Pesticide composition containing thiocyclam as well as preparation method and application of pesticide composition
By rationally mixing isozonil with insecticidal rings, the problems of pest resistance and increased pesticide usage have been solved, resulting in extended pesticide lifespan and improved control efficacy, especially a significant synergistic effect in pest control.
Patent Information
- Application Number
- CN202511053256.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2025-07-29
- Publication Date
- 2025-11-11
AI Technical Summary
Existing pesticide compounds are prone to causing pest resistance after long-term use, resulting in reduced control efficacy. Furthermore, using them alone increases pesticide usage and environmental pollution.
By rationally mixing isotoxam with insecticidal rings to form pesticide compositions, and optimizing their weight ratios and formulations, including water-dispersible granules, wettable powders, and dry suspensions, the service life of isotoxam can be extended and the insecticidal effect enhanced through rational mixing.
It effectively extends the lifespan of isozonil, reduces pesticide usage, and significantly improves the control effect on pests, especially on pests such as rice planthoppers, whiteflies, thrips, and aphids.
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Abstract
Description
Technical Field
[0001] This invention relates to the field of pesticide technology, and in particular to a pesticide composition containing an insecticidal ring, its preparation method, and its application. Background Technology
[0002] Currently, crop pest control primarily relies on chemical pesticides, supplemented by microbial pesticides. Developing a new pesticide compound is difficult, time-consuming, and costly. When a new pesticide compound is introduced into use, long-term use as a single agent can easily lead to resistance, reduced efficacy, and a short lifespan. However, rationally combining new pesticide compounds with existing pesticide components can delay the development of pesticide resistance in pests and effectively control them, thereby promoting agricultural production.
[0003] Isoxazole-containing pyridinium ketone compound is a publicly disclosed patented compound (publication number CN113651811A). It incorporates an isoxazole unit with good insecticidal activity into its mesoionic structure. The compound exhibits a novel structure, good insecticidal activity, and is effective against the resistant pest rice planthopper. The isoxazole unit in the isoxazole structure reduces the activity of metabolic enzymes in resistant pests or increases the penetration of the pesticide into the target site of the pest. The structural formula of isoxazole-containing pyridinium is as follows:
[0004]
[0005] The chemical name of the insecticidal ring is N,N-dimethyl-1,2,3-trithiacyclohexane-5-amine. It belongs to the nereistoxin class of insecticides, and all of its compounds contain the SCC(-N)-CS structure. These compounds enter the insect's body and are easily converted into nereistoxin or its reduced form—dihydronereistoxin (1,3-dimercapto-2-dimethylaminopropane)—within the insect's central nervous system. This results in a blocking effect on the synapses of the insect's central nervous system, that is, it invades the binding site of the insect's nerve cells, blocking the secretion of acetylcholine by a cell and thus eliminating the transmission of excitation. It has contact and stomach poison effects, some systemic activity, and ovicidal properties. This product has a rapid toxic effect on pests, a short residual period, and good control effects on lepidopteran and coleopteran pests.
[0006] Studies have shown that once insects develop resistance to a certain pesticide, they are more likely to develop resistance to other types of pesticides of the same type (with similar molecular structures or mechanisms of action). Therefore, the rational use of new pesticide compounds is an effective measure to reduce the development of insect resistance.
[0007] Single insecticides are prone to developing resistance, which reduces the rate at which pesticides penetrate the insect's epidermis, decreases the insecticidal efficacy, and increases the amount of pesticides used, leading to environmental pollution and other problems. Summary of the Invention
[0008] Purpose of the invention
[0009] To overcome the above shortcomings, the present invention aims to provide a pesticide composition containing an insecticidal ring, its preparation method and application. The present invention rationally mixes isotoxam with an insecticidal ring, effectively extending the service life of isotoxam, giving full play to its superior insecticidal effect, and reducing the amount of pesticide used.
[0010] Solution
[0011] To achieve the objectives of this invention, the technical solution adopted is as follows:
[0012] In a first aspect, the present invention provides a pesticide composition containing an insecticidal ring, wherein the active ingredient of the pesticide composition comprises isotrimazole and an insecticidal ring, wherein the weight ratio of isotrimazole to the insecticidal ring is (0.1:99) to (99:0.1).
[0013] Further, the weight ratio of isozonil to insecticidal ring is (60:1) to (1:30), optionally (49:1) to (1:29), optionally (39:1) to (1:19), optionally (30:1) to (1:20), optionally (29:1) to (1:20).
[0014] 1)~(1:19), optionally (20:1)~(1:10), optionally (19:1)~(1:9), optionally (5:1)~(1:5), optionally (4:1)~(1:4), optionally (1:2)~(1:4), optionally a range of any values consisting of 60:1, 50:1, 49:1, 40:1, 39:1, 30:1, 29:1, 20:1, 19:1, 15:1, 14:1, 10:1, 9:1, 5:1, 4:1, 2:1, 1:1, 1:2, 1:4, 1:5, 1:9, 1:10, 1:14, 1:15, 1:19, 1:20, 1:24, 1:30.
