A herbicidal composition containing butachlor, isoxaben and isoxaflotole and its use

Abstract

The present application belongs to the field of agriculture, and particularly relates to a herbicidal composition containing butachlor, metamifop and isoxaben and application thereof, wherein the herbicidal composition is in the form of dispersible oil suspending agent, and contains the following components in the weight percentage: butachlor 20-28%, metamifop 6-10%, isoxaben 3-9%, emulsifier 10-20%, dispersant 1-5%, organic bentonite 0.5-2%, and methyl oleate to make up 100%. The emulsifier is a combination of EL-10 and Termul 2507, and the dispersant is ATLOX 4916. The dispersible oil suspending agent prepared by the present application has excellent emulsifying performance, suspending performance, good thermal storage stability and cold storage stability, and the specific surfactant combination can further reduce the thermal storage decomposition rate of the active ingredient. The active ingredient of the 38% dispersible oil suspending agent prepared by the present application is used in an amount of 20-30 g / mu to have excellent control effect on weeds in rice fields.

Description

Technical Field

[0001] This invention belongs to the agricultural field, specifically relating to a herbicidal composition containing butachlor, oxazolidinyl and isoxaflutole, and its application. Background Technology

[0002] Oxazolidinone is an aryloxyphenoxypropionate herbicide developed by the Korea Institute of Chemical Technology. Its mechanism of action is the inhibition of acetyl-CoA carboxylase. It primarily controls most annual grasses in transplanted and direct-seeded fields, exhibiting low toxicity and environmental safety. It is mainly absorbed through plant stems and leaves; the active ingredient needs to reach its target within the plant to exert its herbicidal effect. Therefore, the requirements for the adjuvant system are relatively high, utilizing solvents and surfactants to allow the active ingredient to enter the plant and exert its effect.

[0003] Isoxaben is an organic heterocyclic selective pre-emergence herbicide that can be absorbed through plant roots and shoots and translocated upwards to all parts of the plant via transpiration, thereby controlling the biosynthesis of chlorophyll in sensitive plants. Although it can germinate and emerge from the soil, it lacks pigment, causing the plants to die within a short period of time. It has a good control effect on grass weeds such as barnyard grass and wild millet, as well as annual broadleaf weeds such as lambsquarters, knotweed, amaranth, and cocklebur.

[0004] Butachlor is a selective pre-emergence herbicide of the amide class. It is mainly absorbed through the young shoots and small secondary roots of weeds, inhibiting protein synthesis, causing the young weeds to swell, become deformed, and turn dark green, ultimately leading to their death. Butachlor is photostable, can be decomposed by soil microorganisms, and is safe for subsequent crops.

[0005] CN202310986082.0 discloses a method for controlling resistant *Leymus chinensis*, employing a combination of pre-emergence and post-emergence herbicides. The specific application steps include: S1. Sowing rice after germination; 1-2 days after sowing, applying a soil-sealing treatment followed by the first application of a pre-emergence herbicide; S2. 9-10 days after sowing, applying a second application of a selected post-emergence herbicide; S3. 10-11 days after sowing, applying a third application of a suitable amount of dichlorvos·propargyl·pyrimisulfuron. The pre-emergence herbicide is butachlor or pretilachlor; the post-emergence herbicide is two or more of cyhalofop-butyl, oxazolidinyl, propargite, or isoxaflutole. The method specifically discloses that the combination of butachlor + oxazolidinyl + isoxaflutole exhibits excellent control efficacy against resistant *Leymus chinensis* in rice paddies. The three drugs in this document were administered separately and were not mixed, and the relevant formulations were not disclosed.

[0006] Oil-dispersible suspension concentrates are an environmentally friendly pesticide formulation in which the active ingredient is dispersed as solid microparticles in a non-aqueous medium, forming a stable suspension. This formulation offers advantages such as small particle size, high suspension rate, good dispersibility, good adhesion, good affinity for the target, and ease of mechanized application. Currently, there are no reports on the preparation of butachlor, oxazolidinyl, and isoxaflutole into oil-dispersible suspension concentrates. Summary of the Invention

[0007] This invention provides a herbicidal composition formulation with excellent emulsifying and suspending properties, as well as good thermal and cold storage stability, and its application. The specific technical solution is as follows:

[0008] A herbicidal composition containing butachlor, oxazolidinyl and isoxaflutole, comprising the following components in weight percentage: butachlor 20-28%, oxazolidinyl 6-10%, isoxaflutole 3-9%, emulsifier 10-20%, dispersant 1-5%, organobentonite 0.5-2%, and methyl oleate to make up 100%;

[0009] Preferably, the product comprises the following components in weight percentage: butachlor 24%, oxazolidinyl 8%, isoxaflutole 6%, emulsifier 10-20%, dispersant 1-5%, organobentonite 0.5-2%, and methyl oleate to make up 100%.

