A co-melting preparation process of an insecticidal composition, and the insecticidal composition and application thereof

Abstract

This invention relates to the field of sanitary insecticide technology, specifically to a eutectic preparation process for an insecticidal composition, the insecticidal composition itself, and its application. This application involves mixing a low-melting-point, volatile active ingredient A with a higher-melting-point, less volatile active ingredient B, and optionally a solid acid. The mixture is heated to a molten state, and then adsorbed using a carrier to obtain a eutectic powder. The resulting eutectic powder, along with optionally the remaining active ingredient B and other excipients, forms the insecticidal composition. Active ingredient A is selected from one or more of chlorpyrifos, tetrafluoromethrin, cypermethrin, and methoxyfenozide; active ingredient B is selected from one or more of cis-cypermethrin, lambda-cyhalothrin, and chlorfenapyr. The insecticidal composition is preferably a suspension concentrate, wettable powder, or water-dispersible granule. This invention effectively improves the suspension and stability of the active insecticide, allowing for surface residual spraying on various items, ensuring the pesticide remains on the surface. It also provides both rapid action and long-lasting effect, effectively controlling sanitary pests and stored-product pests.

Description

Technical Field

[0001] This application relates to the field of sanitary insecticide technology, specifically to a eutectic preparation process of an insecticidal composition, the insecticidal composition thereof, and its application. Background Technology

[0002] Pesticides are an essential agricultural input, playing a vital role in controlling crop diseases, pests, and weeds and ensuring my country's food security. Improving pesticide utilization and reducing pesticide usage have become critical issues urgently needing to be addressed in agriculture and the environment both in my country and globally.

[0003] Currently, the development of low-melting-point technical materials is a major challenge in the field of pesticide formulations, hindering the development of formulations such as wettable powders, water-dispersible granules, and suspension concentrates. In wettable powders, low-melting-point technical materials tend to agglomerate during heat storage or long-term storage, resulting in decreased product suspension and uncontrolled quality. Decreased technical material quality leads to uneven retention on surfaces, and particle agglomeration reduces absorption by plants and animals, ultimately lowering the product's efficacy. For suspension concentrates, technical materials with melting points above 60℃ are crucial; otherwise, they easily soften and clump together on zirconia beads during formulation processing. Furthermore, after processing, the suspension remains unstable, prone to agglomeration or precipitation. Water-dispersible granules also present processing challenges. Low-melting-point technical materials are prone to particle adhesion or denaturation during extrusion granulation and fluidized bed drying, resulting in particles that fail to disintegrate or experience a decrease in suspension.

[0004] The inconveniences in the preparation and storage of pesticide formulations and sanitary insecticides caused by the low melting point of some agricultural chemical raw materials are currently addressed by methods that alter their properties. These methods typically involve changing their structure or adding adjuvants, which are not only costly but also, in some cases, affect their performance in practical applications due to structural changes.

[0005] Based on the aforementioned problems in this field, there is an urgent need in the field of insecticides for an insecticide composition that can improve the efficacy of low-melting-point active ingredients and maintain efficacy for a long period of time. Summary of the Invention

[0006] The purpose of this invention is to overcome the problems existing in the prior art and provide a co-melting preparation process for an insecticidal composition, as well as the insecticidal composition and its application. This process can improve the suspension and stability of the active ingredient, enhance the rapid and sustained efficacy of the active ingredient, and effectively control sanitary pests and storage pests.

[0007] The effectiveness of pesticides is influenced by the physicochemical properties of their active ingredients, such as stability and solubility. Other influencing factors include formulation stability and particle size. Different solid forms exhibit varying physicochemical properties; therefore, selecting the appropriate solid form for pesticides is crucial for maximizing efficacy. Solid forms of pesticides include salts, eutectics, solvates, polymorphs, and amorphous forms. Co-melting combines two substances with different properties into a stable, non-agglomerated new crystal form, significantly improving the stability of the formulation. It also increases the internal particle resistance, allowing the formed small particles to remain stably on the target surface, thereby enhancing the product's efficacy.

[0008] This application provides a eutectic preparation process for an insecticidal composition, wherein a low-melting-point, volatile active ingredient A is mixed with a high-melting-point, non-volatile active ingredient B, and an optional solid acid are mixed, heated to a molten state, and then adsorbed using a carrier to obtain a eutectic powder. The obtained eutectic powder and the optional remaining amount of active ingredient B and other excipients are used to prepare an insecticidal composition.

[0009] The active ingredient component A is selected from one or more of chlorfluazuron, tetrafluazuron, chlorpyrifos, and methoxyfenozide, and the active ingredient component B is selected from one or more of cis-cypermethrin, lambda-cyhalothrin, and chlorfenapyr.

