Microcapsule suspension-suspension formulations containing clomazone and sulfentrazone, process for their preparation and use

By mixing isoxaflutole and mesotrione in a specific ratio and using sodium lignosulfonate and polycarboxylate dispersants, the preparation challenges of isoxaflutole and mesotrione microcapsule suspensions were solved, achieving stability and simplifying the process, reducing drift phytotoxicity, and expanding market applications.

CN119791122BActive Publication Date: 2026-04-14SHANDONG WEIFANG RAINBOW CHEMICAL CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-11-29
Publication Date
2026-04-14

AI Technical Summary

Technical Problem

The existing technology for mixed microcapsule suspensions of isoxaflutole and mesotrione has the problems of difficult preparation, poor thermal storage stability, difficulty in compounding, and no stable compound formulations have been reported.

Method used

A microcapsule suspension was prepared by mixing isoxaflutole microcapsule suspension and mesotrione suspension in a specific ratio, using sodium lignosulfonate and polycarboxylate as dispersants, via a single-layer interface method, avoiding the use of emulsifiers and simplifying the process.

Benefits of technology

This invention provides a stable microcapsule suspension of isoxaflutole and mesotrione, which solves the problem of stability after mixing, reduces drift phytotoxicity, has a simple process, low equipment requirements, and a broad market.

✦ Generated by Eureka AI based on patent content.

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Abstract

The application discloses a microcapsule suspension-suspension agent containing isoxaben and sulfentrazone, a preparation method and application thereof, and relates to the field of pesticides, and comprises isoxaben microcapsule suspension agent and sulfentrazone suspension agent mixed according to a mass ratio of 1:(0.1-10). The isoxaben microcapsule suspension agent comprises the following raw materials: isoxaben 5-50 parts by weight, solvent oil 2-10 parts by weight, oil-phase wall material 0.4-5 parts by weight, dispersant 1-8 parts by weight, water-phase wall material 0.1-1 part by weight and water 25-80 parts by weight. The sulfentrazone suspension agent comprises the following raw materials: sulfentrazone 5-50 parts by weight, dispersant 1-8 parts by weight and water 45-96 parts by weight. The dispersant is at least one of sodium lignosulfonate and polycarboxylate. The application can ensure that isoxaben and sulfentrazone are compounded, and the two can stably exist after being mixed, and meanwhile, the drawbacks of isoxaben drift and phytotoxicity in use are solved.
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Description

Technical Field

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

[0002] Microencapsulated suspensions are a novel formulation that encapsulates the active ingredient of pesticides within a core-shell structure using a polymer film material as the wall material, and then uniformly disperses this structure in water. The presence of the capsule wall has several advantages. First, it reduces toxicity to non-target organisms, prolongs efficacy, masks the unpleasant odor of most pesticides, facilitates application and washing of colored pesticides like pendimethalin, reduces pesticide irritation to the applicator, and improves pesticide distribution in the soil. Specialized capsule wall materials can also achieve precise release (immediate, sustained, or controlled release), improving pesticide utilization and providing new application methods. Second, the capsule shell reduces the stability of the formulation and the environment before and after application, making it possible to combine pesticides that cannot be otherwise combined. This has led to the development of various formulations such as microencapsulated suspensions-suspension formulations, microencapsulated suspensions-water emulsions, microencapsulated suspensions-suspension emulsions, wettable powders based on spray drying technology, and water-dispersible granules.

[0003] Currently, metsulfuron-methyl herbicide is a rising star in the herbicide market and has a promising future.

[0004] Sulfentrazone is a triazoline herbicide developed by FMC. It is a protoporphyrinogen oxidase inhibitor; its mechanism of action involves inhibiting protoporphyrinogen oxidase during chlorophyll biosynthesis, causing cell membrane damage and rapid leaf drying and death. It is highly effective against weeds germinating in the soil before emergence.

[0005] Methionamide is effective in controlling most annual broadleaf weeds, grasses, and sedges, such as morning glory, amaranth, ironweed, lambsquarters, datura, knotweed, crabgrass, foxtail, cocklebur, goosegrass, oilseed rape, and nutgrass. It is particularly effective against weeds that are currently difficult to control, such as morning glory, lambsquarters, cocklebur, and nutgrass. Suitable crops include soybeans, corn, sorghum, peanuts, and sunflowers. It has a long residual period in the soil, with a half-life of 110–280 days. It is safe for subsequent cereal crops, but it can cause some phytotoxicity to cotton and sugar beets.

[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, converting its active ingredients into non-toxic degradation products, thus ensuring safety. Isoxaflutole is primarily used to control annual grasses and leafy weeds such as barnyard grass, goosegrass, velvetleaf, burdock, cocklebur, crabgrass, foxtail grass, ragweed, sessile grass, 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-emergence soil treatment in soybean fields, or as an early post-emergence foliar treatment. Isoxaflutole 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 also have high resistance to isoxaflutole and are highly selective, making them a viable option for weed control in soybean fields.

