Herbicidal compositions, microcapsule suspensions-suspensions containing isoxaben and terbumeton, and methods of making and using the same

Abstract

The application discloses a herbicidal composition containing isoxaben and terbumeton, a microcapsule suspending-suspension agent and a preparation method and application thereof, and relates to the field of pesticides. Effective components in the herbicidal composition include isoxaben and terbumeton, and the weight ratio of the isoxaben and the terbumeton is (0.1:99)-(99:0.1), optionally (40:1)-(1:40), and optionally (20:1)-(1:30). The composition of the application can improve the control effect, reduce the dosage, reduce the risk of drug damage, and delay the occurrence of drug resistance.

Description

Technical Field

[0001] This invention relates to the field of pesticide technology, and in particular to a herbicidal composition containing isoxaflutole and terbutaline, a microcapsule suspension-suspension agent, its preparation method and application. Background Technology

[0002] Pesticides are mainly divided into herbicides, insecticides, fungicides, and plant growth regulators. Among them, herbicides have the largest market share and the most varieties in the global pesticide market. In certain years and under certain statistical methods, herbicides also account for a considerable proportion of total pesticide sales. Due to the technological barriers in the herbicide industry, a stable global landscape has emerged with six major pesticide companies: Syngenta, Bayer, BASF, Dow, Monsanto, and DuPont. These companies dominate the herbicide market, demonstrating the important position of herbicides in the pesticide industry.

[0003] From an application perspective, weeds compete with crops for soil nutrients, such as nitrogen fertilizer. For example, thistle absorbs 1.5 times more nitrogen fertilizer than grasses, and artemisia absorbs twice as much water as wheat. This can lead to insufficient nutrients, limiting crop growth and consequently affecting yield. The abundant growth of weeds also occupies a large amount of growing space, squeezing out the space for crops. This can reduce photosynthesis, resulting in weak, thin plants with poor grain filling, ultimately impacting yield. For example, wheat yields may decrease by about 30% in fields with abundant weeds, while corn yields may decrease by about 50%. Weeds are not only breeding grounds for pests and diseases but can also act as vectors for their spread. For example, cutworms prefer to lay eggs on field bindweed, so fields with abundant field bindweed have a higher probability of cutworm infestations. This increases the risk of crop damage, further affecting yield. In fields with abundant weeds, agricultural operations such as harvesting and tilling are hindered. For example, if the Gynostemma pentaphyllum in cornfields is not properly controlled, it will affect machine harvesting; wild reeds and paper mulberry shrubs in medicinal herb fields can create significant obstacles to the harvesting of medicinal herbs. All of these factors increase the difficulty and cost of agricultural production, indirectly leading to reduced yields.

[0004] Using herbicides is the most direct, effective, and labor-saving means of weed control. However, with long-term use of herbicides, weed resistance has become increasingly prominent, and resistance levels have been rising year by year. Currently, 267 weed species in 96 crop fields across 72 countries worldwide have developed resistance to herbicides, involving 513 herbicide-resistant biotypes. Even glyphosate, a non-selective broad-spectrum herbicide, has resistant species in 56 weeds globally, including two in my country. Combining herbicides with different mechanisms of action can improve weed control efficacy and reduce the risk of herbicide resistance.

[0005] Therefore, it is particularly important to develop reasonable compound herbicides and apply them rationally.

[0006] Isoxaflutole is a selective pre-emergence herbicide that inhibits carotenoid biosynthesis, with an unknown specific target enzyme. It works by inhibiting the synthesis of pentadiene compounds, thus hindering the biosynthesis of carotene and chlorophyll. After absorption by the roots and shoots of weeds, the herbicide is translocated upwards through the xylem to the leaves, inhibiting pigment synthesis and causing albinism. This prevents the weeds from producing nutrients through photosynthesis, ultimately leading to their death from nutrient depletion. Soybeans have a specific metabolic mechanism that converts it into a weed-free metabolite, resulting in selective herbicide application with moderate soil adhesion. It is primarily biodegraded by microorganisms in the soil. It is more effective in sandy soils under rainy conditions or when temperatures are low and soil moisture is high. Isoxaflutole has a broad spectrum of weed control, effectively controlling a variety of annual grasses and broadleaf weeds.

[0007] After being absorbed by crops such as soybeans and sugarcane, isoxaflutole undergoes a special metabolic process, transforming its active ingredients into non-toxic degradation products, thus ensuring its safety. Isoxaflutole is primarily used to control annual grasses and leafy weeds such as barnyard grass, goosegrass, velvetleaf, burdock, cocklebur, crabgrass, foxtail grass, ragweed, elm, water spinach seedlings, lambsquarters, purslane, willow-leaved knotweed, sorrel-leaved knotweed, purslane, wolfberry, beggar-ticks, and dayflower. It also has a strong inhibitory effect on perennial weeds such as thistle, thistle, sow thistle, and horsetail. It can be used as a pre-sowing or pre-emergence soil treatment in soybean fields, or as an early post-emergence foliar treatment. Isoxaben has a long residual effect; high dosages (more than 53g per acre) not only provide excellent weed control but also significantly promote soybean growth and yield. However, soybeans must be planted the following year, which can negatively impact other crops. Similarly, soybeans exhibit high resistance to isoxaben, making it a highly selective herbicide and a viable option for weed control in soybean fields. It can also be used as a pre-emergence herbicide in sugarcane fields.

[0008] Terbutaline is an inhibitor of photosynthetic electron transport at the photosynthetic system II receptor site. Specifically, its mechanism of action involves inhibiting the Hill reaction in photosynthesis, specifically through the formation of hydrogen bonds between amino or carbonyl oxygen groups and the active sites of chloroplasts. Terbutaline is a systemic soil herbicide with low selectivity, primarily absorbed through the roots and translocated within the plant. It is a broad-spectrum herbicide used to control herbaceous and woody plants (0.6–4.5 kg / hm²), annual weeds (1.3–4.5 kg / hm²), and many perennial and luxuriant weeds (2.2–4.5 kg / hm²). Applications include controlling undesirable woody plants and weeds in non-cultivated vegetation, grasslands, and pastures, as well as grasses and broadleaf weeds in sugarcane fields.

[0009] There are currently no reports of the two being combined. Summary of the Invention

[0010] Purpose of the invention

[0011] To overcome the above-mentioned shortcomings, the present invention aims to provide a herbicidal composition containing isoxaflutole and terbutaline, a microcapsule suspension-suspension agent, a preparation method thereof, and its application. The combination of the composition of the present invention can improve the control effect, reduce the dosage, reduce the risk of phytotoxicity, and delay the occurrence of herbicide resistance.

[0012] Solution

[0013] To achieve the objectives of this invention, the technical solution adopted is as follows:

[0014] In a first aspect, the present invention provides a herbicidal composition containing isoxaflutole and terbutaline, wherein the active ingredients in the herbicidal composition include isoxaflutole and terbutaline, and the weight ratio of isoxaflutole and terbutaline is (0.1:99) to (99:0.1).

[0015] Further, the weight ratio of isoxaflutole and terbutaline is (40:1) to (1:40), optionally (20:1) to (1:30), optionally (10:1) to (1:10), optionally (5:1) to (1:10), optionally (5:1) to (1:5), optionally 20:1, 10:1, 5:1, 1:1, 1:5, 1:10 or 1:20.

[0016] Furthermore, the active ingredient accounts for 1% to 99% of the total weight of the composition, optionally 6% to 80%, optionally 6% to 60%, optionally 30% to 40%.

[0017] Combining two agents within the above range, and using excipients such as solvents, emulsifiers, dispersants, wetting agents, thickeners, fillers, preservatives, antifreeze agents, specific gravity regulators, defoamers, oil-phase wall materials, water-phase wall materials, and water, based on their physicochemical properties, can produce dosage forms such as ZC, WG, WP, DF, EC, EW, and GR.

[0018] Furthermore, the formulation of the herbicidal composition is one or more of the following: microcapsule suspension, emulsifiable concentrate, water emulsion, dry suspension, wettable powder, water-dispersible granules, granules, and seed treatment agent;

[0019] Furthermore, the weeding composition further includes adjuvants, optionally selected from one or more of solvents, emulsifiers, dispersants, wetting agents, thickeners, fillers, preservatives, antifreeze agents, specific gravity regulators, defoamers, oil-phase wall materials, aqueous-phase wall materials, and water.