[0010] This application employs a co-melting and adsorption method, introducing another chemical pesticide with a higher melting point and lower volatility into a low-melting-point, easily volatile target pesticide, or further introducing a solid acid. After heating and co-melting, the pesticide is adsorbed using a carrier to create a compound formulation product. This improves the product's efficacy, stabilizes the low-melting-point pesticide, and enhances product adhesion, resulting in a significant improvement in the control of target pests while balancing stability and rapid action. The insecticidal composition obtained in this application also features low application cost, synergistic effect with compound formulation, low risk of resistance development, and long-lasting insecticidal effect. This application also solves the problem of active ingredients being easily absorbed by rough surfaces during residual spraying. Furthermore, since rough surfaces are generally alkaline, the addition of a solid acid can further adjust the pH and improve efficacy.

[0011] In the co-melting preparation process of the insecticidal composition described in this application, active ingredient A and active ingredient B are mixed at a mass ratio of 2:1 to 1:4 and heated to a molten state; the preferred mass ratio of active ingredient A to active ingredient B is 1:2 to 1:4. Active ingredient A, active ingredient B, and solid acid are mixed at a mass ratio of (1-2):(1-8):(1-8) and heated to a molten state; the preferred mass ratio of active ingredient A to active ingredient B and solid acid is (1-2):(1-2):(1-2), more preferably (1-2):1:(1-2).

[0012] In the eutectic preparation process of the insecticidal composition described in this application, the solid acid is a C12-C20 acid, preferably hexadecanoic acid or octadecanoic acid.

[0013] The co-melting preparation process of the insecticidal composition described in this application uses a carrier selected from one or more of silica, talc, fumed silica, diatomaceous earth, bentonite, corn starch, kaolin, and silicates; the carrier is preferably silica or silicates. The mass amount of the carrier is 1-4 times, preferably 2-3 times, the total amount of technical component A, technical component B, and solid acid.

[0014] This application also provides an insecticidal composition prepared using the aforementioned co-melting preparation process.

[0015] In the insecticidal composition described in this application, the other excipients are preferably a mixture of two or more selected from wetting agents, dispersants, slow-release agents, rain-resistant washout agents, disintegrants, pH adjusters, defoamers, thickeners, preservatives, antifreeze agents, binders, solvents, or fillers.

[0016] The above-mentioned wetting agent is selected from one or more of the following: alkylphenol polyoxyethylene ether formaldehyde condensate sulfate, alkylbenzene polyoxyethylene ether phosphate, phenethylphenol polyoxyethylene ether phosphate, alkyl sulfate, alkyl sulfonate, naphthalene sulfonate, polyether wetting agent (block polyether wetting agent), sodium dodecyl sulfate, pull-out powder BX, wetting and penetrating agent F, and dodecylbenzene sulfonic acid.

[0017] The above dispersants are selected from one or more of the following: polycarboxylates, lignin sulfonates, naphthalene sulfonates, phosphate dispersants, alkylphenol polyoxyethylene ether formaldehyde condensate sulfates, alkylbenzene sulfonate calcium salts, naphthalene sulfonate formaldehyde condensate sodium salts, alkylphenol polyoxyethylene ethers, fatty amine polyoxyethylene ethers, fatty acid polyoxyethylene esters, and glycerol fatty acid ester polyoxyethylene ethers.

[0018] The above-mentioned sustained-release agent is selected from one or more of the following: hydroxymethyl cellulose, modified starch, gum arabic, and polyvinyl alcohol.

[0019] The rain-resistant erosion agent is selected from: trisiloxane surfactants, preferably alkoxy-modified polytrisiloxane.

[0020] The above disintegrants are selected from one or more of the following: corn starch, ammonium sulfate, bentonite, urea, succinic acid, sodium bicarbonate, aluminum chloride, and citric acid.

[0021] The above-mentioned acid-base regulators are selected from one or more of the following: glacial acetic acid, oxalic acid, citric acid, benzoic acid, and dodecylbenzenesulfonic acid.

[0022] The above-mentioned defoamer is selected from one or more of the following: solid defoamer, silicone defoamer S29, and defoamer AF, such as silicone, polyether, fatty alcohol, silicone oil, silicone compound, C10-20 saturated fatty acid and its ester, and C8-12 fatty alcohol defoamer.

[0023] The thickeners mentioned above are selected from one or more of the following: silica, magnesium aluminum silicate, xanthan gum, gelatin, and gum arabic.

[0024] The preservatives mentioned above are selected from one or more of the following: Kathon, MIT, potassium sorbate, sodium benzoate, sodium diacetate, sodium dehydroacetate, bromonidol, and isothiazolinone.

[0025] The antifreeze agent mentioned above is selected from one or more of the following: ethylene glycol, diethylene glycol, glycerol, propylene glycol, glycerin, and urea.

[0026] The above-mentioned binder is selected from one or more of the following: dextrin, methylcellulose, polyvinylpyrrolidone, sodium alginate, and calcium lignosulfonate.

[0027] The solvents mentioned above are selected from one or more of mineral oil, solvent oil, water, etc.