[0015] Further, the active ingredient accounts for 1 to 90% of the total weight of the composition, optionally 1.6 to 80%, optionally 1.6% to 75%, optionally 1.6% to 70%, optionally 16% to 75%.
[0016] Furthermore, the pesticide composition is formulated as one or more of the following: water-dispersible granules, wettable powders, dry suspensions, microcapsule suspensions, granules, emulsifiable concentrates, dispersible oil suspensions, microemulsions, water-in-oil emulsions, suspension seed coating agents, emulsifiable concentrates, and soluble granules.
[0017] Optionally, the pesticide composition further includes an adjuvant, which is selected from at least one of emulsifiers, wetting agents, dispersants, thickeners, antifreeze agents, preservatives, capsule wall materials, film-forming agents, color pastes, defoamers, water, organic solvents, disintegrants, binders, and fillers.
[0018] Furthermore, the emulsifier includes one or at least two of sodium cinnamyl polyoxyethylene ether sulfate, styrene-phenyl polyoxyethylene ether, fatty alcohol polyoxyethylene ether, EO / PO block polyether, and calcium dodecylbenzenesulfonate.
[0019] And / or, the wetting agent is selected from one or at least two of fatty alcohol phosphate, sodium lauryl sulfate, triphenylethylphenol polyoxyethylene ether phosphate, and sodium methylene bisnaphthalene sulfonate;
[0020] And / or, the dispersant is selected from one or at least two of the following: high molecular weight polycarboxylate, sodium salt of naphthalene sulfonate formaldehyde condensate, sodium lignosulfonate, polyether sulfonate, alkenyl sulfonate, polycarboxylate dispersant SP-27001, sodium formaldehyde condensate of alkyl naphthalene sulfonate, sodium salt of phenol sulfonate condensate, and sodium formaldehyde condensate of alkyl naphthalene sulfonate.
[0021] And / or, the thickener is selected from one or more of xanthan gum, magnesium aluminum silicate, silica, bentonite, polyvinyl alcohol, polyurethane, and gum arabic;
[0022] And / or, the antifreeze is one or more of glycerol, ethylene glycol, propylene glycol, urea, and isopropanol;
[0023] And / or, the preservative is one or two of sodium benzoate, Kathon, and potassium sorbate;
[0024] And / or, the capsule wall material is one or more of urea-formaldehyde resin, polyurea, polyurethane, sodium alginate, and chitosan;
[0025] And / or, the film-forming agent is selected from one or at least two of polyvinylpyrrolidone, polyvinyl alcohol, carboxymethyl cellulose, gum arabic, gelatin, xanthan gum, starch, acrylic resin, and polyurethane copolymer resin;
[0026] And / or, the defoamer is silicone and / or polyether;
[0027] And / or, the colorant is selected from one or more of Permanent Red, Bright Red, and Scarlet;
[0028] And / or, the organic solvent is one or more of water, ethyl acetate, xylene, dimethylformamide, and ethyl acetate;
[0029] And / or, the disintegrant includes one or more of sodium carbonate, urea, ammonium sulfate, sodium chloride, sodium bicarbonate, and sodium carboxymethyl starch;
[0030] And / or, the binder is one or more of polyvinyl alcohol, polyvinylpyrrolidone, xanthan gum, starch, and carboxymethyl cellulose;
[0031] And / or, the filler includes one or more of silica, kaolin, and diatomaceous earth.
[0032] In a second aspect, a water-dispersible granule of the pesticide composition described in the first aspect is provided, comprising the following raw materials in weight fractions: isothiazine 3.5-24%, insecticidal ring 4-56%, wetting agent 5-7.2%, dispersant 3-11%, binder 0-3%, disintegrant 1-5%, and filler to 100%;
[0033] Optionally, the raw materials include the following weight fractions: 24% isozonil, 6% chlorpyrifos, 5% DSC-2004 phosphate ester, 6% sodium lauryl polyoxyethylene ether sulfate, 2% sodium naphthalene sulfonic acid condensate, 3% polyvinyl alcohol, 2% sodium chloride, and kaolin to 100%.
[0034] Optionally, the raw materials include the following weight fractions: 14% isothiazine, 56% chlorpyrifos, 6% sodium dodecyl sulfate, 8% sodium naphthalene sulfonate formaldehyde condensate, 3% sodium lignosulfonate, 2% sodium chloride, 5% starch, 5% silica, and kaolin to make up 100%.
[0035] Thirdly, a dry suspension comprising the pesticide composition described in the first aspect is provided, comprising the following raw materials in weight fractions: 5-50% isozonil, 10-20% chlorpyrifos, 5-20% dispersant, 1-8% wetting agent, 1-5% disintegrant, 1-5% defoamer, and filler to 100%;
[0036] Optionally, the raw materials include the following weight fractions: 10% isozonil, 20% chlorpyrifos, 5% modified polycarboxylate DF-1036, 2% fatty alcohol phosphate, 1% sodium lignosulfonate, 5% sodium sulfate, 0.5% organosilicon, and kaolin to make up to 100%.