[0008] Mesotrione and isoxaflutole have overlapping applicable crops and weed control spectrums, and can be used as compound agents to achieve synergistic effects.

[0009] However, most of the current formulations of isoxaflutole and metsulfuron are still in the research and development stage, and there are no reports on microcapsule suspensions of isoxaflutole and metsulfuron. The inventors believe that the high solubility of metsulfuron in organic solvents, the low vapor pressure and low melting point of isoxaflutole make it easy for metsulfuron to mature in the form of microcapsules, resulting in poor thermal storage stability and high development difficulty, which greatly increases the difficulty of developing microcapsule suspensions of isoxaflutole and metsulfuron. Summary of the Invention

[0010] Purpose of the invention

[0011] To overcome the above shortcomings, the purpose of this invention is to provide a microcapsule suspension-suspension agent containing isoxaflutole and mesotrione, its preparation method and application. This invention can provide a stable preparation process for a microcapsule suspension-suspension agent composed of isoxaflutole and mesotrione. This process is simple, has low equipment requirements, is easy to industrialize, and has a broad market.

[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 microcapsule suspension-suspension agent containing isoxaflutole and mesotrione, comprising isoxaflutole microcapsule suspension agent and mesotrione suspension agent mixed at a mass ratio of 1:(0.1-10); wherein,

[0015] The isoxaflutole microcapsule suspension comprises the following raw materials in parts by weight: 5-50 parts isoxaflutole, 2-10 parts solvent oil, 0.4-5 parts oil phase wall material, 1-8 parts dispersant, 0-5 parts thickener, 0-10 parts preservative, 0-5 parts antifreeze, 0.1-1 parts aqueous phase wall material, 0-5 parts specific gravity adjuster, 0-1 parts preservative, and 25-80 parts water;

[0016] Mesotrione suspension concentrate comprises the following raw materials in parts by weight: 5-50 parts by weight of mesotrione, 1-8 parts by weight of dispersant, 0-5 parts by weight of antifreeze agent and 45-96 parts by weight of water.

[0017] In isoxaflutole microcapsule suspension and / or mesotrione suspension, the dispersant is at least one of sodium lignosulfonate and polycarboxylate.

[0018] Further, the mixture includes isoxaflutole microcapsule suspension and mesotrione suspension at a mass ratio of 1:(0.5-10), optionally at a mass ratio of 1:(0.5-9), optionally at a mass ratio of 1:(1-9);

[0019] And / or, the weight ratio of isoxaflutole to mesotrione is (1–7):(1–40), optionally (1–7):

[0020] (1~9), optionally (1~2): (1~4).

[0021] Furthermore, the isoxaflutole microcapsule suspension comprises the following raw materials in parts by weight: 5-50 parts isoxaflutole, 2-10 parts solvent oil, 0.4-5 parts oil phase wall material, 1-6 parts polycarboxylate, 0-4 parts sodium lignosulfonate, 0-5 parts thickener, 0-10 parts preservative, 0-5 parts antifreeze, 0.1-1 parts aqueous phase wall material, 0-5 parts specific gravity adjuster, 0-1 parts preservative, and 25-80 parts water;

[0022] And / or, the metolachlor suspension comprises the following raw materials in parts by weight: 5-50 parts by weight of metolachlor, 1-6 parts by weight of polycarboxylate, 0-4 parts by weight of sodium lignosulfonate, 0-5 parts by weight of antifreeze and 45-96 parts by weight of water.

[0023] And / or, in isoxaflutole microcapsule suspension and / or mesotrione suspension, the mass fraction of polycarboxylate and sodium lignin sulfonate is ≤8%.

[0024] Furthermore, in the isoxaflutole microcapsule suspension, the weight ratio of isoxaflutole to oil phase wall material is 1:(0.05-0.5), optionally 1:(0.08-0.5), or optionally 1:(0.08-0.2).

[0025] Furthermore, in the isoxaflutole microcapsule suspension, isoxaflutole is 5-45 parts by weight, optionally 17-40 parts by weight (when the proportion of isoxaflutole in the isoxaflutole microcapsule suspension is 17-40%, it is considered a suitable concentration).

[0026] And / or, in the isoxaflutole microcapsule suspension, the dispersant is 3 to 8 parts by weight, optionally 4 to 6 parts by weight; optionally, the mass fraction of the dispersant is ≤8%;

[0027] And / or, in the isoxaflutole microcapsule suspension, the oily wall material content is 3-5%, optionally 3-4.5%.

[0028] And / or, in the isoxaflutole microcapsule suspension, the oily wall material is an aromatic isocyanate or its modified form; optionally, the oily wall material is selected from one or more of MDI, HDI, TDI, and IPDI;

[0029] And / or, in the isoxaflutole microcapsule suspension, the aqueous phase wall material is 0.1 to 1.0 parts by weight;

[0030] And / or, in the isoxaflutole microcapsule suspension, the aqueous phase wall material is a polyamine, optionally selected from one or more of diamine, triethylenetetramine, and tetraethylenepentamine.