[0020] Furthermore, the solvent is one or more selected from N,N-dimethylformamide, cyclohexanone, xylene, methylnaphthalene, and solvent oil;

[0021] Furthermore, the emulsifier is one or more of the following: EOPO block polyether emulsifier, calcium dodecylbenzenesulfonate, Tween series, and Span series;

[0022] Furthermore, the dispersant is one or more of polycarboxylate, lignin sulfonate, and naphthalene sulfonate;

[0023] Furthermore, the wetting agent is one or more of sodium dodecyl sulfate and sodium dodecylbenzene sulfonate;

[0024] Furthermore, the thickener is one or more of xanthan gum and magnesium aluminum silicate;

[0025] Furthermore, the filler is one or more of calcined kaolin, bentonite, diatomaceous earth, attapulgite, fumed silica, corn starch, or light calcium carbonate.

[0026] Furthermore, the preservative is isomethylthiazolinone;

[0027] Furthermore, the antifreeze is one or more of ethylene glycol and glycerol;

[0028] Furthermore, the specific gravity regulator is one or more of sodium chloride, calcium chloride, magnesium sulfate, sodium nitrate, potassium chloride, sodium sulfate, and ammonium sulfate; optionally, the specific gravity regulator can also be used as a spray drying aid for DF formulations and a disintegrant for WG formulations.

[0029] Furthermore, the defoamer is an organosilicone emulsion;

[0030] Furthermore, the oil phase wall material is a polyisocyanate; optionally, it is one or more of HDI, IPDI, MDI, and PAPI.

[0031] Further, the aqueous wall material is one or more of polyols and polyamines; optionally, the aqueous wall material is one or more of polyethylene glycol, triethylenetetramine, tetraethylenepentamine, and hexamethylenediamine; optionally, the average molecular weight of the polyethylene glycol is 100-2000, optionally 200-800, optionally 300-500, optionally 300-400; optionally, the polyethylene glycol is PEG400.

[0032] Furthermore, the granular carrier can be selected as coal gangue.

[0033] In a second aspect, a microcapsule suspension-suspension agent comprising the herbicidal composition described in the first aspect is provided, comprising isoxaflutole microcapsule suspension and terbutaline aqueous suspension, optionally wherein the weight ratio of isoxaflutole microcapsule suspension to terbutaline aqueous suspension is (1-3):(2-6).

[0034] Furthermore, the isoxaflutole microcapsule suspension comprises the following raw materials in weight fractions: isoxaflutole 5-60%, solvent 2-20%, oil phase wall material 1-10%, dispersant 1-10%, water 50-70%, aqueous phase wall material 0.2-6.0%, specific gravity adjuster 0-5%, and preservative 0-1%.

[0035] Furthermore, the isoxaflutole microcapsule suspension comprises the following raw materials in weight fractions: isoxaflutole 10-20%, solvent 4-10%, oil phase wall material 1-6%, dispersant 5-10%, water 60-70%, aqueous phase wall material 0.25-4.0%, specific gravity adjuster 3-5%, and preservative 0.1-1%.

[0036] Further optionally, the isoxaflutole microcapsule suspension comprises the following raw materials in weight fractions: 15-20% isoxaflutole, 5-10% solvent, 1-4% oil phase wall material, 5-10% dispersant, 65-70% water, 0.25-4.0% aqueous phase wall material, 3-5% specific gravity adjuster, and 0.1-1% preservative.

[0037] Further optionally, the isoxaflutole microcapsule suspension comprises the following raw materials in weight fractions: 15% isoxaflutole, 5% solvent, 1-4% oil phase wall material, 5% dispersant, 65-70% water, 0.25-4.0% aqueous phase wall material, 3-5% specific gravity adjuster, and 0.1-1% preservative.

[0038] Optionally, the isoxaflutole microcapsule suspension comprises the following raw materials in weight fractions: 15% isoxaflutole, 5% solvent, 2-4% oil phase wall material, 5% dispersant, 65-70% water, 1-4% aqueous phase wall material, 3-5% specific gravity adjuster, and 0.1-1% preservative.

[0039] Optionally, the isoxaflutole microcapsule suspension comprises the following raw materials in weight fractions: 15% isoxaflutole, 5% solvent, 2-4% oil phase wall material, 5% dispersant, 65-70% water, 2-4% aqueous phase wall material, 3-5% specific gravity adjuster, and 0.1-1% preservative.

[0040] Further optionally, the oil phase wall material is a polyisocyanate, optionally one or more of HDI, IPDI, MDI, and PAPI.

[0041] Further optionally, the aqueous wall material is one or more of polyols and polyamines; optionally, the aqueous wall material is one or more of polyethylene glycol, triethylenetetramine, tetraethylenepentamine, and hexamethylenediamine; optionally, the average molecular weight of the polyethylene glycol is 100-2000, optionally 200-800, optionally 300-500, optionally 300-400; optionally, the polyethylene glycol is PEG400.

[0042] Further optionally, the specific gravity adjuster is one or more of sodium chloride, calcium chloride, magnesium sulfate, sodium nitrate, potassium chloride, sodium sulfate, and ammonium sulfate;

[0043] Further optionally, the dispersant is one or more of polycarboxylate, lignin sulfonate, and naphthalene sulfonate; optionally, the dispersant includes polycarboxylate and lignin sulfonate in a weight ratio of (3-6):(2-4);

[0044] Alternatively, the preservative is isomethylthiazolinone.

[0045] Furthermore, the terbutaline aqueous suspension comprises the following raw materials in weight fractions: terbutaline 20-50%, dispersant 5-15%, thickener 0-1%, preservative 0-1%, antifreeze 0-5%, and water 35-50%;

[0046] Further optionally, the terbutaline aqueous suspension comprises the following raw materials in weight fractions: 30-40% terbutaline, 5-15% dispersant, 0-1% thickener, 0-1% preservative, 0-5% antifreeze and 35-50% water;

[0047] Further optionally, the terbutaline aqueous suspension comprises the following raw materials in weight fractions: 35-40% terbutaline, 9-15% dispersant, 0-1% thickener, 0-1% preservative, 0-5% antifreeze and 45-50% water;

[0048] Further optionally, the terbutaline aqueous suspension comprises the following raw materials in weight fractions: 35-40% terbutaline, 9-15% dispersant, 0.1-1% thickener, 0.15-1% preservative, 3-5% antifreeze agent, and 45-50% water;

[0049] Further optionally, the dispersant is one or more of polycarboxylate, lignin sulfonate, and naphthalene sulfonate; optionally, the dispersant comprises polycarboxylate and lignin sulfonate in a weight ratio of (3-9):(2-5); optionally, the dispersant comprises polycarboxylate and lignin sulfonate in a weight ratio of (6-8):(3-4).

[0050] Further optionally, the antifreeze is one or more of ethylene glycol and glycerol;

[0051] Further optionally, the preservative is isomethylthiazolinone;

[0052] Further optionally, the thickener is one or more of xanthan gum and magnesium aluminum silicate.

[0053] Thirdly, a method for preparing the microcapsule suspension / suspension agent described in the first aspect is provided, comprising:

[0054] 1) Preparation of isoxaflutole microcapsule suspension:

[0055] The oil phase is prepared by mixing isoxabar, solvent, and oil-phase wall material.

[0056] The dispersant, thickener, and water are mixed to form the aqueous phase;

[0057] The oil phase is transferred to the aqueous phase and emulsified by high-speed shearing to obtain an emulsion. The aqueous phase wall material is added and stirring is continued. According to the requirements, a specific gravity regulator and / or preservative is added to obtain isoxaflutole microcapsule suspension. Optionally, after adding the aqueous phase wall material, the emulsion is heated to 50-60°C and then a specific gravity regulator and / or preservative is added according to the requirements.

[0058] 2) Preparation of terbutaline aqueous suspension:

[0059] Terbutaline, dispersant, thickener, preservative, antifreeze and water are mixed and wet-milled to the target particle size to obtain terbutaline aqueous suspension.

[0060] 3) Mix the materials from steps 1) and 2) to obtain microcapsule suspension-suspension agent.

[0061] Fourthly, the application of the herbicidal composition described in the first aspect, or the microcapsule suspension-suspension agent described in the second aspect, or the microcapsule suspension-suspension agent prepared by the preparation method described in the third aspect, in the control of weeds in farmland before crop planting, or after sowing and before seedling emergence, or during the crop growth period; optionally, the weeds include broadleaf weeds and / or grass weeds; optionally, the weeds are selected from at least one of crabgrass, goosegrass, and amaranth.