[0037] Fourthly, a suspension comprising the pesticide composition described in the first aspect is provided, comprising the following raw materials in weight fractions: isothiazine 24-40%, insecticidal ring 6-10%, dispersant 4-10%, emulsifier 2-8%, wetting agent 0-5%, antifreeze agent 0-5%, thickener 0-1%, preservative 0-1%, defoamer 1-5%, and water to 100%;
[0038] Optionally, the raw materials may include the following weight fractions: 10% isozonil, 5% chlorpyrifos, 4% DSC-2004 phosphate ester, 2% high molecular weight polycarboxylate, 1.5% styrene-phenyl polyoxyethylene ether, 2% ethylene glycol, 0.3% magnesium aluminum silicate, 0.2% xanthan gum, 0.1% Kathon, 0.5% organosilicon, and water to 100%.
[0039] Fifthly, the application of the pesticide composition described in the first aspect, or the water-dispersible granules described in the second aspect, or the dry suspension agent described in the third aspect, or the suspension agent described in the fourth aspect, in the control of crop pests, wherein the pests are optionally piercing-sucking pests, and optionally the piercing-sucking pests are at least one of rice planthopper, whitefly, thrips, and aphid.
[0040] A sixth aspect provides a method of using the pesticide composition described in the first aspect, or the water-dispersible granules described in the second aspect, or the dry suspension agent described in the third aspect, or the suspension agent described in the fourth aspect, characterized in that the dosage is 60 g / ha to 120 g / ha based on the effective ingredient.
[0041] Beneficial effects
[0042] (1) The present invention uses isozonil and insecticidal ring in a binary compound, and its activity and insecticidal effect are not a simple superposition of the activities of each component. The two have a significant synergistic effect within a reasonable ratio range, and the dosage is small.
[0043] (2) The present invention rationally mixes isozonil with insecticidal ring, effectively extending the service life of isozonil, giving full play to its superior insecticidal effect, and reducing the amount of pesticide used. Detailed Implementation
[0044] To make the objectives, technical solutions, and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.
[0045] Furthermore, to better illustrate the present invention, numerous specific details are provided in the following detailed embodiments. Those skilled in the art should understand that the present invention can be practiced without certain specific details. In some embodiments, materials, methods, means, etc., well-known to those skilled in the art, are not described in detail in order to highlight the spirit of the present invention.
[0046] Unless otherwise expressly stated, throughout the specification and claims, the term "comprising" or its variations such as "including" or "comprises" shall be understood to include the stated elements or components without excluding other elements or other components.
[0047] The present disclosure will be further illustrated by the following examples, but the present disclosure is not limited thereto.
[0048] The insecticidal rings in the following examples are commercially available, and other adjuvants are also commercially available products. For example, HMK-D09 (emulsifier), phosphate ester DSC-2004 (wetting and dispersing agent), modified polycarboxylate DF-1036 (dispersant), and DF-1009G (sodium lignosulfonate, dispersant) were purchased from Beijing Hanmok Chemical Technology Co., Ltd.
[0049] Isolazid compound and its stereoisomers, or their salts or solvates, all have the same effect. Isolazid was provided by Guizhou University and can also be prepared according to the method in CN113651811A. Other agents were commercially available.
[0050] The present invention will be further described in detail below through examples.
[0051] Test Example 1: Indoor Toxicity Determination
[0052] The synergistic effect of isozonil combined with insecticidal ring was determined using an indoor toxicity assay.
[0053] Test reagents: Insecticidal rings were commercially available, and isothiazine was provided by Guizhou University.
[0054] Experimental design: Based on the preliminary experiment, accurately weigh 10.2041 g of 98% isotretinoin technical grade, dissolve it in acetone, and put it into a 100 ml volumetric flask. Dilute to volume with acetone to obtain a 100 g / L stock solution. Accurately weigh 11.1111 g of 90% chlorpyrifos technical grade, dissolve it in acetone, and put it into a 100 ml volumetric flask. Dilute to volume with acetone to obtain a 100 g / L stock solution. Then weigh the isotretinoin stock solution and the chlorpyrifos stock solution separately and mix them according to the ratio in Table 1.
[0055] The test was conducted in accordance with the "NY / T1154.11-2008 Guidelines for Indoor Bioassay of Pesticides (Insecticides)" and the co-toxicity coefficient was determined using the method proposed by Sun Yunpei et al. (1960) for calculating co-toxicity.
[0056] The calculation formula is as follows (using insecticidal rings as the standard pesticide, with a toxicity index of 100).
[0057] The toxicity index (TI) of isozonazole is equal to the ED of the insecticidal ring. 50 ED of isozonazole 50×100.
[0058] Actual Toxicity Index (ATI) of the mixture = ED of the insecticidal ring 50 / M of ED 50 ×100.