[0031] Furthermore, in the isoxaflutole microcapsule suspension, the solvent oil is 3 to 10 parts by weight, optionally 3 to 5 parts by weight;

[0032] And / or, in the isoxaflutole microcapsule suspension, the solvent is one or more of solvent oil 100#, solvent oil 150#, and solvent oil 200#;

[0033] And / or, in the isoxaflutole microcapsule suspension, the thickener is 0.05 to 0.1 parts by weight;

[0034] And / or, in the isoxaflutole microcapsule suspension, the thickener is xanthan gum;

[0035] And / or, in the isoxaflutole microcapsule suspension, the preservative is 0.1 to 0.2 parts by weight;

[0036] And / or, in the isoxaflutole microcapsule suspension, the preservative is a thiazolinone preservative, optionally methylisothiazolinone;

[0037] And / or, in isoxaflutole microcapsule suspension, the specific gravity adjuster is 3 to 5 parts by weight;

[0038] And / or, in the isoxaflutole microcapsule suspension, the specific gravity regulator is anhydrous calcium chloride;

[0039] And / or, in the isoxaflutole microcapsule suspension, the antifreeze agent is ethylene glycol;

[0040] And / or, in isoxaflutole microcapsule suspension, water is added to bring the total to 100 parts by weight.

[0041] Furthermore, in the metolachlor aqueous suspension, metolachlor is present in the form of 20-50 parts by weight, optionally 30-40 parts by weight;

[0042] And / or, in the mesotrione aqueous suspension, the thickener is 0.05 to 0.1 parts by weight;

[0043] And / or, in the metolachlor aqueous suspension, the thickener is xanthan gum;

[0044] And / or, in the mesotrione aqueous suspension, the preservative is 0.1 to 0.2 parts by weight;

[0045] And / or, in the metolachlor aqueous suspension, the preservative is a thiazolinone preservative, optionally methylisothiazolinone;

[0046] And / or, in mesotrione aqueous suspension, the antifreeze is 1-3%.

[0047] And / or, in the mesotrione aqueous suspension, the antifreeze agent is ethylene glycol;

[0048] And / or, in the mesotrione aqueous suspension, water is made up to 100 parts by weight.

[0049] In a second aspect, a method for preparing a microcapsule suspension-suspension agent as described in the first aspect is provided, characterized by comprising the following steps:

[0050] 1) Preparation of isoxaflutole microcapsule suspension:

[0051] The oil phase is prepared by mixing isoxabar, solvent, and oil-phase wall material.

[0052] The dispersant, thickener, and water are mixed to form the aqueous phase;

[0053] 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 tetraethylenepentamine, the emulsion is heated to 50-60°C and then a specific gravity regulator and / or preservative is added according to the requirements.

[0054] 2) Preparation of metolachlor aqueous suspension:

[0055] The terbutaline, dispersant, thickener, preservative, antifreeze and water are mixed and wet-milled to the target particle size to obtain metolachlor aqueous suspension.

[0056] 3) Mix the materials from steps 1) and 2) to obtain microcapsule suspension-suspension agent.

[0057] Thirdly, the application of the microcapsule suspension-suspension agent described in the first aspect, or the microcapsule suspension-suspension agent prepared by the preparation method described in the second aspect, in the control of weeds in farmland before crop planting, or after sowing and before seedling emergence, or during the crop growth period.

[0058] Furthermore, the weeds include broadleaf weeds and / or grass weeds; optionally, the weeds are selected from at least one of goosegrass, crabgrass, lambsquarters, and amaranth.

[0059] Beneficial effects

[0060] (1) This invention provides a stable microcapsule suspension of isoxaflutole and mesotrione through the selection of adjuvants. The preparation process is simple, requires low equipment, is easy to industrialize, and has a broad market. This invention ensures that isoxaflutole and mesotrione remain stable after mixing, while also solving the problem of isoxaflutole drift damage during use.

[0061] (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, requiring only one-step reaction to form capsules; ③ The product exhibits small batch-to-batch variations, good stability, and good storage stability; ④ Through extensive testing and screening of adjuvants, a stable formulation and product have been obtained. The key innovation is that the adjuvants used in the mesotrione aqueous suspension must be consistent with the adjuvant system of the isoxaflutole microcapsule suspension, or the types of adjuvants used must be selected from the adjuvant system of the isoxaflutole microcapsule suspension. Detailed Implementation

[0062] 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.

[0063] 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.

[0064] 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.

[0065] The above-described fungicidal composition provides a new option for weed control. The following examples further illustrate this disclosure, but this disclosure is not intended to be limiting.