[0028] The fillers mentioned above are selected from one or more of the following: kaolin, clay, diatomaceous earth, bentonite, silica, talc, attapulgite, starch, and light calcium carbonate.

[0029] The insecticidal composition described in this application comprises 0.5-10% by mass of technical component A and 1-40% by mass of technical component B; preferably, it comprises 1-5% by mass of technical component A and 5-30% by mass of technical component B; more preferably, it comprises 1.5-3% by mass of technical component A and 10-20% by mass of technical component B.

[0030] The insecticidal composition described in this application is preferably a wettable powder, suspension concentrate, water-dispersible tablet, or water-dispersible granule.

[0031] The insecticidal composition described in this application is preferably a wettable powder. The other excipients include 1-6% by mass of a wetting agent, 2-8% by mass of a dispersant, 0.1-2% by mass of an defoamer, 1-20% by mass of an acid-base regulator, and the balance being filler. The wetting agent in the wettable powder includes, but is not limited to, alkyl sulfonates; the dispersant includes, but is not limited to, lignin sulfonates, naphthalene sulfonates, and polycarboxylates; the defoamer includes, but is not limited to, organosilicon, polyether, and fatty alcohols, such as organosilicon defoamer S29; the acid-base regulator includes, but is not limited to, citric acid and benzoic acid; and the filler includes, but is not limited to, diatomaceous earth, bentonite, kaolin, talc, and corn starch.

[0032] The preparation method of the wettable powder described in this application is as follows: the eutectic powder is mixed evenly with the optional balance of the original drug component B, wetting agent, dispersant, defoamer, acid-base regulator and filler according to the formula ratio, and then subjected to air jet milling. After milling, the mixture is mixed again to obtain the product.

[0033] The insecticidal composition described in this application can be a suspension concentrate. The other excipients include 0.5-2% by mass of a wetting agent, 2-8% by mass of a dispersant, 0.1-2% by mass of an antifoaming agent, 1-20% by mass of an antifreeze agent, 0.1-3% by mass of a thickener, 0.1-1% by mass of a preservative, and the balance being a solvent. The wetting agent and dispersant in the suspension concentrate include, but are not limited to, phosphate esters and block polyether surfactants. The antifoaming agent is selected from one or more of silicone oils, silicone compounds, C10-20 saturated fatty acids and their esters, and C8-12 fatty alcohols. The antifreeze agent is selected from one or more of ethylene glycol, propylene glycol, glycerin, and urea. The thickener is selected from one or more of xanthan gum, gelatin, and gum arabic. The preservative is selected from one or more of potassium sorbate, sodium benzoate, sodium diacetate, sodium dehydroacetate, Kathon, and bromonitol. The solvent is selected from one or more of mineral oil, solvent oil, water, etc.

[0034] The preparation method of the suspension agent described in this application is as follows: the eutectic powder is mixed evenly with the optional balance of the original drug component B, wetting agent, dispersant, preservative, defoamer, antifreeze, thickener and solvent according to the formula ratio, and wet milled until the particle size D90 is between 3-10μm to obtain the product.

[0035] The insecticidal composition described in this application can be a water-dispersible granule, and the other excipients include a wetting agent with a mass fraction of 1-6%, a dispersant with a mass fraction of 2-8%, a disintegrant with a mass fraction of 2-8%, an antifoaming agent with a mass fraction of 0.1-2%, an acid-base regulator with a mass fraction of 1-20%, a binder with a mass fraction of 2-8%, and the balance being filler.

[0036] The water-dispersible granules contain, but are not limited to, alkyl sulfonates as wetting agents, lignin sulfonates, naphthalene sulfonates, polycarboxylate salts, etc. as dispersants, and organosilicon, polyether, fatty alcohols, etc. as defoamers. The disintegrants include, but are not limited to, corn starch disintegrants and ammonium sulfate. The acid-base regulators include, but are not limited to, citric acid and benzoic acid. The binder is selected from one or more of dextrin, methylcellulose, etc., and the fillers include, but are not limited to, diatomaceous earth, bentonite, kaolin, talc, corn starch, etc.

[0037] The method for preparing the water-dispersible granules described in this application is as follows: the eutectic powder is mixed evenly with the optional balance of the original drug component B, wetting agent, dispersant, defoamer, disintegrant, acid-base regulator, binder, and filler according to the formula ratio, and then subjected to air jet milling. After milling, the mixture is mixed evenly again, and an appropriate amount of water is sprayed in for extrusion granulation. After granulation, the mixture is dried using a fluidized bed dryer to obtain the product.

[0038] This application also provides the use of the insecticidal composition, characterized in that it is used to control sanitary pests or storage pests. Preferably, it is used to control mosquitoes, horseflies, midges, black flies, sandflies, flies, cockroaches, cockroaches, fleas, lice, and bedbugs.

[0039] The insecticidal composition described in this application is used to control pests by residual spraying. After diluting the insecticidal composition with water by 100 to 500 times, preferably 200 to 300 times, it is sprayed on the surfaces of objects such as walls, doors, windows, ceilings, and furniture, so that the sanitary insecticide remains on the surface of the above objects, thereby achieving the effect of knocking down and killing sanitary pests.