[0062] Beneficial effects

[0063] (1) The combination of the present invention can improve the prevention and control effect, reduce the dosage, reduce the risk of phytotoxicity, and delay the occurrence of drug resistance.

[0064] (2) The advantages of this invention include: ① The raw materials are conventional, making procurement, storage, and use convenient and safe; ② The process is simple and easy to industrialize; ③ The product has small batch-to-batch differences, good stability, and good storage stability; ④ The optimal compound ratio of terbutaline and isoxaflutole has been screened through numerous experiments; ⑤ A stable formulation and product have been obtained through extensive adjuvant screening; ⑥ It has a synergistic effect in weed control, which can improve the efficacy of the pesticide against weeds, reduce the amount of pesticide used, lower costs, and delay the risk of weed resistance. Detailed Implementation

[0065] 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.

[0066] 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.

[0067] 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.

[0068] The above-described herbicidal composition provides a new option for weed control. The following examples further illustrate this disclosure, but this disclosure is not intended to be limiting.

[0069] In the following examples, both terbutaline and isoxaflutole are commercially available, and the other adjuvants are also commercially available products.

[0070] The present invention will be further described in detail below through examples.

[0071] Test Example 1: Indoor Toxicity Determination

[0072] The herbicidal synergistic effect of terbutaline and isoxaflutole was determined using an indoor toxicity assay. The indoor toxicity assay was conducted according to the Sun Yunpei method to determine the co-toxicity coefficient (CTC) of the herbicides when mixed in a certain proportion. A CTC < 80 indicated an antagonistic effect, 80 ≤ CTC ≤ 120 indicated an additive effect, and a CTC > 120 indicated a synergistic effect.

[0073] All test reagents were provided by Shandong Weifang Runfeng Chemical Co., Ltd.

[0074] Experimental Design: After preliminary testing to determine the effective inhibitory concentration range of each pesticide, a series of concentration treatments were set for each pesticide according to the content of its active ingredient, with a water control included. The experiment was conducted in accordance with the "Guidelines for Indoor Bioassay Testing of Pesticides (Herbicides)". Soil spraying was used to determine the inhibitory concentration of the pesticide and its mixtures, and the co-toxicity coefficient was calculated using the method proposed by Sun Yunpei et al. (1960) for calculating combined toxicity.

[0075] The calculation formula is as follows (using terbutaline as the standard agent, with a toxicity index of 100).

[0076] Isoxaflutole Toxicity Index (TI) = Terbutaline ED 50 / Isobarbital ED 50 ×100.

[0077] Actual Toxicity Index (ATI) of M = ED of terbutaline 50 / M of ED 50 ×100.

[0078] Theoretical toxicity index (TTI) of M = Isoxamethasone TI × P 异噁草松 +Texafluthrin TI×P 特丁噻草隆 .

[0079]

[0080] In the formula: M is a mixture of isoxaflutole and terbutaline in different proportions;

[0081] P 异噁草松 The percentage of isoxaflutole in the compound composition;

[0082] P 特丁噻草隆 This refers to the proportion of terbutaline in the compound composition.

[0083] The experimental results are shown in Table 1:

[0084] Table 1. Toxicity test results of isoxaflutole and terbutaline combined with amaranth.

[0085]

[0086]

[0087] Table 1 shows that isoxaflutole and terbutaline have different effects on the ED of Amaranthus retroflexus. 50The concentrations were 48.45 mg / L and 191.85 mg / L, respectively. When the mass ratio of isoxaflutole to terbutaline was (40:1) to (1:40), an additive effect was observed. Preferably, the co-toxicity coefficient was greater than 120 at (20:1) to (1:30), showing a significant synergistic effect. More preferably, the mass ratio was (10:1) to (1:10), and more preferably (5:1) to (1:5). Synergistic effects were also observed at 20:1, 10:1, 5:1, 1:1, 1:5, 1:10, and 1:20. Among these, the synergistic effect was most pronounced when the mass ratio of isoxaflutole to terbutaline was 1:5.

[0088] Preparation Examples

[0089] 1. Emulsifiable concentrate

[0090] Example 1 (40% isoxaflutole + 1% terbutaline) EC (mass ratio 40:1)

[0091] Take 41.67% of isoxaflutole technical grade (96% isoxaflutole content) and 1.04% of terbutaline technical grade (96% terbutaline content), add 6% EOPO block polyether emulsifier and 5% calcium dodecylbenzenesulfonate as emulsifiers, add 10% cyclohexanone as a co-solvent, and make up the solvent oil to 100%, then stir evenly. This yields a (40% isoxaflutole + 1% terbutaline) emulsifiable concentrate.

[0092] Example 2 (5% isoxaflutole + 1% terbutaline) EC (mass ratio 5:1)

[0093] Take 5.21% of isoxaflutole technical grade (96% isoxaflutole content) and 1.04% of terbutaline technical grade (96% terbutaline content), add 6% Tween-80 and 4% Span-80 as emulsifiers, add 20% N,N-dimethylformamide as a co-solvent, and make up the volume to 100% with xylene, and stir well to obtain (5% isoxaflutole + 1% terbutaline) emulsifiable concentrate.

[0094] 2. Water-based emulsion

[0095] Example 3 (1% isoxaflutole + 1% terbutaline) water-in-oil emulsion (mass ratio 1:1)

[0096] 1) Oil phase preparation

[0097] Take 1.04% of isoxaflutole technical grade (96% isoxaflutole content) and 1.04% of terbutaline technical grade (96% terbutaline content), add 4% EOPO block polyether emulsifier and 4% calcium dodecylbenzenesulfonate as emulsifiers, add 10% cyclohexanone as a co-solvent, and add solvent oil to make up to 40% and stir evenly to form the oil phase.

[0098] 2) EW preparation

[0099] Prepare 60% water as the aqueous phase, transfer the prepared oil phase into the aqueous phase and shear and disperse evenly to obtain (1% isoxaflutole + 1% terbutaline) emulsion.

[0100] 3. Granules

[0101] Example 4 (1% isoxaflutole + 5% terbutaline) granules (mass ratio 1:5)

[0102] Take 1.04% of isoxaflutole technical grade (96% isoxaflutole content) and 5.21% of terbutaline technical grade (96% terbutaline content), and dissolve them completely with N,N-dimethylformamide. Mix the solution with 93.75% coal gangue and dry to obtain (1% isoxaflutole + 5% terbutaline) granules.

[0103] 4. Dry suspension

[0104] Example 5 (30% isoxaflutole + 30% terbutaline) dry suspension (mass ratio 1:1)

[0105] (I) Preparation of 30% isoxaflutole microcapsule suspension

[0106] 31.25% isoxaflutole technical grade (96% isoxaflutole content) was dissolved in 5.35% solvent oil 100#, then 3% MDI was added and mixed evenly to form the oil phase; 7% polycarboxylate and 50% water were mixed evenly under shear homogenization conditions to form the aqueous phase; the oil phase was transferred to the aqueous phase, and an emulsion was obtained by shearing using a high-speed shear emulsifier, then 0.4% hexamethylenediamine was slowly added and stirred continuously; under continuous stirring, the emulsion was heated to 55℃, and the system was kept at this temperature for 4 hours, then 3% calcium chloride was added; finally, after keeping it at this temperature for a certain period of time, it was cooled to 20-25℃, and the 30% isoxaflutole microcapsule suspension was prepared.

[0107] (II) Preparation of 30% Terbutaline Aqueous Suspension

[0108] 31.25% terbutaline technical grade (96% terbutaline content), 8.42% polycarboxylate, 10% lignin sulfonate, and 50% water were added to the preparation apparatus and dispersed evenly. The material system was then ground using a wet grinding process to the target particle size, yielding a 30% terbutaline aqueous suspension. The 30% terbutaline aqueous suspension was filtered and stored in a transfer container for later use.

[0109] (III) Mixed isoxaflutole (15% isoxaflutole + 15% terbutaline) microcapsule suspension - suspension concentrate

[0110] The previously prepared 30% isoxaflutole microcapsule suspension and 30% terbutaline aqueous suspension were mixed in a 1:1 ratio and stirred evenly to obtain (15% isoxaflutole + 15% terbutaline) microcapsule suspension-suspension, which is a slurry with a solid content of 50%.

[0111] (iv) Preparation of (30% isoxaflutole + 30% terbutaline) dry suspension

[0112] After spray drying the microcapsule suspension of (15% isoxaflutole + 15% terbutaline) (50% water content), a dry suspension of (30% isoxaflutole + 30% terbutaline) is obtained.