[0066] The present invention relates to a microencapsulated suspension of isoxaflutole and mesotrione, and its preparation method. The method involves microencapsulating isoxaflutole using a single-layer interface method. The required raw materials include: solvent, oil phase wall material, dispersant, thickener, preservative, specific gravity adjuster, and aqueous phase wall material. Through continuous research and development, the present invention has found that by abandoning the use of emulsifiers (generally used in microencapsulation preparation) in the adjuvant system, only sodium lignosulfonate and polycarboxylate are used as dispersants. This dispersant system is then used as an optional system for mesotrione aqueous suspensions. This ensures that isoxaflutole and mesotrione remain stable after mixing, while simultaneously addressing the issue of isoxaflutole drift and phytotoxicity during use.

[0067] In the following examples, isoxaflutole and mesotrione are both commercially available, and the other adjuvants are also commercially available products.

[0068] The present invention will be further described in detail below through examples.

[0069] Example 1 (Isoxamethonium and metsulfuron-methyl in a weight ratio of 1:1)

[0070] Preparation of (17.5% isoxaflutole + 17.5% mesotrione) microcapsule suspension-suspension.

[0071] (I) Preparation of 35% isoxaflutole microcapsule suspension

[0072] A. Dissolve 36.46% isoxaflutole technical grade (of which isoxaflutole content is 96%) in 4.5% solvent oil 100#, then add 3.5% MDI and mix well to form the oil phase;

[0073] B. Mix 5% polycarboxylate, 0.05% xanthan gum, and 46.04% water under shear homogenization conditions to prepare the aqueous phase for later use;

[0074] C. Transfer the oil phase to the aqueous phase, use a high-speed shear emulsifier to shear to obtain an emulsion, and then slowly add 0.35% hexamethylenediamine while stirring continuously;

[0075] D. 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 and 0.1% methylisothiazolinone were added, and stirring was continued for 0.5 hours.

[0076] E. Finally, after maintaining the temperature for a certain period of time, cool down to 20-25℃ to prepare 35% isoxaflutole microcapsule suspension. Discharge and set aside.

[0077] (II) Preparation of 35% Methionil Aqueous Suspension

[0078] F. Add 36.84% of metolachlor technical (of which metolachlor content is 95%), 5% polycarboxylate, 0.07% xanthan gum, 0.15% methylisothiazolinone, 2% ethylene glycol and 55.94% water to the preparation apparatus and disperse evenly.

[0079] G. Using a wet grinding process, the material system is ground to the target particle size to obtain 35% metsulfuron-methyl aqueous suspension.

[0080] H. The 35% metsulfuron-methyl aqueous suspension is stored in a transfer container through a filter for later use.

[0081] (III) Mixed (17.5% isoxaflutole + 17.5% mesotrione) microcapsule suspension - suspension concentrate

[0082] I. Mix the 35% isoxaflutole microcapsule suspension prepared in step (I) and the 35% mesotrione aqueous suspension prepared in step (II) at a mass ratio of 1:1 and stir evenly to obtain (17.5% isoxaflutole + 17.5% mesotrione) microcapsule suspension-suspension.

[0083] Example 2 (Isoxamethonium and metsulfuron-methyl in a weight ratio of 2:1)

[0084] Preparation of (20% isoxaflutole + 10% mesotrione) microcapsule suspension-suspension agent.

[0085] (I) Preparation of 30% isoxaflutole microcapsule suspension

[0086] A. Dissolve 31.25% isoxaflutole technical grade (96% isoxaflutole content) in 5% solvent oil 100#, then add 3% MDI and mix well to form the oil phase;

[0087] B. Take 4% polycarboxylate, 0.1% xanthan gum, and 53.05% water and mix them evenly under shear homogenization conditions to prepare the aqueous phase for later use;

[0088] C. Transfer the oil phase to the aqueous phase, use a high-speed shear emulsifier to shear to obtain an emulsion, and then slowly add 0.4% hexamethylenediamine while stirring continuously;

[0089] D. Under continuous stirring, the emulsion was heated to 55°C, and the system was kept at this temperature for 4 hours. Then, 3% calcium chloride and 0.2% methylisothiazolinone were added, and stirring was continued for 0.5 hours.

[0090] E. Finally, after maintaining the temperature for a certain period of time, cool down to 20-25℃ to obtain isoxaflutole microcapsule suspension. Discharge and set aside.

[0091] (II) Preparation of 30% Methionil Aqueous Suspension

[0092] F. Add 31.58% of metolachlor technical (of which metolachlor content is 95%), 4% polycarboxylate, 0.1% xanthan gum, 0.2% methylisothiazolinone, 3% ethylene glycol and 61.12% water to the preparation apparatus and disperse evenly.

[0093] G. The material system is ground using a wet grinding process to the target particle size to obtain 30% metsulfuron-methyl aqueous suspension. H. The 30% metsulfuron-methyl aqueous suspension is filtered and stored in a transfer container for later use.

[0094] (III) Mixed (20% isoxaflutole + 10% mesotrione) microcapsule suspension - suspension concentrate

[0095] I. Mix the 30% isoxaflutole microcapsule suspension prepared in step (I) and the 30% mesotrione aqueous suspension prepared in step (II) at a mass ratio of 2:1 and stir evenly to obtain (20% isoxaflutole + 10% mesotrione) microcapsule suspension-suspension.