[0040] The dosage of the insecticidal composition described in this application is 100-200 mg / m³, preferably 150 mg / m³. 2 .

[0041] Compared with the prior art, the beneficial effects of the present invention are as follows:

[0042] (1) The product described in this invention has better long-lasting retention activity and better rapid knockdown activity, thus improving the speed and duration of efficacy. The insecticidal composition obtained in this application also has the technical advantages of low cost, synergistic effect when combined with other ingredients, and low risk of developing resistance.

[0043] (2) The present invention achieves improved formulation stability and further enhances the retention effect of low-melting-point volatile active ingredients by using a co-melting process of low-melting-point non-volatile active ingredients.

[0044] (3) The present invention further improves the stability of the active ingredients on the alkaline rough surface by using low melting point volatile active ingredients, high melting point non-volatile active ingredients, and solid acid ternary eutectic process, making the active ingredients less likely to be absorbed and improving the retention effect.

[0045] (4) This invention adds a new formulation preparation method to the domestic sanitary insecticide field. It has significant efficacy and can be widely promoted and applied. Detailed Implementation

[0046] The present invention will be further described below with reference to specific embodiments, but the invention is not limited to these specific embodiments. Those skilled in the art should recognize that the present invention covers all alternatives, improvements, and equivalents that may be included within the scope of the claims.

[0047] 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.

[0048] (I) Preparation Examples

[0049] Example 1:

[0050] 1.6g of cypermethrin and 0.8g of cis-cypermethrin were mixed and heated to a molten state. After stirring evenly, 10g of silica was used to adsorb the mixture to obtain a eutectic powder. Then, 12.6g of cis-cypermethrin, 4g of alkyl sulfonate wetting agent, 6g of naphthalene sulfonate dispersant, 3g of lignin sulfonate dispersant, 1.5g of benzoic acid acid regulator, 1g of organosilicon defoamer S29, and kaolin were added to make up to 100%. After mixing, the mixture was air-jet milled to obtain 15% cypermethrin·cis-cypermethrin wettable powder WP.

[0051] Example 2:

[0052] 1.6g of cypermethrin and 3.2g of cis-cypermethrin were mixed and heated to a molten state. After stirring evenly, 10g of silica was used to adsorb the mixture to obtain a eutectic powder. Then, 10.2g of cis-cypermethrin, 4g of alkyl sulfonate wetting agent, 6g of naphthalene sulfonate dispersant, 3g of lignin sulfonate dispersant, 1.5g of benzoic acid acid regulator, 1g of organosilicon defoamer S29, and kaolin were added to make up to 100%. After mixing, air jet milling was performed to obtain 15% cypermethrin·cis-cypermethrin wettable powder WP.

[0053] Example 3:

[0054] 1.6g of cypermethrin and 6.4g of cis-cypermethrin were mixed and heated to a molten state. After stirring evenly, 10g of silica was used to adsorb the mixture to obtain a eutectic powder. Then, 7.0g of cis-cypermethrin, 4g of alkyl sulfonate wetting agent, 6g of naphthalene sulfonate dispersant, 3g of lignin sulfonate dispersant, 1.5g of benzoic acid acid regulator, 1g of organosilicon defoamer S29, and kaolin were added to make up to 100%. After mixing, the mixture was air-jet milled to obtain 15% cypermethrin·cis-cypermethrin wettable powder WP.

[0055] Example 4:

[0056] 1.6g of cypermethrin, 1.6g of cis-cypermethrin, and 1.6g of hexadecanoic acid were mixed and heated to a molten state. After stirring evenly, 10g of silica was used to adsorb the mixture to obtain a eutectic powder. Then, 11.8g of cis-cypermethrin, 4g of alkyl sulfonate wetting agent, 6g of naphthalene sulfonate dispersant, 3g of lignin sulfonate dispersant, 1.5g of benzoic acid (a pH adjuster), 1g of organosilicon defoamer S29, and kaolin were added to make up to 100%. After mixing, the mixture was air-jet milled to obtain 15% cypermethrin·cis-cypermethrin wettable powder WP.

[0057] Example 5:

[0058] 1.6g of cypermethrin, 1.6g of cis-cypermethrin, and 3.2g of hexadecanoic acid were mixed and heated to a molten state. After stirring evenly, 10g of silica was used to adsorb the mixture to obtain a eutectic powder. Then, 11.8g of cis-cypermethrin, 4g of alkyl sulfonate wetting agent, 6g of naphthalene sulfonate dispersant, 3g of lignin sulfonate dispersant, 1.5g of benzoic acid (a pH adjuster), 1g of organosilicon defoamer S29, and kaolin were added to make up to 100%. After mixing, air jet milling was performed to obtain 15% cypermethrin·cis-cypermethrin wettable powder WP.