[0113] 5. Wettable powder

[0114] Example 6 (10% isoxaflutole + 40% terbutaline) wettable powder (mass ratio 1:4)

[0115] (I) Preparation of 20% isoxaflutole microcapsule suspension

[0116] 20.83% isoxaflutole technical grade (96% isoxaflutole content) was dissolved in 5.35% xylene, and then 2% PAPI was added and mixed evenly to form the oil phase. 6% polycarboxylate and 60% water were mixed evenly under shear homogenization conditions to form the aqueous phase. The oil phase was transferred to the aqueous phase, and an emulsion was obtained by shearing using a high-speed shear emulsifier. Then, 0.2% hexamethylenediamine was slowly added while stirring continuously. Under continuous stirring, the emulsion was heated to 55°C, and the system was kept at this temperature for 4 hours. Then, 4% calcium chloride was added. Finally, the temperature was kept at this temperature for a certain period of time and then cooled to 20-25°C. The 30% isoxaflutole microcapsule suspension was thus prepared.

[0117] (II) Preparation of 50% isoxaflutole microcapsule dry suspension

[0118] Spray-dry 20% isoxaflutole microcapsule suspension to obtain 50% isoxaflutole microcapsule dry suspension for later use.

[0119] (III) Preparation of 50% Terbutaline Wettable Powder

[0120] Take 52.08% of terbutaline technical grade (of which terbutaline content is 96%), 4% polycarboxylate, 4% lignin sulfonate, 2% naphthalene sulfonate, 2% sodium dodecylbenzene sulfonate, and calcined kaolin to make up to 100%, mix them, and then pulverize them by air jet to obtain 50% terbutaline wettable powder.

[0121] (IV) Preparation of (10% isoxaflutole + 40% terbutaline) wettable powder

[0122] The previously prepared 50% isoxaflutole microcapsule dry suspension and 50% terbutaline wettable powder were mixed in a 1:4 ratio and stirred evenly to obtain (10% isoxaflutole + 40% terbutaline) wettable powder.

[0123] Example 7 (1% isoxaflutole + 40% terbutaline) wettable powder (mass ratio 1:40)

[0124] 1.04% isoxaflutole technical grade (96% isoxaflutole content) was adsorbed and melted using 2% fumed silica and used as isoxaflutole masterbatch. The previously mixed isoxaflutole masterbatch and 41.67% terbutaline technical grade (96% terbutaline content) were added to a mixer, along with 5% polycarboxylate, 2% lignin sulfonate, 4% naphthalene sulfonate, 3% sodium dodecylbenzene sulfonate, and bentonite to make up to 100%. After mixing, the mixture was pulverized by air jet milling and collected to obtain a wettable powder of (1% isoxaflutole + 40% terbutaline).

[0125] 6. Water-dispersible granules

[0126] Example 8 (3% isoxaflutole + 76% terbutaline) water-dispersible granules (mass ratio 3:76)

[0127] 3% fumed silica was used to adsorb and melt 3.125% isoxaflutole technical grade (96% isoxaflutole content) as isoxaflutole masterbatch. The previously mixed isoxaflutole masterbatch, 80.20% terbutaline technical grade (96% terbutaline content), 4% lignin sulfonate, 3% naphthalene sulfonate, 1% sodium dodecylbenzene sulfonate, 0.2% defoamer (mixed into the granulation solution), and polycarboxylate dispersant were added to make up to 100%. After mixing, the mixture was air-jet pulverized to obtain a fine powder of 3% isoxaflutole + 76% terbutaline. 20% water was added by weight of the fine powder to form a granulation solution, and the mixture was mixed to form a wet material. The wet material was granulated by extrusion, and after drying, a water-dispersible granule of (3% isoxaflutole + 76% terbutaline) was obtained.

[0128] 7. Microcapsule suspension - suspending agent

[0129] Example 9 (30% isoxaflutole + 1.5% terbutaline) microcapsule suspension-suspension concentrate (mass ratio 30:1.5)

[0130] (I) Preparation of 35% isoxaflutole microcapsule suspension

[0131] Dissolve 36.46% isoxaflutole technical grade (96% isoxaflutole content) in 4.5% solvent oil, then add 3.5% MDI and mix thoroughly to form the oil phase. Mix 5% polycarboxylate, 0.05% xanthan gum, and 46.04% water under shear homogenization conditions to form the aqueous phase. Transfer the oil phase to the aqueous phase and shear using a high-speed shear emulsifier to obtain an emulsion. Slowly add 0.35% hexamethylenediamine while continuously stirring. Heat the emulsion to 55°C while continuously stirring, and maintain the temperature for 4 hours. Then add 4% calcium chloride and 0.1% methylisothiazolinone, and continue stirring for 0.5 hours. Finally, maintain the temperature for a certain period and then cool to 20-25°C. The 35% isoxaflutole microcapsule suspension is now ready. Discharge and set aside.

[0132] (II) Preparation of 10.5% Terbuthylazine Aqueous Suspension

[0133] 10.94% terbutaline technical grade (96% terbutaline content), 4% polycarboxylate, 0.2% xanthan gum, 0.10% methylisothiazolinone, 3% ethylene glycol, and 81.76% water were added to the preparation apparatus and dispersed evenly. The material system was then ground using a wet grinding process to the target particle size, yielding a 10.5% terbutaline aqueous suspension. The 10.5% terbutaline aqueous suspension was filtered and stored in a transfer container for later use.

[0134] (III) Mixed (30% isoxaflutole + 1.5% terbutaline) microcapsule suspension - suspension concentrate

[0135] The previously prepared 35% isoxaflutole microcapsule suspension and 10.5% terbutaline aqueous suspension were mixed in a ratio of 85.71:14.29 and stirred evenly to obtain (30% isoxaflutole + 1.5% terbutaline) microcapsule suspension-suspension.

[0136] Example 10 (25% isoxaflutole + 5% terbutaline) microcapsule suspension-suspension (mass ratio 5:1)

[0137] (I) Preparation of 40% isoxaflutole microcapsule suspension

[0138] 41.67% isoxaflutole technical grade (96% isoxaflutole content) was dissolved in 4% xylene, then 4% IPDI was added and mixed thoroughly to form the oil phase. 6% polycarboxylate, 0.05% xanthan gum, and 38.88% water were mixed thoroughly under shear homogenization conditions to form the aqueous phase. The oil phase was transferred to the aqueous phase, and an emulsion was obtained using a high-speed shear emulsifier. Then, 0.3% hexamethylenediamine was slowly added with continuous stirring. The emulsion was heated to 55°C with continuous stirring and kept at this temperature for 4 hours. Then, 5% calcium chloride and 0.1% methylisothiazolinone were added, and stirring continued for 0.5 hours. Finally, the temperature was maintained for a certain period and then lowered to 20-25°C. The 40% isoxaflutole microcapsule suspension was then prepared. The material was discharged and set aside for later use.

[0139] (II) Preparation of 13.33% Terbutaline Aqueous Suspension

[0140] 13.89% terbutaline technical grade (96% terbutaline content), 3% polycarboxylate, 2% sodium lignosulfonate, 1% sodium dodecyl sulfate, 0.05% xanthan gum, 0.1% methylisothiazolinone, 2% ethylene glycol, and 77.96% water were added to a preparation apparatus and dispersed evenly. The material system was then ground using a wet grinding process to the target particle size, yielding a 13.3% terbutaline aqueous suspension.

[0141] (III) Mixed (25% isoxaflutole + 5% terbutaline) microcapsule suspension - suspension concentrate

[0142] The previously prepared 40% isoxaflutole microcapsule suspension and 13.33% terbutaline aqueous suspension were mixed in a ratio of 62.5:37.5 and stirred evenly to obtain (25% isoxaflutole + 5% terbutaline) microcapsule suspension-suspension.