[0096] Example 3 (Isoxamethonium and metsulfuron-methyl in a weight ratio of 1:3)

[0097] Preparation of (10% isoxaflutole + 30% mesotrione) microcapsule suspension-suspension agent.

[0098] (I) Preparation of 40% isoxaflutole microcapsule suspension

[0099] A. Dissolve 41.67% isoxaflutole technical grade (of which isoxaflutole content is 96%) in 4% solvent oil 100#, then add 4% MDI and mix well as the oil phase;

[0100] B. Mix 6% polycarboxylate, 0.05% xanthan gum, and 38.88% water under shear homogenization conditions to prepare the aqueous phase for later use;

[0101] C. Transfer the oil phase to the aqueous phase, use a high-speed shear emulsifier to shear to obtain an emulsion, and then slowly add 0.3% hexamethylenediamine while stirring continuously;

[0102] D. Under continuous stirring, the emulsion was heated to 55°C, and the system was kept at this temperature for 4 hours. Then, 5% calcium chloride and 0.1% methylisothiazolinone were added, and stirring was continued for 0.5 hours.

[0103] E. Finally, after maintaining the temperature for a certain period of time, cool down to 20-25℃ to obtain 40% isoxaflutole microcapsule suspension. Discharge and set aside.

[0104] (II) Preparation of 40% Methionil Aqueous Suspension

[0105] F. Add 42.11% of metolachlor technical (of which metolachlor content is 95%), 6% polycarboxylate, 0.05% xanthan gum, 0.1% methylisothiazolinone, 1% ethylene glycol and 50.74% water used in isoxaflutole microcapsule suspension to the preparation apparatus and disperse evenly.

[0106] G. The material system is ground using a wet grinding process to the target particle size, thus obtaining 40% metsulfuron-methyl aqueous suspension.

[0107] H. The 40% metsulfuron-methyl aqueous suspension is stored in a transfer container through a filter for later use.

[0108] (III) Mixed (10% isoxaflutole + 30% mesotrione) microcapsule suspension - suspension concentrate

[0109] I. Mix the 40% isoxaflutole microcapsule suspension prepared in step (I) and the 40% mesotrione aqueous suspension prepared in step (II) at a ratio of 1:3 and stir evenly to obtain (10% isoxaflutole + 30% mesotrione) microcapsule suspension-suspension.

[0110] Example 4 (Isoxam and mesotrione in a weight ratio of 3:4)

[0111] Preparation of (15% isoxaflutole + 20% mesotrione) microcapsule suspension-suspension agent.

[0112] (I) Preparation of 30% isoxaflutole microcapsule suspension

[0113] A. Dissolve 31.25% isoxaflutole technical grade (96% isoxaflutole content) in 5% solvent oil 100#, then add 3% MDI and mix well to form the oil phase;

[0114] B. Take 4% polycarboxylate, 0.1% xanthan gum, and 53.05% water and mix them evenly under shear homogenization conditions to prepare the aqueous phase for later use;

[0115] C. Transfer the oil phase to the aqueous phase, use a high-speed shear emulsifier to shear to obtain an emulsion, and then slowly add 0.4% hexamethylenediamine while stirring continuously;

[0116] D. Under continuous stirring, the emulsion was heated to 55°C, and the system was kept at this temperature for 4 hours. Then, 3% calcium chloride and 0.2% methylisothiazolinone were added, and stirring was continued for 0.5 hours.

[0117] E. Finally, after maintaining the temperature for a certain period of time, cool down to 20-25℃ to prepare 30% isoxaflutole microcapsule suspension. Discharge and set aside.

[0118] (II) Preparation of 40% Methionil Aqueous Suspension

[0119] F. Add 42.11% of metolachlor technical (of which metolachlor content is 95%), 6% polycarboxylate, 0.05% xanthan gum, 0.1% methylisothiazolinone, 1% ethylene glycol and 50.74% water used in isoxaflutole microcapsule suspension to the preparation apparatus and disperse evenly.

[0120] G. The material system is ground using a wet grinding process to the target particle size, thus obtaining 40% metsulfuron-methyl aqueous suspension.

[0121] H. The 40% metsulfuron-methyl aqueous suspension is stored in a transfer container through a filter for later use.

[0122] (III) Mixed (15% isoxaflutole + 20% mesotrione) microcapsule suspension - suspension concentrate

[0123] I. Mix the 30% isoxaflutole microcapsule suspension prepared in step (I) and the 40% mesotrione aqueous suspension prepared in step (II) at a mass ratio of 1:1 and stir evenly to obtain (15% isoxaflutole + 20% mesotrione) microcapsule suspension-suspension.

[0124] Example 5 (Isoxamethonium and metsulfuron-methyl in a weight ratio of 4:3)

[0125] Preparation of (20% isoxaflutole + 15% mesotrione) microcapsule suspension-suspension.