[0059] Example 6:

[0060] 1.6g of cypermethrin, 0.8g of cis-cypermethrin, and 1.6g of hexadecanoic acid were mixed and heated to a molten state. After stirring evenly, 10g of silica was used to adsorb the mixture to obtain a eutectic powder. Then, 12.6g of cis-cypermethrin, 4g of alkyl sulfonate wetting agent, 6g of naphthalene sulfonate dispersant, 3g of lignin sulfonate dispersant, 1.5g of benzoic acid (a pH adjuster), 1g of organosilicon defoamer S29, and kaolin were added to make up to 100%. After mixing, the mixture was air-jet milled to obtain 15% cypermethrin·cis-cypermethrin wettable powder WP.

[0061] Example 7:

[0062] 1g of chlorpyrifos, 1g of lambda-cyhalothrin, and 1g of stearic acid were mixed and heated to a molten state. After stirring evenly, 10g of silica was used for adsorption. Then, 8g of lambda-cyhalothrin, 4g of alkyl sulfonate wetting agent, 6g of polycarboxylate dispersant, 8g of corn starch disintegrant, 1g of organosilicon defoamer S29, 6g of dextrin, and ammonium sulfate were added to make up to 100%. 10% chlorpyrifos·lambda-cyhalothrin WDG was prepared according to the water-dispersible granule processing method.

[0063] Example 8:

[0064] 2g of chlorfenapyr, 2g of chlorfenapyr, and 3g of hexadecanoic acid were mixed and heated to a molten state. After stirring evenly, 10g of silica was used for adsorption. Then, 16g of chlorfenapyr, 0.5g of polyether wetting agent, 4.5g of phosphate dispersant, 0.1g of silicone defoamer S29, 5g of ethylene glycol, 0.25g of xanthan gum, 0.1g of Kathon, and water were added to make up to 100%. 20% chlorfenapyr·chlorfenapyr SC was prepared according to the suspension processing method.

[0065] Example 9:

[0066] 1.5g of tetrafluoromethrin, 2.0g of lambda-cyhalothrin, and 1g of stearic acid were mixed and heated to a molten state. After stirring evenly, 8g of silica was used for adsorption. Then, 21.5g of lambda-cyhalothrin, 6g of alkyl sulfonate wetting agent, 6g of naphthalene sulfonate dispersant, 3g of lignin sulfonate dispersant, 0.3g of citric acid, 1g of organosilicon defoamer S29, and kaolin were added to make up to 100%. 25% tetrafluoromethrin·lambda-cyhalothrin WP was prepared according to the wettable powder processing method.

[0067] Example 10:

[0068] 10g of chlorpyrifos, 5g of cis-cypermethrin, and 10g of stearic acid were mixed and heated to a molten state. After stirring evenly, 12g of silica was used for adsorption. Then, 35g of cis-cypermethrin, 8g of alkyl sulfonate wetting agent, 6g of naphthalene sulfonate dispersant, 3g of lignin sulfonate dispersant, 0.3g of citric acid, 1g of organosilicon defoamer S29, and kaolin were added to make up to 100%. 50% chlorpyrifos·cis-cypermethrin WP was prepared according to the water-dispersible granule processing method.

[0069] Example 11:

[0070] 0.5g of methoxybenzylflufenicol, 0.5g of chlorfenapyr, and 0.5g of stearic acid were mixed and heated to a molten state. After stirring evenly, 10g of silica was used for adsorption. Then, 9g of chlorfenapyr, 0.5g of polyether wetting agent, 2.5g of block polyether dispersant, 0.1g of silicone defoamer S29, 5g of ethylene glycol, 0.25g of xanthan gum, 0.1g of Kathon, and water were added to make up to 100%. 10% methoxybenzylflufenicol·chlorfenapyr SC was prepared according to the suspension processing method.

[0071] Example 12:

[0072] 1.5g of chlorfluazuron and 3.0g of lambda-cyhalothrin were mixed and heated to a molten state. After stirring evenly, 10g of silica was used to adsorb the mixture to obtain a eutectic powder. Then, 15.5g of lambda-cyhalothrin, 6g of alkyl sulfonate wetting agent, 6g of naphthalene sulfonate dispersant, 3g of lignin sulfonate dispersant, 0.3g of citric acid, 1g of organosilicon defoamer S29, and kaolin were added to make up to 100%. After mixing, the mixture was air-jet pulverized to obtain 20% chlorfluazuron·lambda-cyhalothrin wettable powder WP.

[0073] Example 13:

[0074] 1.5g of chlorpyrifos, 1.5g of lambda-cyhalothrin, and 1.5g of hexadecanoic acid were mixed and heated to a molten state. After stirring evenly, 10g of silica was used to adsorb the mixture to obtain a eutectic powder. Then, 17g of lambda-cyhalothrin, 6g of alkyl sulfonate wetting agent, 6g of naphthalene sulfonate dispersant, 3g of lignin sulfonate dispersant, 0.3g of citric acid, 1g of organosilicon defoamer S29, and kaolin were added to make up to 100%. After mixing, the mixture was air-jet milled to obtain 20% chlorpyrifos·lambda-cyhalothrin wettable powder WP.