[0143] Example 11 (15% isoxaflutole + 15% terbutaline) microcapsule suspension-suspension concentrate (mass ratio 1:1)

[0144] (I) Preparation of 30% isoxaflutole microcapsule suspension

[0145] 31.25% isoxaflutole technical grade (96% isoxaflutole content) was dissolved in 5% solvent oil, then 3% MDI was added and mixed thoroughly to form the oil phase. 4% polycarboxylate, 0.1% xanthan gum, and 53.05% water were mixed thoroughly under shear homogenization conditions to form the aqueous phase. The oil phase was transferred to the aqueous phase, and an emulsion was obtained using a high-speed shear emulsifier. Then, 0.4% hexamethylenediamine was slowly added with continuous stirring. The emulsion was heated to 55°C with continuous stirring and kept at this temperature for 4 hours. Then, 3% calcium chloride and 0.2% methylisothiazolinone were added, and stirring continued for 0.5 hours. Finally, the temperature was maintained for a certain period and then lowered to 20-25°C. The 30% isoxaflutole microcapsule suspension was then prepared. The material was discharged and set aside for later use.

[0146] (II) Preparation of 30% Terbutaline Aqueous Suspension

[0147] 31.25% of terbutaline technical grade (96% terbutaline content), 4% polycarboxylate, 0.1% xanthan gum, 0.2% methylisothiazolinone, 3% ethylene glycol, and 61.45% water were added to the preparation apparatus and dispersed evenly. The material system was then ground using a wet grinding process to the target particle size to obtain a 30% terbutaline aqueous suspension. The 30% terbutaline aqueous suspension was filtered and stored in a transfer container for later use.

[0148] (III) Mixed isoxaflutole (15% isoxaflutole + 15% terbutaline) microcapsule suspension - suspension concentrate

[0149] The previously prepared 30% isoxaflutole microcapsule suspension and 30% terbutaline aqueous suspension were mixed in a 1:1 ratio and stirred evenly to obtain (15% isoxaflutole + 15% terbutaline) microcapsule suspension-suspension.

[0150] Example 12 (5% isoxaflutole + 25% terbutaline) microcapsule suspension-suspension (mass ratio 1:5)

[0151] (I) Preparation of 15% isoxaflutole microcapsule suspension

[0152] 15.62% isoxaflutole technical grade (96% isoxaflutole content) was dissolved in 5% xylene, then 2% HDI was added and mixed thoroughly to form the oil phase. 3% polycarboxylate, 2% sodium lignosulfonate, 0.1% xanthan gum, and 68.93% water were mixed thoroughly under shear homogenization conditions to form the aqueous phase. The oil phase was transferred to the aqueous phase, and an emulsion was obtained using a high-speed shear emulsifier. Then, 0.25% tetraethylenepentamine was slowly added while stirring continuously. The emulsion was heated to 55°C under continuous stirring and kept at this temperature for 4 hours. Then, 3% calcium chloride and 0.1% methylisothiazolinone were added, and stirring continued for 0.5 hours. Finally, the temperature was maintained for a certain period and then lowered to 20-25°C. The 15% isoxaflutole microcapsule suspension was then prepared. The material was discharged and set aside for later use.

[0153] (II) Preparation of 37.5% Terbutaline Aqueous Suspension

[0154] 39.06% terbutaline technical grade (96% terbutaline content), 6% polycarboxylate, 3% sodium lignosulfonate, 0.1% xanthan gum, 0.15% methylisothiazolinone, 3% ethylene glycol, and 48.69% water were added to a preparation apparatus and dispersed evenly. The material system was then ground using a wet grinding process to the target particle size, yielding a 37.5% terbutaline aqueous suspension. The 37.5% terbutaline aqueous suspension was filtered and stored in a transfer container for later use.

[0155] (III) Mixed isoxaflutole (5% isoxaflutole + 25% terbutaline) microcapsule suspension - suspension concentrate

[0156] I. Mix the previously prepared 15% isoxaflutole microcapsule suspension and 37.5% terbutaline aqueous suspension at a ratio of 1:2 and stir evenly to obtain (5% isoxaflutole + 25% terbutaline) microcapsule suspension-suspension.

[0157] Example 13 (3% isoxaflutole + 30% terbutaline) microcapsule suspension-suspension (mass ratio 1:10)

[0158] (I) Preparation of 15% isoxaflutole microcapsule suspension

[0159] 15.62% isoxaflutole technical grade (96% isoxaflutole content) was dissolved in 5% xylene, then 2% HDI was added and mixed thoroughly to form the oil phase. 3% polycarboxylate, 2% sodium lignosulfonate, 0.1% xanthan gum, and 68.93% water were mixed thoroughly under shear homogenization conditions to form the aqueous phase. The oil phase was transferred to the aqueous phase, and an emulsion was obtained using a high-speed shear emulsifier. Then, 0.25% tetraethylenepentamine was slowly added while stirring continuously. Under continuous stirring, the emulsion was heated to 55°C and kept at this temperature for 4 hours. Then, 3% calcium chloride and 0.1% methylisothiazolinone were added, and stirring continued for 0.5 hours. Finally, after maintaining the temperature for a certain period, the temperature was lowered to 20-25°C. The 15% isoxaflutole microcapsule suspension was thus prepared. The material was discharged and set aside for later use.

[0160] (II) Preparation of 37.5% Terbutaline Aqueous Suspension

[0161] 39.06% terbutaline technical grade (96% terbutaline content), 6% polycarboxylate, 3% sodium lignosulfonate, 0.1% xanthan gum, 0.15% methylisothiazolinone, 3% ethylene glycol, and 48.69% water were added to a preparation apparatus and dispersed evenly. The material system was then ground using a wet grinding process to the target particle size, yielding a 37.5% terbutaline aqueous suspension. The 37.5% terbutaline aqueous suspension was filtered and stored in a transfer container for later use.

[0162] (III) Mixed isoxaflutole (3% isoxaflutole + 30% terbutaline) microcapsule suspension - suspension concentrate

[0163] I. Mix the previously prepared 15% isoxaflutole microcapsule suspension and 37.5% terbutaline aqueous suspension at a ratio of 1:4 and stir evenly to obtain (3% isoxaflutole + 30% terbutaline) microcapsule suspension-suspension.

[0164] Example 14 (1% isoxaflutole + 30% terbutaline) microcapsule suspension-suspension (mass ratio 1:30)

[0165] (I) Preparation of 5% isoxaflutole microcapsule suspension

[0166] 5.21% isoxaflutole technical grade (96% isoxaflutole content) was dissolved in 5% solvent oil, then 0.4% IPDI was added and mixed thoroughly to form the oil phase. 3% polycarboxylate, 1% sodium lignosulfonate, 0.1% xanthan gum, and 81.99% water were mixed thoroughly under shear homogenization conditions to form the aqueous phase. The oil phase was transferred to the aqueous phase, and an emulsion was obtained using a high-speed shear emulsifier. Then, 0.1% triethylenetetramine was slowly added with continuous stirring. While continuously stirring, the emulsion was heated to 55°C and kept at this temperature for 4 hours. Then, 3% calcium chloride and 0.2% methylisothiazolinone were added, and stirring continued for 0.5 hours. Finally, after maintaining the temperature for a certain period, it was cooled to 20-25°C. The 5% isoxaflutole microcapsule suspension was then prepared and stored for later use.

[0167] (II) Preparation of 37.5% Terbutaline Aqueous Suspension

[0168] 39.06% terbutaline technical grade (96% terbutaline content), 4% polycarboxylate, 4% sodium lignosulfonate, 1% sodium dodecylbenzenesulfonate, 0.1% xanthan gum, 0.15% methylisothiazolinone, 3% ethylene glycol, and 48.69% water were added to a preparation apparatus and dispersed evenly. The material system was then ground using a wet grinding process to the target particle size, yielding a 37.5% terbutaline aqueous suspension. The 37.5% terbutaline aqueous suspension was filtered and stored in a transfer container for later use.

[0169] (III) Mixed isoxaflutole (1% isoxaflutole + 30% terbutaline) microcapsule suspension - suspension concentrate

[0170] I. Mix the previously prepared 5% isoxaflutole microcapsule suspension and 37.5% terbutaline aqueous suspension at a ratio of 1:4 and stir evenly to obtain (5% isoxaflutole + 30% terbutaline) microcapsule suspension-suspension.

[0171] Example 15 (5% isoxaflutole + 25% terbutaline) microcapsule suspension-suspension concentrate (mass ratio 1:5)

[0172] (I) Preparation of 15% isoxaflutole microcapsule suspension

[0173] 15.62% isoxaflutole technical grade (96% isoxaflutole content) was dissolved in 5% xylene, then 2% HDI was added and mixed thoroughly to form the oil phase. 3% polycarboxylate, 2% sodium lignosulfonate, 0.1% xanthan gum, and 67.18% water were mixed thoroughly under shear homogenization conditions to form the aqueous phase. The oil phase was transferred to the aqueous phase, and an emulsion was obtained using a high-speed shear emulsifier. 2% PEG 400 was then slowly added with continuous stirring. The emulsion was heated to 55°C with continuous stirring and kept at this temperature for 4 hours. Then, 3% calcium chloride and 0.1% methylisothiazolinone were added, and stirring continued for 0.5 hours. Finally, the temperature was maintained for a certain period and then lowered to 20-25°C. The 15% isoxaflutole microcapsule suspension was then prepared and stored for later use.