[0059] Theoretical Toxicity Index (TTI) of Mixtures = Isoxamethonium TI × P 异唑虫嘧啶 +Insecticide Ring TI×P 杀虫环 .
[0060] Co-toxicity coefficient (CTC) = [Actual toxicity index (ATI) of the mixture / Theoretical toxicity index (TTI) of the mixture] × 100
[0061] In the formula: P 异唑虫嘧啶 This refers to the proportion of isozonazole in the compound composition;
[0062] P 杀虫环 This refers to the proportion of the insecticidal ring in the compound composition.
[0063] Evaluation criteria: When CTC≤80, the composition exhibits antagonistic effects; when 80<CTC<120, the composition exhibits additive effects; when CTC≥120, the composition exhibits synergistic effects.
[0064] Indoor toxicity test of isothiazine mixed with insecticidal ring for the control of rice planthoppers
[0065] Test method: Refer to "NY / T1154.9-2008 Guidelines for Indoor Bioassay of Pesticides - Part 9: Spraying Method".
[0066] The experimental results are shown in Table 1:
[0067] Table 1. Results of toxicity assays on rice planthoppers using a mixture of isozonil and insecticidal rings.
[0068] deal with <![CDATA[LC 50 (μg / L)]]> ATI TTI CTC Isozopyr (A) 3.10 558.91 / / Insecticide ring (B) 17.35 100.00 / / A:B = 60:1 2.45 707.72 551.38 128.4 A:B = 50:1 2.38 728.75 549.91 132.5 A:B = 40:1 2.54 682.33 547.71 124.6 A:B = 30:1 2.43 713.82 544.10 131.2 A:B = 20:1 2.31 750.45 537.05 139.7 A:B = 15:1 2.22 782.92 530.22 147.7 A:B = 10:1 2.34 742.16 517.19 143.5 A:B = 4:1 2.19 790.81 467.12 169.3 A:B = 2:1 2.65 655.66 405.94 161.5 A:B = 1:1 3.32 523.04 329.45 158.8 A:B = 1:2 4.02 431.28 252.97 170.5 A:B = 1:4 4.81 360.70 191.78 188.1 A:B = 1:10 8.68 199.86 141.72 141.0 A:B = 1:15 9.85 176.14 128.68 136.9 A:B = 1:20 10.77 161.03 121.85 132.1 A:B = 1:30 12.26 141.47 114.80 123.2 A:B = 1:40 13.18 131.67 111.19 118.4
[0069] Table 1 shows that when the mass ratio of isotrazine to insecticidal ring is (60:1) to (1:30), the co-toxicity coefficient is greater than 120, exhibiting a significant synergistic effect against rice planthoppers. The preferred mass ratios are (30:1) to (1:20), (20:1) to (1:10), (4:1) to (1:4), and (1:2) to (1:4). Synergistic effects are also observed at ratios of 60:1, 50:1, 40:1, 30:1, 20:1, 15:1, 10:1, 4:1, 2:1, 1:1, 1:2, 1:4, 1:10, 1:15, 1:20, and 1:30. Among these, the synergistic effect is most pronounced when the weight ratio of isotrazine to insecticidal ring is 1:4.
[0070] Activity assay of isozonil and insecticidal ring mixture in controlling cabbage aphids
[0071] Experimental method: Refer to "NYT 1154.14-2008 Guidelines for Indoor Bioassay Testing of Pesticides - Part 14: Leaf Dipping Method".
[0072] The experimental results are shown in Table 2:
[0073] Table 2. Indoor toxicity test against cabbage aphids
[0074] deal with <![CDATA[LC 50 (μg / l)]]> ATI TTI CTC Isozopyr (A) 19.41 37.24 / / Insecticide ring (B) 7.23 100.00 / / A:B = 49:1 14.93 48.42 38.50 125.8 A:B = 39:1 14.33 50.44 38.81 130.0 A:B = 29:1 13.43 53.83 39.33 136.8 A:B = 24:1 13.23 54.64 39.75 137.4 A:B = 19:1 12.03 60.08 40.38 148.8 A:B = 9:1 11.61 62.24 43.52 143.0 A:B = 5:1 7.91 91.33 47.70 191.5 A:B = 1:1 6.55 110.38 68.62 160.9 A:B = 1:5 5.09 142.02 89.54 158.6 A:B = 1:9 5.21 138.76 93.72 148.0 A:B = 1:14 5.43 133.06 95.82 138.9 A:B = 1:19 5.56 129.97 96.86 134.2 A:B = 1:29 5.83 124.09 97.91 126.7 A:B = 1:39 6.41 112.75 98.43 114.55
[0075] Table 2 shows that when the mass ratio of isotrazine to insecticidal ring is (49:1) to (1:29), the co-toxicity coefficient is greater than 120, exhibiting a significant synergistic effect against cabbage aphids. The preferred mass ratios are (39:1) to (1:19), (29:1) to (1:19), (19:1) to (1:9), and (5:1) to (1:5). Synergistic effects are also observed at ratios of 49:1, 39:1, 29:1, 19:1, 9:1, 5:1, 1:1, 1:5, 1:9, 1:14, 1:19, and 1:29. Among these, the synergistic effect is most pronounced when the weight ratio of isotrazine to insecticidal ring is 5:1.
