tetrachlorantraniliprole against corn armyworm.

[0122] The test results show that, in controlling corn armyworm, the combination of compound I and tetrachlorantraniliprole, compared with the single agent, at the same dosage of active ingredient (comparative examples 5 and 6 corresponding to Examples 26-32), demonstrates significantly higher control efficacy of compound I and tetrachlorantraniliprole for 1, 3, and 7 days compared to the single agent. The 7-day control efficacy still reaches over 93.60%, indicating a longer residual effect.

[0123] Table 16. Field efficacy test of compound I combined with tetrachlorfenapyr against diamondback moth in cabbage.

[0124] The test results show that, in controlling the diamondback moth in cabbage, the combination of compound I and tetrachlorantraniliprole, compared with the single agent, under the same dosage of active ingredient (comparative examples 7 and 8 corresponding to Examples 33-39), demonstrates significantly higher control efficacy of compound I and tetrachlorantraniliprole for 1, 3, and 7 days compared to the single agent. The 7-day control efficacy still reaches over 93.26%, indicating a longer duration of effectiveness.

[0125] Table 17. Field efficacy test of compound I combined with flubendiamide against diamondback moth in cabbage.

[0126] The results in the table show that, in controlling the diamondback moth in cabbage, the combination of compound I and flubendiamide, compared with the single agent, exhibited significantly higher control efficacy for the diamondback moth at 1 day, 3 days, and 7 days, under the same effective ingredient dosage (comparative examples 9 and 10 correspond to Examples 40-46). The 7-day control efficacy still reached over 93.22%, demonstrating a longer residual effect.

[0127] Table 18. Field efficacy test of compound I combined with flubendiamide against corn armyworm.

[0128] The results in the table show that, in controlling corn armyworm, the combination of compound I and flubendiamide, compared with single agents, exhibited significantly higher control efficacy for corn armyworm at 1 day, 3 days, and 7 days under the same effective ingredient dosage (Comparative Examples 11 and 12 correspond to Examples 47-53). The 7-day control efficacy still reached over 92.70%, demonstrating a longer residual effect.

[0129] The embodiments of the present invention have been described above. However, the present invention is not limited to the above embodiments. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the protection scope of the present invention.

Claims

1. A composition comprising compound I and a diamide insecticide, characterized in that, The diamide insecticide is selected from one of the following: flubendiamide, chlorfenapyr, flufenoxuron, and thiamethoxam; The structure of compound I is shown below. I The mass ratio of compound I to the diamide insecticide is 50~1:1~50.

2. The composition according to claim 1, characterized in that, The mass ratio of compound I to the diamide insecticide is 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.

3. The composition according to claim 1 or 2, characterized in that, The composition further includes at least one of the following: deionized water, organic solvent, emulsifier, dispersant, wetting agent, thickener, defoamer, stabilizer, binder, disintegrant, antifreeze, anticaking agent, suspending agent, film-forming agent, preservative, colorant, polymeric capsule wall material, pH adjuster, or filler.

4. The composition according to claim 1, characterized in that, The composition is formulated into various dosage forms, including wettable powders, water-dispersible granules, suspensions, water-emulsions, suspension seed coatings, microcapsule suspensions, microcapsule-suspension mixtures, emulsifiable concentrates, microemulsions, dispersible liquids, or granules.

5. Use of the composition according to any one of claims 1-4 for the prevention and control of pests in agriculture or non-agriculture.

6. The use according to claim 5, characterized in that, The pests are selected from Lepidoptera, Hemiptera, Coleoptera, Thysanoptera, Diptera, or mites.

7. A method for controlling pests in agricultural or non-agricultural fields, characterized in that, This includes applying the composition of any one of claims 1-4 to plants infested with pests.

8. A composition for controlling invertebrate pests, characterized in that, It contains a biologically effective amount of compound I, a diamide insecticide, and at least one other component selected from surfactants, solid diluents, and liquid diluents, wherein the diamide insecticide is selected from one of the following: flubendiamide, chlorfenapyr, fluoxastrobin, and thiamethoxam; The structure of compound I is shown below. I The mass ratio of compound I to the diamide insecticide is 50~1:1~50.

9. A method for controlling invertebrate pests, characterized in that, This includes contacting invertebrate pests or their environment with a biologically effective amount of the composition according to any one of claims 1-4.

10. A spray composition comprising the composition according to any one of claims 1-4 and a propellant; or, A bait composition comprising the composition according to any one of claims 1-4; one or more food materials; optional insect attractant; and optional wetting agent.

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