[0075] Example 14:

[0076] 1.5g of chlorfenapyr and 3.0g of chlorfenapyr were mixed and heated to a molten state. After stirring evenly, 10g of silica was used to adsorb the mixture to obtain a eutectic powder. Then, 15.5g of chlorfenapyr, 6g of alkyl sulfonate wetting agent, 6g of naphthalene sulfonate dispersant, 3g of lignin sulfonate dispersant, 0.3g of citric acid, 1g of organosilicon defoamer S29, and kaolin were added to make up to 100%. After mixing, the mixture was air-jet milled to obtain 20% chlorfenapyr·chlorfenapyr wettable powder WP.

[0077] Example 15:

[0078] 1.5g of chlorfenapyr, 1.5g of chlorfenapyr, and 1.5g of hexadecanoic acid were mixed and heated to a molten state. After stirring evenly, 10g of silica was used to adsorb the mixture to obtain a eutectic powder. Then, 17g of chlorfenapyr, 6g of alkyl sulfonate wetting agent, 6g of naphthalene sulfonate dispersant, 3g of lignin sulfonate dispersant, 0.3g of citric acid, 1g of organosilicon defoamer S29, and kaolin were added to make up to 100%. After mixing, the mixture was air-jet milled to obtain 20% chlorfenapyr·chlorfenapyr wettable powder WP.

[0079] Example 16:

[0080] 1.5g of tetrafluoromethrin and 3.0g of cis-cypermethrin were mixed and heated to a molten state. After stirring evenly, 10g of silica was used to adsorb the mixture to obtain a eutectic powder. Then, 10.5g of cis-cypermethrin, 6g of alkyl sulfonate wetting agent, 6g of naphthalene sulfonate dispersant, 3g of lignin sulfonate dispersant, 0.3g of citric acid, 1g of organosilicon defoamer S29, and kaolin were added to make up to 100%. After mixing, the mixture was air-jet milled to obtain 15% tetrafluoromethrin·cis-cypermethrin wettable powder WP.

[0081] Example 17:

[0082] 1.5g of tetrafluoromethrin, 1.5g of cis-cypermethrin, and 1.5g of stearic acid were mixed and heated to a molten state. After stirring evenly, 10g of silica was used to adsorb the mixture to obtain a eutectic powder. Then, 12g of cis-cypermethrin, 6g of alkyl sulfonate wetting agent, 6g of naphthalene sulfonate dispersant, 3g of lignin sulfonate dispersant, 0.3g of citric acid, 1g of organosilicon defoamer S29, and kaolin were added to make up to 100%. After mixing, the mixture was air-jet milled to obtain 15% tetrafluoromethrin·cis-cypermethrin wettable powder WP.

[0083] Example 18:

[0084] 3.0g of chlorpyrifos and 6.0g of cis-cypermethrin were mixed and heated to a molten state. After stirring evenly, 10g of silica was used to adsorb the mixture to obtain a eutectic powder. Then, 11g of cis-cypermethrin, 6g of alkyl sulfonate wetting agent, 6g of naphthalene sulfonate dispersant, 3g of lignin sulfonate dispersant, 0.3g of citric acid, 1g of organosilicon defoamer S29, and kaolin were added to make up to 100%. After mixing, the mixture was air-jet milled to obtain 20% chlorpyrifos·cis-cypermethrin wettable powder WP.

[0085] Example 19:

[0086] 3.0g of chlorpyrifos, 3.0g of cis-cypermethrin, and 15g of hexadecanoic acid were mixed and heated to a molten state. After stirring evenly, 10g of silica was used to adsorb the mixture to obtain a eutectic powder. Then, 14g of cis-cypermethrin, 6g of alkyl sulfonate wetting agent, 6g of naphthalene sulfonate dispersant, 3g of lignin sulfonate dispersant, 0.3g of citric acid, 1g of organosilicon defoamer S29, and kaolin were added to make up to 100%. After mixing, the mixture was air-jet milled to obtain 20% chlorpyrifos·cis-cypermethrin wettable powder WP.

[0087] Example 20:

[0088] 1.5g of methoxybenzyl fluoride and 3.0g of cis-cypermethrin were mixed and heated to a molten state. After stirring evenly, 10g of silica was used to adsorb the mixture to obtain a eutectic powder. Then, 10.5g of cis-cypermethrin, 6g of alkyl sulfonate wetting agent, 6g of naphthalene sulfonate dispersant, 3g of lignin sulfonate dispersant, 0.3g of citric acid, 1g of organosilicon defoamer S29, and kaolin were added to make up to 100%. After mixing, air jet milling was performed to obtain 15% methoxybenzyl fluoride·cis-cypermethrin wettable powder WP.