[0076] Example 1: 61% Isolazid·Insecticidal wettable powder (60:1)
[0077] 60% isazolidinium, 1% chlorpyrifos, 5% alkylnaphthalene sulfonate, 1% DF-1009G (sodium lignosulfonate, dispersant, purchased from Beijing Hanmok Chemical Technology Co., Ltd.), 1% silica, and kaolin to make up to 100%.
[0078] Processing technology: Mix the above materials evenly, and then pulverize them evenly using an air jet mill to obtain 61% isozonil·carbendazim wettable powder.
[0079] Example 2: 30% isotretinoin·carbendazim water-dispersible granules (4:1)
[0080] 24% isothiazine, 6% chlorpyrifos, 5% DSC-2004 phosphate ester, 6% sodium lauryl polyoxyethylene ether sulfate (emulsifier), 2% sodium naphthalene sulfonic acid condensate (dispersant), 3% polyvinyl alcohol (binder), 2% sodium chloride (disintegrant), and kaolin to make up to 100%.
[0081] Processing technology: The above materials are pulverized by an air jet mill, granulated, dried and sieved to obtain water-dispersible granule dosage form products.
[0082] Example 3: 15% isotretinoin·carbendazim wettable powder (2:1)
[0083] 10% isazolidin, 5% chlorpyrifos, 4% DSC-2004 phosphate ester (dispersant), 2% high molecular weight polycarboxylate (dispersant), 1.5% styrene-phenyl polyoxyethylene ether (wetting agent), and kaolin to make up to 100%.
[0084] Processing technology: Refer to Example 1.
[0085] Example 4: 30% isazolidin·carbendazim dispersible oil suspension (1:2)
[0086] 10% isothiazine, 20% chlorpyrifos, 5% modified polycarboxylate DF-1036 (dispersant), 2% fatty alcohol phosphate (wetting agent), 1% sodium lignosulfonate (dispersant), 0.5% silica (thickener), methyl oleate (filler) to make up to 100%.
[0087] The preparation method is as follows: Prepare raw materials according to the above-mentioned composition, and then carry out the preparation according to the following steps:
[0088] S1. Isopyrimidine, insecticidal ring, wetting agent, dispersant and thickener are added to the filler in sequence and stirred thoroughly to obtain a slurry.
[0089] S2. Pour the slurry obtained in step S1 into a sand mill containing zirconia beads and grind it in the sand mill for 2-3 hours until the slurry has a particle size of 2-5 micrometers. After grinding, filter to remove the zirconia beads and collect the filtrate to obtain the dispersible oil suspension.
[0090] Example 5: 70% isazolidin·carbendazim water-dispersible granules (1:4)
[0091] 14% isothiazine, 56% insecticidal ring, 2% sodium alkyl sulfonate (wetting agent), 10% sodium polycarboxylate (dispersant), 3% sodium lignin sulfonate (dispersant), and corn starch to make up 100%.
[0092] Processing technology: The above materials are pulverized by an air jet mill, granulated, dried and sieved to obtain water-dispersible granule dosage form products.
[0093] Example 6: 35% isotretinoin·carbendazim water-dispersible granules (1:9)
[0094] 3.5% isazolidinium, 31.5% chlorpyrifos, 6% sodium dodecyl sulfate (wetting agent), 5% sodium naphthalenesulfonic acid formaldehyde condensate (dispersant), 2.5% carboxymethyl cellulose (binder), 2% sodium carbonate (disintegrant), and diatomaceous earth to make up 100%.
[0095] Processing technology: Refer to Example 5.
[0096] Example 7: 32% isotretinoin·carbendazim water-dispersible granules (15:1)
[0097] 30% isothiazine, 2% insecticidal ring, 6% HMK-D09 (emulsifier), 3% high molecular weight polycarboxylate (dispersant), 1% triphenylethylphenol polyoxyethylene ether phosphate, corn starch supplement 100%.
[0098] Processing technology: Refer to Example 5.
[0099] Example 8: 1.6% isazolidin-carbendazim granules (1:15)
[0100] 0.1% isazolidin, 1.5% insecticidal ring, 4% naphthalenesulfonate formaldehyde condensate, 1% high molecular weight polycarboxylate, 2% ammonium dihydrogen phosphate fertilizer, 2% corn starch, 10% urea, and kaolin to make up 100%.
[0101] Processing technology: Mix isozonazole, insecticidal ring, wetting and dispersing agent, binder and filler evenly according to the formula ratio, and then granulate to obtain granule product.