[0126] (I) Preparation of 40% isoxaflutole microcapsule suspension

[0127] A. Dissolve 41.67% isoxaflutole technical grade (of which isoxaflutole content is 96%) in 4% solvent oil 100#, then add 4% MDI and mix well as the oil phase;

[0128] B. Mix 6% polycarboxylate, 0.05% xanthan gum, and 38.88% water under shear homogenization conditions to prepare the aqueous phase for later use;

[0129] C. Transfer the oil phase to the aqueous phase, use a high-speed shear emulsifier to shear to obtain an emulsion, and then slowly add 0.3% hexamethylenediamine while stirring continuously;

[0130] D. Under continuous stirring, the emulsion was heated to 55°C, and the system was kept at this temperature for 4 hours. Then, 5% calcium chloride and 0.1% methylisothiazolinone were added, and stirring was continued for 0.5 hours.

[0131] E. Finally, after maintaining the temperature for a certain period of time, cool down to 20-25℃ to prepare 40% isoxaflutole microcapsule suspension. Discharge and set aside.

[0132] (II) Preparation of 30% Methionil Aqueous Suspension

[0133] F. Add 31.58% of metolachlor technical (of which metolachlor content is 95%), 4% polycarboxylate, 0.1% xanthan gum, 0.2% methylisothiazolinone, 3% ethylene glycol and 61.12% water to the preparation apparatus and disperse evenly.

[0134] G. The material system is ground using a wet grinding process to the target particle size, thus obtaining 30% metsulfuron-methyl aqueous suspension.

[0135] H. The 30% metsulfuron-methyl aqueous suspension is stored in a transfer container through a filter for later use.

[0136] (III) Mixed (20% isoxaflutole + 15% mesotrione) microcapsule suspension - suspension concentrate

[0137] I. Mix the 40% isoxaflutole microcapsule suspension prepared in step (I) and the 30% mesotrione aqueous suspension prepared in step (II) in a 1:1 ratio and stir evenly to obtain (20% isoxaflutole + 15% mesotrione) microcapsule suspension-suspension.

[0138] Example 6 (Isoxam and metsulfuron-methyl in a weight ratio of 1:1)

[0139] Preparation of (17.5% isoxaflutole + 17.5% mesotrione) microcapsule suspension-suspension.

[0140] (I) Preparation of 35% isoxaflutole microcapsule suspension

[0141] A. Dissolve 36.46% isoxaflutole technical grade (of which isoxaflutole content is 96%) in 4.5% solvent oil 150#, then add 3.5% HDI and mix well to form the oil phase;

[0142] B. Take 2% polycarboxylate, 3% sodium lignosulfonate, 0.05% xanthan gum, and 46.04% water and mix them evenly under shear homogenization conditions to prepare the aqueous phase for later use;

[0143] C. Transfer the oil phase to the aqueous phase, use a high-speed shear emulsifier to shear to obtain an emulsion, and then slowly add 0.35% tetraethylenepentamine while stirring continuously;

[0144] D. 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 and 0.1% methylisothiazolinone were added, and stirring was continued for 0.5 hours.

[0145] E. Finally, after maintaining the temperature for a certain period of time, cool down to 20-25℃ to prepare 35% isoxaflutole microcapsule suspension. Discharge and set aside.

[0146] (II) Preparation of 35% Methionil Aqueous Suspension

[0147] F. Add 36.84% of metolachlor technical (of which metolachlor content is 95%), 2% polycarboxylate, 3% sodium lignosulfonate, 0.07% xanthan gum, 0.15% methylisothiazolinone, 2% ethylene glycol and 55.94% water to the preparation apparatus and disperse evenly.

[0148] G. The material system is ground using a wet grinding process to the target particle size, thus obtaining 35% metsulfuron-methyl aqueous suspension.

[0149] H. The 35% metsulfuron-methyl aqueous suspension is stored in a transfer container through a filter for later use.

[0150] (III) Mixed (17.5% isoxaflutole + 17.5% mesotrione) microcapsule suspension - suspension concentrate

[0151] I. Mix the 35% isoxaflutole microcapsule suspension prepared in step (I) and the 35% mesotrione aqueous suspension prepared in step (II) at a mass ratio of 1:1 and stir evenly to obtain (17.5% isoxaflutole + 17.5% mesotrione) microcapsule suspension-suspension.

[0152] Example 7 (Isoxamethonium and metsulfuron-methyl in a weight ratio of 2:3)

[0153] Preparation of (2% isoxaflutole + 3% mesotrione) microcapsule suspension-suspension agent.

[0154] (I) Preparation of 5% isoxaflutole microcapsule suspension

[0155] A. Dissolve 5.21% isoxaflutole technical grade (96% isoxaflutole content) in 10% solvent oil 150#, then add 0.4% IPDI and mix well to form the oil phase;

[0156] B. Take 1% polycarboxylate, 1% sodium lignosulfonate, 0.1% xanthan gum, and 78.99% water and mix them evenly under shear homogenization conditions to prepare the aqueous phase for later use;

[0157] C. Transfer the oil phase to the aqueous phase, use a high-speed shear emulsifier to shear to obtain an emulsion, and then slowly add 0.1% triethylenetetramine while stirring continuously;

[0158] D. Under continuous stirring, the emulsion was heated to 55°C, and the system was kept at this temperature for 4 hours. Then, 3% calcium chloride and 0.2% methylisothiazolinone were added, and stirring was continued for 0.5 hours.