[0089] Example 21:

[0090] 1.5g of methoxybenzyl fluoride, 1.5g of cis-cypermethrin, and 1.5g of stearic acid were mixed and heated to a molten state. After stirring evenly, 10g of silica was used to adsorb the mixture to obtain a eutectic powder. Then, 12g of cis-cypermethrin, 6g of alkyl sulfonate wetting agent, 6g of naphthalene sulfonate dispersant, 3g of lignin sulfonate dispersant, 0.3g of citric acid, 1g of organosilicon defoamer S29, and kaolin were added to make up to 100%. After mixing, air jet milling was performed to obtain 15% methoxybenzyl fluoride·cis-cypermethrin wettable powder WP.

[0091] Comparative Example 1: The mixture was prepared according to Example 1, without melt adsorption, and then directly mixed and pulverized by airflow to obtain the finished product of Comparative Example 1.

[0092] Comparative Example 2: The mixture was prepared according to Example 4, without melt adsorption, and then directly mixed and pulverized by airflow to obtain the finished product of Comparative Example 2.

[0093] Comparative Example 3: The mixture was prepared according to Example 12, without melt adsorption, and then directly mixed and pulverized by airflow to obtain the finished product of Comparative Example 3.

[0094] Comparative Example 4: The mixture was prepared according to Example 14, without melt adsorption, and then directly mixed and pulverized by airflow to obtain the finished product of Comparative Example 4.

[0095] Comparative Example 5: The mixture was prepared according to Example 16, without melt adsorption, and then directly mixed and pulverized by airflow to obtain the finished product of Comparative Example 5.

[0096] Comparative Example 6: The mixture was prepared according to Example 18, without melt adsorption, and then directly mixed and pulverized by airflow to obtain the finished product of Comparative Example 6.

[0097] Comparative Example 7: The mixture was prepared according to Example 20, without melt adsorption, and directly mixed and then subjected to air jet pulverization to obtain the finished product of Comparative Example 7.

[0098] (II) Detection Examples

[0099] GB / T 1600-2001 Method for Determination of Moisture Content in Pesticides

[0100] GB / T 1601-1993 Method for Determination of pH Value of Pesticides

[0101] GB / T5451-2001 Test Method for Wetness of Pesticide Wettable Powders

[0102] GB / T6682-2008 Specifications and Test Methods for Water Used in Analytical Laboratories

[0103] GB / T14825-2006 Method for Determination of Pesticide Suspension Rate

[0104] GB / T16150-1995 Method for Determination of Fineness of Pesticide Powders and Wettable Powders

[0105] GB / T19136-2003 Method for Determination of Thermal Storage Stability of Pesticides

[0106] GB / T28137-2011 Determination of persistent foaming properties of pesticides

[0107] The initial test results of formulation examples 1-26 and control examples 1-7 according to the above method are shown in Table 1 below:

[0108] Table 1 Initial test results of various product indicators

[0109]

[0110] The test results of formulation examples 1-21 and control examples 1-7 after 14 days of heat storage are shown in Table 2 below:

[0111] Table 2. Test results of various product indicators after 14 days of heat storage.

[0112]

[0113]

[0114] The above results show that the insecticidal composition prepared using the eutectic process of this application has significantly better suspension rate and stability than the comparative example.

[0115] (III) Examples of Biological Testing

[0116] Target species: Culex pipiens pallens and houseflies;

[0117] Test method: Residual spraying test, according to GB / T 13917.1-2009 Indoor efficacy test and evaluation of pesticide registration sanitary insecticides Part 1: Residual spraying test in sprays, the knockdown time KT50 and mortality rate were determined 30 days after coating the absorbent surface.

[0118] Experimental treatment: Formulations 1-11 and Comparative Examples 1-2 were diluted 200 times with water to prepare a spray solution. The solution was then applied to lime boards at a dosage of 150 mg / m². The knockdown time (KT) was measured 30 days after application. 50 and mortality rate.

[0119] The results of the assays for Culex pipiens pallens and houseflies are shown in Table 3 below.

[0120] Table 3. Results of the product's 30-day efficacy test against Culex pipiens pallens and houseflies:

[0121]

[0122]

[0123] The above results show that the formulations of Examples 1-21 of this invention are significantly more effective than those of Comparative Examples 1-7 in controlling Culex pipiens pallens and houseflies. The ratio of active ingredient A to active ingredient B (cypermethrin and cis-cypermethrin) in a ratio of 2:1 to 1:4 shows a significant improvement in efficacy, especially at a ratio of 1:2 where the best effect is observed. Further co-melting with the solid acid further enhances the efficacy. When active ingredients A and B are other than those listed above, the resulting composition also exhibits similar effects.

[0124] The above embodiments are merely exemplary implementations used to illustrate the present invention, and the present invention is not limited thereto. Obviously, those skilled in the art can make various modifications and variations to this application without departing from the scope and spirit of the present invention. If such modifications and variations fall within the scope of the claims of this application and their equivalents, then the intent of this application also includes such modifications and variations.