[0102] Example 9: 21% isozonil·insecticide suspension seed coating agent (20:1)
[0103] 20% isazolidinium, 1% chlorpyrifos, 2% fatty alcohol phosphate, 3% high molecular weight polycarboxylate, 3% polyvinylpyrrolidone (film-forming agent), 0.5% xanthan gum, 0.05% organosilicon, 2% glycerol, 0.2% carmine, water to 100%.
[0104] Processing technology: Mix isozonil, insecticide ring, surfactant or wetting and dispersing agent evenly according to the above formula ratio, then add an appropriate amount of water, wet grind with a sand mill, then transfer the material to a shearing kettle, add film-forming agent, thickener, antifreeze, defoamer, warning color and the remaining water, and shear at high speed until the viscosity and particle size meet the standards to obtain the suspension seed coating agent product.
[0105] Example 10: 48% Isolazid·Insecticidal water-dispersible granules (15:1)
[0106] 45% isazolidinium, 3% chlorpyrifos, 7.2% sodium naphthalenesulfonic acid formaldehyde condensate, 3% modified polycarboxylate, 3% sodium lignosulfonate, 2% sodium chloride (disintegrant), 10% starch (binder), and kaolin to make up 100%.
[0107] Processing technology: Refer to Example 5.
[0108] Example 11: 50% isazolidinone·carbendazim soluble granules (9:1)
[0109] 45% isothiazine, 5% insecticidal ring, 5% pyrethroid, 3.5% polyether sulfonate, 1.5% sodium lignosulfonate, 5% polyvinyl alcohol (binder), diatomaceous earth to make up 100%.
[0110] Processing technology: After the above materials are pulverized by an air jet mill, they are mixed evenly, granulated, dried, and sieved to obtain soluble granules.
[0111] Comparative Example 1: 30% Isolazid Suspension
[0112] 30% isothiazine, 5% DSC-2004 phosphate ester (wetting agent), 6% sodium lauryl polyoxyethylene ether sulfate (emulsifier), 2% sodium naphthalene sulfonic acid condensate (dispersant), 3% ethylene glycol (antifreeze), 0.5% magnesium aluminum silicate (thickener), 0.5% organosilicon (defoamer), water to 100%.
[0113] Processing technology: Mix isozonil, emulsifier or wetting and dispersing agent evenly according to the above formula ratio, then add an appropriate amount of water, wet grind with a sand mill, then transfer the material to a shearing machine, add antifreeze, defoamer and the remaining water, and shear at high speed for 3-4 hours to obtain the suspension product.
[0114] Test Example 2: Field efficacy trial for controlling rice planthoppers
[0115] Experimental subjects: Naturally occurring populations in paddy fields surrounding Qintang District, Guigang City, Guangxi Province, during August and September 2024.
[0116] Experimental method: During the tillering stage of late-season rice, all pesticides were added to 30L / mu of water according to the actual dosage, stirred well, and then sprayed evenly at the base of the rice plants. Refer to GB / T 17980.4-2000 Guidelines for Field Efficacy Testing of Pesticides (I) Insecticides for the Control of Rice Planthoppers.
[0117] Test reagents: Reagents prepared in Examples 1-7 and Example 10, and control reagents CK1 and CK2. Among them,
[0118] Control agent CK 1: 30% isotretinoin suspension (Comparative Example 1).
[0119] Control agent CK 2: 50% insecticide ring soluble powder, registration certificate number PD20212416, purchased from Hunan Haohua Chemical Co., Ltd.
[0120] The experimental rice was grown in the late tillering stage, and the experiment was conducted in early to mid-August. Each treatment was replicated four times, and 10 points were surveyed in each plot using the parallel skip method, with two clumps at each point, for a total of 80 clumps.
[0121] Target pest: Rice planthopper.
[0122] Application method: conventional spraying.
[0123] Calculation formula:
[0124]
[0125] The insect population in each group was investigated 10 days and 30 days after pesticide application. The investigation method was in accordance with "GB / T 17980.4-2000 Field Efficacy Test Guidelines for Pesticides (I) Insecticides for the Control of Rice Planthoppers". The results are shown in Table 3.
[0126] Table 3. Results of field trials for controlling rice brown planthopper
[0127] As shown in Table 3, the control efficacy of Examples 1-7 and Example 10 was higher than that of CK1 and CK2 10 days and 30 days after application, and the dosage was also significantly lower than that of CK1 and CK2. Moreover, the control efficacy was still above 92% 30 days after application, with a long duration of effect, which greatly reduced the number of times to apply pesticides to control brown planthoppers during the rice growing season.
[0128] Test Example 3: Field efficacy trial of pesticides for controlling aphids on cruciferous vegetables, such as cabbage.
[0129] Experimental methods: Refer to "NY / T 1464.27-2010 Field Efficacy Test Guidelines for Pesticides, Part 27: Insecticide Control of Aphids in Cruciferous Vegetables". Spraying began at the initial stage of aphid infestation. There were 9 treatments, with 4 replicates per treatment. Five samples were taken from each plot, and 3 cabbage plants were surveyed at each sample point.