[0174] (II) Preparation of 37.5% Terbutaline Aqueous Suspension

[0175] 39.06% terbutaline technical grade (96% terbutaline content), 6% polycarboxylate, 3% sodium lignosulfonate, 0.1% xanthan gum, 0.15% methylisothiazolinone, 3% ethylene glycol, and 48.69% water were added to a preparation apparatus and dispersed evenly. The material system was then ground using a wet grinding process to the target particle size, yielding a 37.5% terbutaline aqueous suspension. The 37.5% terbutaline aqueous suspension was filtered and stored in a transfer container for later use.

[0176] (III) Mixed isoxaflutole (5% isoxaflutole + 25% terbutaline) microcapsule suspension - suspension concentrate

[0177] I. Mix the previously prepared 15% isoxaflutole microcapsule suspension and 37.5% terbutaline aqueous suspension at a ratio of 1:2 and stir evenly to obtain (5% isoxaflutole + 25% terbutaline) microcapsule suspension-suspension.

[0178] Example 16 (5% isoxaflutole + 25% terbutaline) microcapsule suspension-suspension (mass ratio 1:5)

[0179] (I) Preparation of 15% isoxaflutole microcapsule suspension

[0180] 15.62% isoxaflutole technical grade (96% isoxaflutole content) was dissolved in 5% xylene, then 1% HDI was added and mixed thoroughly to form the oil phase. 3% polycarboxylate, 2% sodium lignosulfonate, 0.1% xanthan gum, and 69.18% water were mixed thoroughly under shear homogenization conditions to form the aqueous phase. The oil phase was transferred to the aqueous phase, and an emulsion was obtained using a high-speed shear emulsifier. 1% PEG 400 was then slowly added with continuous stirring. The emulsion was heated to 55°C with continuous stirring and kept at this temperature for 4 hours. Then, 3% calcium chloride and 0.1% methylisothiazolinone were added, and stirring continued for 0.5 hours. Finally, the temperature was maintained for a certain period and then lowered to 20-25°C. The 15% isoxaflutole microcapsule suspension was then prepared and stored for later use.

[0181] (II) Preparation of 37.5% Terbutaline Aqueous Suspension

[0182] 39.06% terbutaline technical grade (96% terbutaline content), 6% polycarboxylate, 3% sodium lignosulfonate, 0.1% xanthan gum, 0.15% methylisothiazolinone, 3% ethylene glycol, and 48.69% water were added to a preparation apparatus and dispersed evenly. The material system was then ground using a wet grinding process to the target particle size, yielding a 37.5% terbutaline aqueous suspension. The 37.5% terbutaline aqueous suspension was filtered and stored in a transfer container for later use.

[0183] (III) Mixed isoxaflutole (5% isoxaflutole + 25% terbutaline) microcapsule suspension - suspension concentrate

[0184] I. Mix the previously prepared 15% isoxaflutole microcapsule suspension and 37.5% terbutaline aqueous suspension at a ratio of 1:2 and stir evenly to obtain (5% isoxaflutole + 25% terbutaline) microcapsule suspension-suspension.

[0185] Example 17 (5% isoxaflutole + 25% terbutaline) microcapsule suspension-suspension (mass ratio 1:5)

[0186] (I) Preparation of 15% isoxaflutole microcapsule suspension

[0187] 15.62% isoxaflutole technical grade (96% isoxaflutole content) was dissolved in 5% xylene, then 3% HDI was added and mixed thoroughly to form the oil phase. 3% polycarboxylate, 2% sodium lignosulfonate, 0.1% xanthan gum, and 65.18% water were mixed thoroughly under shear homogenization conditions to form the aqueous phase. The oil phase was transferred to the aqueous phase, and an emulsion was obtained using a high-speed shear emulsifier. 3% PEG 400 was then slowly added with continuous stirring. The emulsion was heated to 55°C with continuous stirring and kept at this temperature for 4 hours. Then, 3% calcium chloride and 0.1% methylisothiazolinone were added, and stirring continued for 0.5 hours. Finally, the temperature was maintained for a certain period and then lowered to 20-25°C. The 15% isoxaflutole microcapsule suspension was then prepared and stored for later use.

[0188] (II) Preparation of 37.5% Terbutaline Aqueous Suspension

[0189] 39.06% terbutaline technical grade (96% terbutaline content), 6% polycarboxylate, 3% sodium lignosulfonate, 0.1% xanthan gum, 0.15% methylisothiazolinone, 3% ethylene glycol, and 48.69% water were added to a preparation apparatus and dispersed evenly. The material system was then ground using a wet grinding process to the target particle size, yielding a 37.5% terbutaline aqueous suspension. The 37.5% terbutaline aqueous suspension was filtered and stored in a transfer container for later use.

[0190] (III) Mixed isoxaflutole (5% isoxaflutole + 25% terbutaline) microcapsule suspension - suspension concentrate

[0191] I. Mix the previously prepared 15% isoxaflutole microcapsule suspension and 37.5% terbutaline aqueous suspension at a ratio of 1:2 and stir evenly to obtain (5% isoxaflutole + 25% terbutaline) microcapsule suspension-suspension.

[0192] Example 18 (5% isoxaflutole + 25% terbutaline) microcapsule suspension-suspension (mass ratio 1:5)

[0193] (I) Preparation of 15% isoxaflutole microcapsule suspension

[0194] 15.62% isoxaflutole technical grade (96% isoxaflutole content) was dissolved in 5% xylene, then 4% HDI was added and mixed thoroughly to form the oil phase. 3% polycarboxylate, 2% sodium lignosulfonate, 0.1% xanthan gum, and 63.18% water were mixed thoroughly under shear homogenization conditions to form the aqueous phase. The oil phase was transferred to the aqueous phase, and an emulsion was obtained using a high-speed shear emulsifier. 4% PEG 400 was then slowly added with continuous stirring. The emulsion was heated to 55°C with continuous stirring and kept at this temperature for 4 hours. Then, 3% calcium chloride and 0.1% methylisothiazolinone were added, and stirring continued for 0.5 hours. Finally, the temperature was maintained for a certain period and then lowered to 20-25°C. The 15% isoxaflutole microcapsule suspension was then prepared. The material was discharged and set aside for later use.

[0195] (II) Preparation of 37.5% Terbutaline Aqueous Suspension

[0196] 39.06% terbutaline technical grade (96% terbutaline content), 6% polycarboxylate, 3% sodium lignosulfonate, 0.1% xanthan gum, 0.15% methylisothiazolinone, 3% ethylene glycol, and 48.69% water were added to a preparation apparatus and dispersed evenly. The material system was then ground using a wet grinding process to the target particle size, yielding a 37.5% terbutaline aqueous suspension. The 37.5% terbutaline aqueous suspension was filtered and stored in a transfer container for later use.

[0197] (III) Mixed isoxaflutole (5% isoxaflutole + 25% terbutaline) microcapsule suspension - suspension concentrate

[0198] I. Mix the previously prepared 15% isoxaflutole microcapsule suspension and 37.5% terbutaline aqueous suspension at a ratio of 1:2 and stir evenly to obtain (5% isoxaflutole + 25% terbutaline) microcapsule suspension-suspension.

[0199] Field trial example: Herbal efficacy test of annual weeds in sugarcane fields

[0200] This experiment was conducted in a sugarcane field on the outskirts of Yongning District, Nanning City, Guangxi Zhuang Autonomous Region. The terrain was flat, the land was level, irrigation and drainage facilities were complete, field management was consistent, and fertility was uniform and moderate. The main weeds in the experimental field were goosegrass, crabgrass, lambsquarters, and amaranth. There was no rainfall during the experiment, which was conducted in spring, from March to April.