[0125] In the description of this specification, the terms "one specific embodiment," "some embodiments," "example," "specific example," etc., refer to a specific feature, structure, material, or characteristic described in connection with that embodiment or example, which is included in at least one embodiment or example of this application. In this specification, the illustrative expressions of the above terms do not necessarily refer to the same embodiment or example. Furthermore, the specific features, structures, materials, or characteristics described may be combined in a suitable manner in any one or more embodiments or examples. Moreover, without contradiction, those skilled in the art can combine and integrate the different embodiments or examples described in this specification, as well as the features of different embodiments or examples.

Claims

1. A eutectic preparation process for an insecticidal composition, characterized in that, A low-melting-point, volatile active ingredient A is mixed with a high-melting-point, non-volatile active ingredient B and an optional solid acid. The mixture is heated to a molten state and then adsorbed using a carrier to obtain a eutectic powder. The resulting eutectic powder, along with the optional remaining amount of active ingredient B and other excipients, is used to prepare an insecticidal composition. The active ingredient A is selected from one or more of chlorfluazuron, tetrafluazuron, cypermethrin, and methoxyfenozide, and the active ingredient B is selected from one or more of cis-cypermethrin, lambda-cyhalothrin, and chlorfenapyr. The active pharmaceutical ingredient A and the active pharmaceutical ingredient B are mixed at a mass ratio of 2:1 to 1:4 and heated to a molten state. or The active ingredient A and active ingredient B, along with the solid acid, are mixed in a mass ratio of (1-2):(1-8):(1-8) and heated to a molten state.

2. The eutectic preparation process of the insecticidal composition according to claim 1, characterized in that, The active ingredient A and active ingredient B are mixed in a mass ratio of 1:2 to 1:4 and heated to a molten state; or active ingredient A, active ingredient B, and solid acid are mixed in a mass ratio of (1-2):(1-2):(1-2) and heated to a molten state.

3. The eutectic preparation process of the insecticidal composition according to claim 1, characterized in that, The active ingredient A and active ingredient B, along with the solid acid, are mixed in a mass ratio of (1-2):1:(1-2) and heated to a molten state.

4. The co-melting preparation process of the insecticidal composition according to any one of claims 1-3, characterized in that, The solid acid is a C12-C20 acid.

5. The eutectic preparation process of the insecticidal composition according to claim 4, characterized in that, The solid acid is hexadecanoic acid or octadecanoic acid.

6. The co-melting preparation process of the insecticidal composition according to any one of claims 1-3, characterized in that, The carrier is selected from one or more of the following: silica, talc, fumed silica, diatomaceous earth, bentonite, corn starch, kaolin, and silicates.

7. The eutectic preparation process of the insecticidal composition according to claim 6, characterized in that, The carrier is silica or silicate.

8. The eutectic preparation process of the insecticidal composition according to claim 6, characterized in that, The mass of the carrier is 1-4 times the total mass of drug component A, drug component B, and solid acid.

9. The eutectic preparation process of the insecticidal composition according to claim 8, characterized in that, The mass of the carrier is 2-3 times the total mass of drug component A, drug component B, and solid acid.

10. An insecticidal composition prepared by the eutectic process according to any one of claims 1-9.

11. The insecticidal composition according to claim 10, characterized in that, The insecticidal composition is a wettable powder, suspension concentrate, water-dispersible tablet, or water-dispersible granule.

12. The insecticidal composition according to claim 10, characterized in that, The insecticidal composition comprises 0.5-10% by mass of technical component A and 1-40% by mass of technical component B.

13. The insecticidal composition according to claim 12, characterized in that, The insecticidal composition comprises 1-5% by mass of technical component A and 5-30% by mass of technical component B.

14. The insecticidal composition according to claim 13, characterized in that, The insecticidal composition comprises 1.5-3% by mass of technical component A and 10-20% by mass of technical component B.

15. The insecticidal composition according to any one of claims 12-14, characterized in that, The insecticidal composition is a wettable powder, and the other excipients include a wetting agent with a mass fraction of 1-6%, a dispersant with a mass fraction of 2-8%, an antifoaming agent with a mass fraction of 0.1-2%, an acid-base regulator with a mass fraction of 1-20%, and the balance being filler.

16. The insecticidal composition according to claim 15, characterized in that, The wetting agent is selected from alkyl sulfonates, and the dispersant is selected from naphthalene sulfonates and lignin sulfonates.

17. The use of the insecticidal composition according to any one of claims 10-16, characterized in that, Used for the prevention and control of sanitary pests or storage pests.

18. The use of the insecticidal composition according to claim 17, characterized in that, Used to control mosquitoes, horseflies, midges, gnats, sandflies, flies, cockroaches, cockroaches, fleas, lice, and bedbugs.

19. The use according to claim 17 or 18, characterized in that, The insecticidal composition is used to control pests by residual spraying.

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