[0159] E. Finally, after maintaining the temperature for a certain period of time, cool down to 20-25℃ to prepare 5% isoxaflutole microcapsule suspension. Discharge and set aside.

[0160] (II) Preparation of 5% Methionil Aqueous Suspension

[0161] F. Add 5.26% metsulfuron-methyl technical (95% metsulfuron content), 1% polycarboxylate, 0.05% xanthan gum, 0.2% methylisothiazolinone, 1% ethylene glycol, and 92.49% water to the preparation apparatus and disperse evenly. G. Grind the material system using a wet grinding process to the target particle size to obtain a 5% metsulfuron-methyl aqueous suspension. H. Filter the 5% metsulfuron-methyl aqueous suspension and store it in a transfer container for later use.

[0162] (III) Mixed (2% isoxaflutole + 3% mesotrione) microcapsule suspension - suspension concentrate

[0163] I. Mix the 5% isoxaflutole microcapsule suspension prepared in step (I) and the 5% mesotrione aqueous suspension prepared in step (II) in a 2:3 ratio and stir evenly to obtain (2% isoxaflutole + 3% mesotrione) microcapsule suspension-suspension.

[0164] Example 8 (Isoxam and mesotrione in a weight ratio of 1:9)

[0165] Preparation of (5% isoxaflutole + 45% mesotrione) microcapsule suspension-suspension agent.

[0166] (I) Preparation of 50% isoxaflutole microcapsule suspension

[0167] A. Melt 52.08% isoxaflutole technical grade (of which isoxaflutole content is 96%) at 50°C, then add 5% TDI and mix well to form the oil phase;

[0168] B. Take 4% polycarboxylate, 4% sodium lignosulfonate, 0.05% xanthan gum, and 28.77% water and mix them evenly under shear homogenization conditions to prepare the aqueous phase for later use;

[0169] C. Transfer the oil phase to the aqueous phase, use a high-speed shear emulsifier to shear the oil-in-water emulsion, and then slowly add 1% triethylenetetramine while stirring continuously.

[0170] D. Under continuous stirring, the emulsion was heated to 55°C, and the system was kept at this temperature for 4 hours. Then, 5% calcium chloride and 0.1% methylisothiazolinone were added, and stirring was continued for 0.5 hours.

[0171] E. Finally, after maintaining the temperature for a certain period of time, cool down to 20-25℃ to prepare 50% isoxaflutole microcapsule suspension. Discharge and set aside.

[0172] (II) Preparation of 50% Methionil Aqueous Suspension

[0173] F. Add 52.63% of metolachlor technical (of which metolachlor content is 95%), 8% of polycarboxylate, 0.1% xanthan gum, 0.1% methylisothiazolinone, 3% ethylene glycol and 36.17% water to the preparation apparatus and disperse evenly.

[0174] G. The material system is ground using a wet grinding process to the target particle size, thus obtaining 50% metsulfuron-methyl aqueous suspension.

[0175] H. The 50% metsulfuron-methyl aqueous suspension is stored in a transfer container through a filter for later use.

[0176] (III) Mixed (5% isoxaflutole + 45% mesotrione) microcapsule suspension - suspension concentrate

[0177] I. Mix the 50% isoxaflutole microcapsule suspension prepared in step (I) and the 50% mesotrione aqueous suspension prepared in step (II) at a ratio of 1:9 and stir evenly to obtain (5% isoxaflutole + 45% mesotrione) microcapsule suspension-suspension.

[0178] Example 9 (Isoxamethonium and metsulfuron-methyl in a weight ratio of 1:40)

[0179] Preparation of (1% isoxaflutole + 40% mesotrione) microcapsule suspension-suspension.

[0180] (I) Preparation of 5% isoxaflutole microcapsule suspension

[0181] A. Dissolve 5.21% isoxaflutole technical grade (96% isoxaflutole content) in 10% solvent oil 150#, then add 0.4% IPDI and mix well to form the oil phase;

[0182] B. Take 1% polycarboxylate, 1% sodium lignosulfonate, 0.1% xanthan gum, and 78.99% water and mix them evenly under shear homogenization conditions to prepare the aqueous phase for later use;

[0183] C. Transfer the oil phase to the aqueous phase, use a high-speed shear emulsifier to shear to obtain an emulsion, and then slowly add 0.1% triethylenetetramine while stirring continuously;

[0184] D. Under continuous stirring, the emulsion was heated to 55°C, and the system was kept at this temperature for 4 hours. Then, 3% calcium chloride and 0.2% methylisothiazolinone were added, and stirring was continued for 0.5 hours.