[0130] Test reagents: Examples 1-6, control reagent CK1, control reagent CK2, wherein,
[0131] Control agent CK1: 30% isotretinoin suspension (Comparative Example 1).
[0132] Control agent CK2: 50% insecticidal ring soluble powder, registration certificate number PD20212416, Hunan Haohua Chemical Co., Ltd.
[0133] Target pest: Cabbage aphid.
[0134] Application method: conventional spraying.
[0135] Calculation formula:
[0136]
[0137] The insect population in each group was investigated 7 days and 14 days after application of the pesticide. The results are shown in Table 4.
[0138] Table 4. Results of field trials for controlling aphids on cruciferous vegetables, specifically cabbage. As shown in Table 4, the efficacy of Examples 1-6 was higher than that of CK1 and CK2 at 7 and 14 days after administration, and the dosage was also lower. Moreover, the efficacy was still above 91% at 14 days after administration, with a long duration of effect, which greatly reduced the number of times the drug was used.
[0139] Test Example 4: Field efficacy trial for controlling tomato whiteflies
[0140] Test reagents: Examples 1-6, Example 11, control reagent CK1, control reagent CK2, wherein,
[0141] Control agent CK1: 30% isotretinoin suspension (Comparative Example 1).
[0142] Control agent CK2: 50% insecticide ring soluble powder, registration certificate number PD20212416, Hunan Haohua Chemical Co., Ltd.
[0143] Experimental design: 10 treatments, 4 replicates per treatment.
[0144] Experimental Methods and Survey: During the tomato fruiting period, at the early stage of whitefly infestation (July 20th), the pesticide was sprayed. The experimental pesticide was diluted with 50 kg / mu of water, and an electric sprayer was used to evenly spray both sides of the tomato leaves. The entire experiment was conducted with one spraying. In each plot, the number of live insects on the middle 10 tomato plants was surveyed. The initial insect population was surveyed before spraying, and the number of remaining live insects was surveyed 1 day and 3 days after spraying.
[0145] Calculation formula:
[0146]
[0147] The results are shown in Table 5.
[0148] Table 5. Results of field trials for controlling tomato whiteflies As shown in Table 5, the control efficacy of Examples 1-6 and Example 11 against tomato whiteflies was higher than that of the control agents CK1 and CK2, especially the control efficacy was more prominent 14 days after application.
[0149] In summary, the binary combination of isozonil and insecticidal ring of the present invention is not a simple superposition of the activities of each component. The two have a significant synergistic effect within a reasonable ratio range, and the dosage is small.
[0150] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims
1. A pesticide composition containing an insecticidal ring, characterized in that, The active ingredients of the pesticide composition include isothiazine and cyclophosphamide, wherein the weight ratio of isothiazine to cyclophosphamide is (0.1:99) to (99:0.1).
2. The pesticide composition according to claim 1, characterized in that, The weight ratio of isozonil to insecticidal ring is (60:1) to (1:30), optionally (49:1) to (1:29), optionally (39:1) to (1:19), optionally (30:1) to (1:20), optionally (29:1) to (1:19), optionally (20:1) to (1:10), optionally (19:1) to (1:9), optionally (5:1) to (1:5), optionally (4:1) to (1:10). :4), optionally (1:2) to (1:4), optionally a range of any values consisting of 60:1, 50:1, 49:1, 40:1, 39:1, 30:1, 29:1, 20:1, 19:1, 15:1, 14:1, 10:1, 9:1, 5:1, 4:1, 2:1, 1:1, 1:2, 1:4, 1:5, 1:9, 1:10, 1:14, 1:15, 1:19, 1:20, 1:24, 1:
30.
3. The pesticide composition according to claim 1 or 2, characterized in that, The active ingredient accounts for 1-90% of the total weight of the composition, optionally 1.6-80%, optionally 1.6%-75%, optionally 1.6%-70%, optionally 16%-75%.
4. The pesticide composition according to any one of claims 1 to 3, characterized in that, The pesticide composition is formulated as one or more of the following: water-dispersible granules, wettable powders, dry suspensions, microcapsule suspensions, granules, emulsifiable concentrates, oil-dispersible suspensions, microemulsions, water-in-oil emulsions, suspension seed coating agents, emulsifiable concentrates, and soluble granules. Optionally, the pesticide composition further includes an adjuvant, which is selected from at least one of emulsifiers, wetting agents, dispersants, thickeners, antifreeze agents, preservatives, capsule wall materials, film-forming agents, color pastes, defoamers, water, organic solvents, disintegrants, binders, and fillers.