[0010] Preferably, the product comprises the following components in weight percentage: butachlor 24%, oxazolidinyl 8%, isoxaflutole 6%, emulsifier 16%, dispersant 2%, organobentonite 1%, and methyl oleate to make up 100%.

[0011] The emulsifier is a combination of EL-10 and Termul 2507, and the dispersant is ATLOX 4916. The preferred mass ratio of EL-10 to Termul 2507 is 1:5-5:1; the mass ratio of emulsifier to dispersant is 6-10:1.

[0012] The herbicidal composition of the present invention is formulated as a dispersible oil suspension.

[0013] The formulation of the present invention is used to control weeds in crop fields, preferably grass weeds, broadleaf weeds and sedges in paddy fields.

[0014] Compared with existing technologies, it has the following beneficial technical effects.

[0015] When the surfactant combination of EL-10, Termul 2507, and ATLOX 4916 is selected in the dispersible oil suspension, the formulation exhibits excellent emulsifying properties, satisfactory thermal and cold storage performance, and effectively reduces the thermal decomposition rate of the active ingredient. Furthermore, the 38% dispersible oil suspension prepared by this invention demonstrates excellent weed control efficacy in paddy fields at an active ingredient dosage of 20-30 g / mu. Detailed Implementation

[0016] The present invention will be further described below with reference to embodiments, but the present invention is not limited thereto.

[0017] Example 1: Preparation of 38% Butane·Oxazole·Isoxamethasone Dispersible Oil Suspension.

[0018] The dispersible oil suspension contains the following components by weight percentage: butachlor 24%, oxazolidinyl 8%, isoxaflutole 6%, surfactant (emulsifier + dispersant) 18%, organobentonite 1%, and methyl oleate to make up to 100%.

[0019] Table 1. Surfactant Screening Scheme

[0020] 1 EL-10+ATLOX 4916 16+2 2 AEO-3+ATLOX 4916 16+2 3 Termul 2507 + ATLOX 4916 16+2 4 EL-10+AEO-3+ATLOX 4916 8+8+2 5 EL-10 + Terminus 2507 + ATLOX 4916 8+8+2 6 AEO-3 + Terminus 2507 + ATLOX 4916 8+8+2 7 EL-10 + Terminus 2507 + ATLOX 1086 8+8+2 8 EL-10+Termul 2507+Tersperse2700 8+8+2 9 EL-10 + Terminus 2507 + ATLOX 4916 8+8+1 10 EL-10 + Terminus 2507 + ATLOX 4916 8+8+3

[0021] Among them: EL-10, AEO-3, and Termul 2507 are emulsifiers; ATLOX 4916, ATLOX 1086, and Tersperse 2700 are dispersants.

[0022] Wet grinding is employed, with a certain amount of medium, emulsifier, dispersant, thickener, and active ingredient added in sequence. The mixture is then poured into the grinding chamber of a sand mill and ground for 1.5–2.5 hours. Grinding is stopped when the material D90 is measured to be ≤5μm using a laser particle size analyzer, and the mixture is filtered to obtain the final product.

[0023] Storage physical stability is expressed as the oil separation rate (the percentage of oil separation volume to the total volume). Hot storage is defined as storage at (54±2)℃ for 14 days; cold storage is defined as standing at (0±2)℃ for 7 days, and the oil separation rate is then determined. Suspension rate determination: performed according to GB / T14825—2006.

[0024] Table 2. Effects of different emulsifier combinations on formulation performance.

[0025]

[0026] Table 2 shows that the formulations using single emulsifiers and dispersants in treatments 1-3 exhibited poor emulsification performance and high oil separation rates during both hot and cold storage. Treatments 4-6, using composite emulsifiers, effectively improved the emulsification performance and reduced oil separation rates during both hot and cold storage. In particular, treatment 5, using the surfactant combination of EL-10, Termul 2507, and ATLOX 4916, demonstrated excellent emulsification performance and passed both hot and cold storage tests.