[0201] A total of 21 treatments were set up, namely: Treatment 1: water spray, blank control; Treatment 2: Example 1; Treatment 3: Example 2; Treatment 4: Example 3; Treatment 5: Example 4; Treatment 6: Example 5; Treatment 7: Example 6; Treatment 8: Example 7; Treatment 9: Example 8; Treatment 10: Example 9; Treatment 11: Example 10; Treatment 12: Example 11; Treatment 13: Example 12; Treatment 14: Example 13; Treatment 15: Example 14; Treatment 16: Example 15; Treatment 17: Example 16; Treatment 18: Example 17; Treatment 19: Example 18; Treatment 20: 360 g / L isoxaflutole microcapsule suspension (commercially available); Treatment 21: 46% terbutaline aqueous suspension (commercially available).

[0202] The recommended dosage of isoxaflutole is 300g per hectare of active ingredient, and the recommended dosage of terbutaline is 1500g per hectare of active ingredient. The dosages in this embodiment are calculated according to the following formula:

[0203] Dosage of M (gai·hm) -2 = Recommended dosage of isoxaflutole (gai·hm) -2 )×P 异噁草松 +Recommended dosage of terbutaline (gai·hm) -2 )×P 特丁噻草隆 .

[0204] Among them, P 异噁草松 P 特丁噻草隆 P represents the proportion of isoxaflutole and terbutaline in the compound composition of the active ingredients. 异噁草松 +P 特丁噻草隆 =100%.

[0205] The pesticide was applied once using a Gongnong-16 backpack manual sprayer, with the dosage of the formulation diluted in 450L of water per hectare, and sprayed evenly. The weather was favorable during the trial, with an average daily temperature of 18-23℃. There was no rain on the day of application and no rainfall for 10 days afterward.

[0206] The weed control efficacy of each treatment was investigated 10, 20 and 30 days after application.

[0207] Methods for visually assessing the effectiveness of weed control:

[0208] Ten, twenty, and thirty days after application, refer to the guidelines for pesticide field efficacy trials (1): herbicide control of sugarcane weeds (GB / T 17980.49-2000). Visually assess the weed coverage of each treated area and its adjacent control area using the estimated value survey method. The results are expressed as a simple percentage (0 for no control effect, 100% for complete weed control). The following grading standards can be used for the survey:

[0209] Level 1: No grass;

[0210] Grade 2: Equivalent to 0-2.5% of the blank control area;

[0211] Grade 3: Equivalent to 2.6%–5% of the empty mortar control area;

[0212] Level 4: Equivalent to 5.1%–10% of the blank control area;

[0213] Level 5: Equivalent to 10.1%–15% of the blank control area;

[0214] Level 6: Equivalent to 15.1% to 25% of the area under aerial solar contrast;

[0215] Level 7: Equivalent to 25.1%–35% of the blank control area;

[0216] Level 8: Equivalent to 35.1%–67.5% of the blank control area;

[0217] Level 9: Equivalent to 67.6%–100% of the blank control area.

[0218] The formula for calculating the protective effect is as follows:

[0219] Efficacy (%) = (10 - Treatment grade) / 9 × 100%

[0220] The visual efficacy was measured 10, 20 and 30 days after application, as shown in Table 2.

[0221] Table 2. Results of visual efficacy tests on annual weeds of each treatment at 10, 20, and 30 days.

[0222]

[0223]

[0224] On day 30, at the end of the experiment, four points were randomly selected from each cell, each 0.25m away. 2 Weeds were removed, and their fresh weight was measured. The weed control efficacy was calculated based on the fresh weight of the weeds.

[0225]

[0226] The 30-day fresh weight efficacy results are shown in Table 3.

[0227] Table 3 shows the efficacy of each treatment on the fresh weight of annual weeds after 30 days.

[0228]

[0229]

[0230] The results of the above visual inspection and fresh weight efficacy tests show that: ① Under the same formulation, the combination of isoxaflutole and terbutaline has a good control effect on annual weeds. Example 15 (isoxaflutole: terbutaline = 1:5) showed the highest efficacy, followed by Example 18 (isoxaflutole: terbutaline = 1:5), Example 17 (isoxaflutole: terbutaline = 1:5), Example 16 (isoxaflutole: terbutaline = 1:5), and Example 12 (isoxaflutole: terbutaline = 1:5). This is superior to other examples, such as Example 1 (isoxaflutole: terbutaline = 40:1) and Example 9 (isoxaflutole: terbutaline = 20:1). Examples 10 (isoxamethonium: terbutaline = 5:1), 11 (isoxamethonium: terbutaline = 1:1), 6 (isoxamethonium: terbutaline = 1:4), 13 (isoxamethonium: terbutaline = 1:10), 8 (isoxamethonium: terbutaline = 3:76), 14 (isoxamethonium: terbutaline = 1:30), and 7 (isoxamethonium: terbutaline = 1:40) demonstrate that a reasonable ratio exhibits a synergistic effect. The efficacy comparison between the examples and single-agent applications shows that a ratio range of 40:1 to 1:40 has a synergistic effect in controlling annual weeds when applied in the field. ② Regarding formulation, visual data analysis showed that 10 days after application, the differences between treatments were not significant, with the control examples slightly outperforming the control examples. This was likely because the weeds were in their initial growth and germination stages, resulting in minimal differences and less noticeable treatment effects. However, over time, under the same ratios, for example, microcapsule suspensions compared to other formulations (e.g., Example 10 vs. Example 2 (isoxamethonium: terbutaline = 5:1), Example 11 vs. Example 3 (isoxamethonium: terbutaline = 1:1), and Example 12 vs. Example 4 (isoxamethonium: terbutaline = 1:5) showed superior visual efficacy after 20 days, with the advantage becoming more pronounced after 30 days. This indicates that microcapsule suspensions, due to their unique slow-release and dispersion effects, are more effective than other formulations in field application, have a longer duration of action, and can achieve long-term control with a single application, reducing pesticide dosage and labor input. ③ In the experiment, we found that compared with Example 12, which had the same formulation and ratio, Example 15 had better control efficacy than Example 12. The reason is that Example 15 used polyol (PEG 400) as the aqueous phase wall material, which made the capsule wall more flexible. The flexible capsule wall is more conducive to the continuous and stable release of the active ingredients, and also reduces the leaching of microcapsule particles in the soil, thus increasing the effect of soil sealing in controlling weeds.④ Regarding the dosage of the aqueous wall material, in samples using polyols as the aqueous wall material, lower dosage resulted in higher efficacy and better rapid action at 10 days, but decreased efficacy at 30 days. Increased dosage led to decreased rapid action but improved sustained efficacy. Visual data and fresh weight efficacy at 30 days indicated that the dosage affected efficacy, with 2% showing the best results. Follow-up monitoring of sugarcane growth in each treatment plot revealed no significant abnormalities, demonstrating the high safety and good application effect of the drug combination covered in this invention.

[0231] 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 microcapsule suspension-suspension formulation comprising isoxaflutole and terbutaline, characterized in that, Including isoxaflutole microcapsule suspension and terbutaline aqueous suspension, with a weight ratio of isoxaflutole microcapsule suspension to terbutaline aqueous suspension of (1~3):(2~6); The isoxaflutole microcapsule suspension comprises the following raw materials in weight fractions: isoxaflutole 5-60%, solvent 2-20%, oil phase wall material 1-10%, dispersant 1-10%, water 50-70%, aqueous phase wall material 0.2-6.0%, specific gravity adjuster 0-5%, and preservative 0-1%; the oil phase wall material is one or more of HDI, IPDI, MDI, and PAPI; the aqueous phase wall material is one or more of polyethylene glycol, triethylenetetramine, tetraethylenepentamine, and hexamethylenediamine; wherein the average molecular weight of polyethylene glycol is 200-800; wherein the dispersant comprises polycarboxylate and lignin sulfonate in a weight ratio of (3-6):(2-4); Terbutaline aqueous suspension comprises the following raw materials in weight fractions: terbutaline 20-50%, dispersant 5-15%, thickener 0-1%, preservative 0-1%, antifreeze 0-5%, and water 35-50%; wherein the dispersant comprises polycarboxylate and lignin sulfonate in a weight ratio of (3-9):(2-5); The active ingredients in the herbicidal composition are isoxaflutole and terbutaline, with a weight ratio of isoxaflutole to terbutaline of (20:1) to (1:30).

2. The microcapsule suspension-suspension agent according to claim 1, characterized in that, The isoxaflutole microcapsule suspension comprises the following raw materials in weight fractions: isoxaflutole 10-20%, solvent 4-10%, oil phase wall material 1-6%, dispersant 5-10%, water 60-70%, aqueous phase wall material 0.25-4.0%, specific gravity adjuster 3-5%, and preservative 0.1-1%.