5. The pesticide composition according to claim 4, characterized in that, The emulsifiers include one or at least two of the following: sodium cinnamyl polyoxyethylene ether sulfate, HMK-D09, styrene-phenyl polyoxyethylene ether, fatty alcohol polyoxyethylene ether, EO / PO block polyether, and calcium dodecylbenzene sulfonate. And / or, the wetting agent is selected from one or at least two of sodium alkyl sulfonate, fatty alcohol phosphate, sodium dodecyl sulfate, triphenylethylphenol polyoxyethylene ether phosphate, and sodium methylene bisnaphthalene sulfonate; And / or, the dispersant is selected from one or at least two of the following: sodium polycarboxylate, high molecular weight polycarboxylate, sodium naphthalene sulfonate formaldehyde condensate, modified polycarboxylate DF-1036, sodium lignosulfonate, polyether sulfonate, alkenyl sulfonate, polycarboxylate dispersant SP-27001, sodium alkyl naphthalene sulfonate formaldehyde condensate, sodium phenol sulfonate condensate, and sodium alkyl naphthalene sulfonate formaldehyde condensate; And / or, the thickener is selected from one or more of xanthan gum, magnesium aluminum silicate, silica, bentonite, polyvinyl alcohol, polyurethane, and gum arabic; And / or, the antifreeze is one or more of glycerol, ethylene glycol, propylene glycol, urea, and isopropanol; And / or, the preservative is one or two of sodium benzoate, Kathon, and potassium sorbate; And / or, the capsule wall material is one or more of urea-formaldehyde resin, polyurea, polyurethane, sodium alginate, and chitosan; And / or, the film-forming agent is selected from one or at least two of polyvinylpyrrolidone, polyvinyl alcohol, carboxymethyl cellulose, gum arabic, gelatin, xanthan gum, starch, acrylic resin, and polyurethane copolymer resin; And / or, the defoamer is silicone and / or polyether; And / or, the colorant is selected from one or more of Permanent Red, Bright Red, and Scarlet; And / or, the organic solvent is one or more of water, ethyl acetate, xylene, dimethylformamide, and ethyl acetate; And / or, the disintegrant includes one or more of sodium carbonate, urea, ammonium sulfate, sodium chloride, sodium bicarbonate, and sodium carboxymethyl starch; And / or, the binder is one or more of polyvinyl alcohol, polyvinylpyrrolidone, xanthan gum, starch, and carboxymethyl cellulose; And / or, the filler includes one or more of the following: white carbon black, kaolin, diatomaceous earth, and corn starch.
6. A water-dispersible granule comprising the pesticide composition according to any one of claims 1 to 5, characterized in that, The raw materials include the following weight fractions: isothiazine 3.5-24%, insecticidal ring 4-56%, wetting agent 5-7.2%, dispersant 3-11%, binder 0-3%, disintegrant 1-5%, and filler to 100%; Optionally, the raw materials include the following weight fractions: 24% isozonil, 6% chlorpyrifos, 5% DSC-2004 phosphate ester, 6% sodium lauryl polyoxyethylene ether sulfate, 2% sodium naphthalene sulfonic acid condensate, 3% polyvinyl alcohol, 2% sodium chloride, and kaolin to 100%. Optionally, the raw materials include the following weight fractions: 14% isozonil, 56% chlorpyrifos, 2% sodium alkyl sulfonate, 10% sodium polycarboxylate, 3% sodium lignin sulfonate, and corn starch to make up 100%.
7. A dispersible oil suspension comprising the pesticide composition according to any one of claims 1 to 5, characterized in that, The raw materials include the following weight fractions: isothiazine 5-50%, insecticidal ring 10-20%, dispersant 5-20%, wetting agent 1-8%, thickener 1-5%, and solvent to 100%; Optionally, the raw materials include the following weight fractions: 10% isozonil, 20% chlorpyrifos, 5% modified polycarboxylate DF-1036, 2% fatty alcohol phosphate, 1% sodium lignosulfonate, 0.5% silica, and methyl oleate to make up to 100%.
8. A wettable powder comprising the pesticide composition according to any one of claims 1 to 5, characterized in that, The raw materials include the following weight fractions: isothiazine 24-40%, insecticidal ring 6-10%, dispersant 4-10%, emulsifier 2-8%, wetting agent 0-5%, and kaolin to make up to 100%; Optionally, the raw materials may include the following weight fractions: 10% isozonil, 5% chlorpyrifos, 4% DSC-2004 phosphate ester, 2% high molecular weight polycarboxylate, 1.5% styrene-phenyl polyoxyethylene ether, and kaolin to make up to 100%.
9. The application of a pesticide composition according to any one of claims 1 to 5, or a water-dispersible granule according to claim 6, or a dispersible oil suspension according to claim 7, or a wettable powder according to claim 8, in the control of crop pests, wherein the pests are optionally piercing-sucking pests, and optionally the piercing-sucking pests are at least one of rice planthoppers, whiteflies, thrips, and aphids.
10. A method of using the pesticide composition according to any one of claims 1 to 5, or the water-dispersible granules according to claim 6, or the dispersible oil suspension according to claim 7, or the wettable powder according to claim 8, characterized in that, The dosage is calculated based on the active ingredient and is 60-120 grams per hectare.
Citation Information
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Isoxazole-containing pyridopyrimidinone compound as well as preparation method and application thereof
CN113651811A