[0027] Table 3. Effects of Emulsifier and Dispersant Combinations on the Physical Stability of Formulations

[0028] 5 99.7 qualified qualified 7 90.2 qualified Oil separation 5.1% 8 84.1 Oil separation 4.9% Oil separation 17.4% 9 97.2 qualified Oil separation 2.5% 10 98.0 qualified qualified

[0029] Since some active pharmaceutical ingredients and other solid particles are insoluble in the oil phase and are merely suspended within it, they are thermodynamically unstable. Therefore, emulsifiers alone are insufficient to ensure the physical stability of the formulation; a suitable dispersant must also be added. The main function of the dispersant is to ensure the long-term stable and uniform dispersion of solid active pharmaceutical ingredient particles in oil-based dispersion media, preventing flocculation and particle size growth. Table 3 shows that in treatments 5, 7, and 8, the combination of the composite emulsifier (EL-10 + Termul 2507) with different dispersants significantly affects the suspension rate and physical stability of the formulation. Compared with dispersants ATLOX 1086 or Tersperse 2700, the combination of dispersant ATLOX 4916 with the composite emulsifier significantly improves the suspension performance and stability of the formulation, with an optimal dosage of 2%.

[0030] Table 4. Effect of surfactant selection on the thermal storage stability of active ingredients

[0031]

[0032] As shown in Table 4, the surfactant combinations of treatments 1-5 can all control the thermal decomposition rate of the active ingredient in the formulation to ≤5% after 14 days of heat storage. Compared with other treatments, the combination of surfactant EL-10 + Termul 2507 + ATLOX 4916 can further reduce the thermal decomposition rate of the active ingredient.

[0033] Example 2: Field control efficacy of 38% dispersible oil suspension against weeds in paddy fields.

[0034] Experimental site: The terrain is flat, the soil pH is 6.8, and the organic matter content is 2.7%. The rice was transplanted on May 28, 2023, and is in the 4-5 leaf stage. The target weeds in the experimental site include barnyard grass, crabgrass, Echinochloa crus-galli, Polygonum hydropiper, and Cyperus difformis.

[0035] Experimental design: There were 3 treatments, with 4 replicates per treatment, for a total of 12 plots. Each plot had an area of ​​30 m2 and the plots were arranged in a randomized block design.

[0036] Test reagent: 38% Butane·Oxazole·Isoxamethasone dispersible oil suspension (Formulation for Treatment 5 in Table 1)

[0037] Application method: The pesticide was applied on June 8, 2023. At the time of application, the rice seedlings had recovered and turned green, and the weeds were in the germination to 2-3 leaf stage. The treatment was carried out by foliar spraying.

[0038] Survey Methods and Data Analysis: Four points were randomly selected from each community, each 0.25m wide. 2 For each quadrat, the fresh weight of the above-ground portion of weeds at each sampling point in each plot was recorded 21 days after application, and the fresh weight control efficacy was calculated according to the formula.

[0039] Fresh weight control efficacy / % = (fresh weight of weeds in blank control area - fresh weight of weeds in chemically treated area) / fresh weight of weeds in blank control area × 100.

[0040] Test results:

[0041] Table 5. Field control efficacy of 38% dispersible oil suspension against weeds in paddy fields.

[0042]

[0043] As shown in Table 5, the active ingredient dosage of 38% dispersible oil suspension at 20-30 g / mu has excellent control effect on weeds in paddy fields.

[0044] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and are not intended to limit it.

Claims

1. A herbicidal composition containing butachlor, oxazolidinyl and isoxaflutole, characterized in that, It contains the following components in weight percentage: butachlor 20-28%, oxazolidinyl 6-10%, isoxaflutole 3-9%, emulsifier 10-20%, dispersant 1-5%, organobentonite 0.5-2%, and methyl oleate to make up 100%; the mass ratio of the emulsifier and dispersant is 6-10:1; the dispersant is ATLOX 4916; the emulsifier is a combination of EL-10 and Termul 2507, with a mass ratio of 1:5-5:

1.

2. The herbicidal composition according to claim 1, characterized in that, It contains the following ingredients in weight percentage: butachlor 24%, oxazolidinyl 8%, isoxaflutole 6%, emulsifier 10-20%, dispersant 1-5%, organobentonite 0.5-2%, and methyl oleate to make up 100%.

3. The herbicidal composition according to claim 2, characterized in that, It contains the following ingredients in weight percentage: butachlor 24%, oxazolidinyl 8%, isoxaflutole 6%, emulsifier 16%, dispersant 2%, organobentonite 1%, and methyl oleate to make up 100%.

4. Use of the herbicidal composition according to any one of claims 1-3 for controlling weeds in crop fields.

5. The use according to claim 4, characterized in that, The weeds mentioned are grassy weeds, broadleaf weeds, and sedges in paddy fields.

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