3. The microcapsule suspension-suspension agent according to claim 1, characterized in that, The isoxaflutole microcapsule suspension comprises the following raw materials in the following weight fractions: isoxaflutole 15-20%, solvent 5-10%, oil phase wall material 1-4%, dispersant 5-10%, water 65-70%, aqueous phase wall material 0.25-4.0%, specific gravity adjuster 3-5%, and preservative 0.1-1%.

4. The microcapsule suspension-suspension agent according to claim 1, characterized in that, The isoxaflutole microcapsule suspension comprises the following raw materials in weight fractions: isoxaflutole 15%, solvent 5%, oil phase wall material 1-4%, dispersant 5%, water 65-70%, aqueous phase wall material 0.25-4.0%, specific gravity adjuster 3-5%, and preservative 0.1-1%.

5. The microcapsule suspension-suspension agent according to claim 1, characterized in that, The isoxaflutole microcapsule suspension comprises the following raw materials in the following weight fractions: isoxaflutole 15%, solvent 5%, oil phase wall material 2-4%, dispersant 5%, water 65-70%, aqueous phase wall material 1-4%, specific gravity adjuster 3-5%, and preservative 0.1-1%.

6. The microcapsule suspension-suspension agent according to claim 1, characterized in that, The isoxaflutole microcapsule suspension comprises the following raw materials in the following weight fractions: isoxaflutole 15%, solvent 5%, oil phase wall material 2%, dispersant 5%, water 65-70%, aqueous phase wall material 2-4%, specific gravity adjuster 3-5%, and preservative 0.1-1%.

7. The microcapsule suspension-suspension agent according to claim 1, characterized in that, In isoxaflutole microcapsule suspensions, the average molecular weight of polyethylene glycol is 300-500.

8. The microcapsule suspension-suspension agent according to claim 1, characterized in that, In isoxaflutole microcapsule suspensions, the average molecular weight of polyethylene glycol is 300-400.

9. The microcapsule suspension-suspension agent according to claim 1, characterized in that, In the isoxaflutole microcapsule suspension, the polyethylene glycol is PEG400.

10. The microcapsule suspension-suspension agent according to claim 1, characterized in that, In the isoxaflutole microcapsule suspension, the specific gravity adjuster is one or more of sodium chloride, calcium chloride, magnesium sulfate, sodium nitrate, potassium chloride, sodium sulfate, and ammonium sulfate.

11. The microcapsule suspension-suspension agent according to claim 1, characterized in that, In the isoxaflutole microcapsule suspension, the preservative is isomethylthiazolinone.

12. The microcapsule suspension-suspension agent according to claim 1, characterized in that, In the isoxaflutole microcapsule suspension, the solvent is one or more of N,N-dimethylformamide, cyclohexanone, xylene, methylnaphthalene, and solvent oil.

13. The microcapsule suspension-suspension agent according to claim 1, characterized in that, Terbutaline aqueous suspension comprises the following raw materials in weight fractions: terbutaline 20-50%, dispersant 5-15%, thickener 0-1%, preservative 0-1%, antifreeze 0-5%, and water 35-50%.

14. The microcapsule suspension-suspension agent according to claim 1, characterized in that, Terbutaline aqueous suspension comprises the following raw materials in weight fractions: terbutaline 30-40%, dispersant 5-15%, thickener 0-1%, preservative 0-1%, antifreeze 0-5%, and water 35-50%.

15. The microcapsule suspension-suspension agent according to claim 1, characterized in that, Terbutaline aqueous suspension comprises the following raw materials in weight fractions: terbutaline 35-40%, dispersant 9-15%, thickener 0-1%, preservative 0-1%, antifreeze 0-5%, and water 45-50%.

16. The microcapsule suspension-suspension agent according to claim 1, characterized in that, Terbutaline aqueous suspension comprises the following raw materials in weight fractions: terbutaline 35-40%, dispersant 9-15%, thickener 0.1-1%, preservative 0.15-1%, antifreeze 3-5%, and water 45-50%.

17. The microcapsule suspension-suspension agent according to claim 1, characterized in that, In the terbutaline aqueous suspension, the dispersant comprises a polycarboxylate and a lignin sulfonate in a weight ratio of (6~8):(3~4).

18. The microcapsule suspension-suspension agent according to claim 1, characterized in that, In the terbutaline aqueous suspension, the antifreeze agent is one or more of ethylene glycol and glycerol.

19. The microcapsule suspension-suspension agent according to claim 1, characterized in that, In the terbutaline aqueous suspension, the preservative is isomethylthiazolinone.

20. The microcapsule suspension-suspension agent according to claim 1, characterized in that, In the terbutaline aqueous suspension, the thickener is one or more of xanthan gum and magnesium aluminum silicate.

21. The microcapsule suspension-suspension agent according to any one of claims 1 to 20, characterized in that, The weight ratio of isoxaflutole and terbutaline is (10:1) to (1:10).

22. The microcapsule suspension-suspension agent according to any one of claims 1 to 20, characterized in that, The weight ratio of isoxaflutole and terbutaline is (5:1) to (1:10).

23. The microcapsule suspension-suspension agent according to any one of claims 1 to 20, characterized in that, The weight ratio of isoxaflutole and terbutaline is (5:1) to (1:5).

24. The microcapsule suspension-suspension agent according to any one of claims 1 to 20, characterized in that, The weight ratio of isoxaflutole to terbutaline is 20:

1.

25. The microcapsule suspension-suspension agent according to any one of claims 1 to 20, characterized in that, The weight ratio of isoxaflutole to terbutaline is 10:

1.

26. The microcapsule suspension-suspension agent according to any one of claims 1 to 20, characterized in that, The weight ratio of isoxaflutole to terbutaline is 5:

1.

27. The microcapsule suspension-suspension agent according to any one of claims 1 to 20, characterized in that, The weight ratio of isoxaflutole to terbutaline is 1:

1.

28. The microcapsule suspension-suspension agent according to any one of claims 1 to 20, characterized in that, The weight ratio of isoxaflutole to terbutaline is 1:

5.

29. The microcapsule suspension-suspension agent according to any one of claims 1 to 20, characterized in that, The weight ratio of isoxaflutole to terbutaline is 1:

10.

30. The microcapsule suspension-suspension agent according to any one of claims 1 to 20, characterized in that, The weight ratio of isoxaflutole to terbutaline is 1:

20.

31. The microcapsule suspension-suspension agent according to any one of claims 1 to 20, characterized in that, The active ingredient accounts for 6% to 60% of the total weight of the composition.

32. The microcapsule suspension-suspension agent according to any one of claims 1 to 20, characterized in that, The active ingredient accounts for 30% to 40% of the total weight of the composition.

33. The microcapsule suspension-suspension agent according to any one of claims 1 to 20, characterized in that, The specific gravity regulator is used as a spray drying aid or a disintegrant.

34. A method for preparing a microcapsule suspension-suspension agent according to any one of claims 1 to 33, characterized in that, include: 1) Preparation of isoxaflutole microcapsule suspension: The oil phase is prepared by mixing isoxabar, solvent, and oil-phase wall material. The dispersant, thickener, and water are mixed to form the aqueous phase; The oil phase is transferred to the aqueous phase, and emulsified by high-speed shearing to obtain an emulsion. The aqueous phase wall material is added and stirring is continued. According to the requirements, a specific gravity regulator and / or preservative are added to prepare isoxaflutole microcapsule suspension. 2) Preparation of terbutaline aqueous suspension: Terbutaline, dispersant, thickener, preservative, antifreeze and water are mixed and wet-milled to the target particle size to obtain terbutaline aqueous suspension. 3) Mix the materials from steps 1) and 2) to obtain microcapsule suspension-suspension agent.

35. The preparation method according to claim 34, characterized in that, In step 1), after adding the aqueous wall material, the emulsion is heated to 50~60℃, and then a specific gravity adjuster and / or preservative is added as needed.

36. The application of a microcapsule suspension-suspension agent according to any one of claims 1 to 33, or a microcapsule suspension-suspension agent prepared by the preparation method according to claims 34 or 35, in the control of weeds in farmland before crop planting, or after sowing and before seedling emergence, or during the crop growth period.

37. The preparation method according to claim 36, characterized in that, The weeds include broadleaf weeds and / or grass weeds.

38. The preparation method according to claim 36, characterized in that, The weeds are selected from at least one of crabgrass, goosegrass, and amaranth.

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