[0185] E. Finally, after maintaining the temperature for a certain period of time, cool down to 20-25℃ to prepare 5% isoxaflutole microcapsule suspension. Discharge and set aside.

[0186] (II) Preparation of 50% Methionil Aqueous Suspension

[0187] F. Add 52.63% of metolachlor technical (of which metolachlor content is 95%), 8% polycarboxylate, 0.1% xanthan gum, 0.1% methylisothiazolinone, 3% ethylene glycol and 36.17% water to the preparation apparatus and disperse evenly.

[0188] G. The material system is ground using a wet grinding process to the target particle size, thus obtaining 50% metsulfuron-methyl aqueous suspension.

[0189] H. The 50% metsulfuron-methyl aqueous suspension is stored in a transfer container through a filter for later use.

[0190] (III) Mixed (1% isoxaflutole + 40% mesotrione) microcapsule suspension - suspension concentrate

[0191] I. Mix the 5% isoxaflutole microcapsule suspension prepared in step (I) and the 50% mesotrione aqueous suspension prepared in step (II) at a ratio of 1:4 and stir evenly to obtain (4% isoxaflutole + 40% mesotrione) microcapsule suspension-suspension.

[0192] Example 10 (Isoxamethonium and metsulfuron-methyl in a weight ratio of 20:3)

[0193] Preparation of (20% isoxaflutole + 3% mesotrione) microcapsule suspension-suspension agent.

[0194] (I) Preparation of 50% isoxaflutole microcapsule suspension

[0195] A. Melt 52.08% isoxaflutole technical grade (of which isoxaflutole content is 96%) at 50°C, then add 5% TDI and mix well to form the oil phase;

[0196] B. Take 4% polycarboxylate, 4% sodium lignosulfonate, 0.05% xanthan gum, and 28.77% water and mix them evenly under shear homogenization conditions to prepare the aqueous phase for later use;

[0197] C. Transfer the oil phase to the aqueous phase, use a high-speed shear emulsifier to shear the oil-in-water emulsion, and then slowly add 1% triethylenetetramine while stirring continuously.

[0198] D. Under continuous stirring, the emulsion was heated to 55°C, and the system was kept at this temperature for 4 hours. Then, 5% calcium chloride and 0.1% methylisothiazolinone were added, and stirring was continued for 0.5 hours.

[0199] E. Finally, after maintaining the temperature for a certain period of time, cool down to 20-25℃ to prepare 50% isoxaflutole microcapsule suspension. Discharge and set aside.

[0200] (II) Preparation of 5% Methionil Aqueous Suspension

[0201] F. Add 5.26% metsulfuron-methyl technical (of which metsulfuron-methyl content is 95%), 1% of the polycarboxylate used in isoxaflutole microcapsule suspension, 0.05% xanthan gum, 0.2% methylisothiazolinone, 1% ethylene glycol and 92.49% water to the preparation apparatus and disperse evenly.

[0202] G. The material system is ground using a wet grinding process to the target particle size to obtain 5% metsulfuron-methyl aqueous suspension.

[0203] H. The 5% metsulfuron-methyl aqueous suspension is stored in a transfer container through a filter for later use.

[0204] (III) Mixed (20% isoxaflutole + 3% mesotrione) microcapsule suspension - suspension concentrate

[0205] I. Mix the 50% isoxaflutole microcapsule suspension prepared in step (I) and the 5% mesotrione aqueous suspension prepared in step (II) in a 2:3 ratio and stir evenly to obtain (20% isoxaflutole + 3% mesotrione) microcapsule suspension-suspension.

[0206] Comparative Example 1 (Isoxamethonium and metsulfuron-methyl in a weight ratio of 1:1)

[0207] Preparation of (17.5% isoxaflutole + 17.5% mesotrione) microcapsule suspension-suspension.

[0208] (I) Preparation of 35% isoxaflutole microcapsule suspension

[0209] A. Dissolve 36.46% isoxaflutole technical grade (of which isoxaflutole content is 96%) in 4.5% solvent oil 100#, then add 3.5% MDI and mix well to form the oil phase;

[0210] B. Mix 5% sodium lignosulfonate, 0.05% xanthan gum, and 46.04% water under shear homogenization conditions to prepare the aqueous phase for later use;

[0211] C. Transfer the oil phase to the aqueous phase, use a high-speed shear emulsifier to shear to obtain an emulsion, and then slowly add 0.35% hexamethylenediamine while stirring continuously;

[0212] D. 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 and 0.1% methylisothiazolinone were added, and stirring was continued for 0.5 hours.

[0213] E. Finally, after maintaining the temperature for a certain period of time, cool down to 20-25℃ to prepare 35% isoxaflutole microcapsule suspension. Discharge and set aside.

[0214] (II) Preparation of 35% Methionil Aqueous Suspension

[0215] F. Add 36.84% of metolachlor technical (of which metolachlor content is 95%), 2% block polyether nonionic emulsifier, 3% phosphate ester dispersant, 0.07% xanthan gum, 0.15% methylisothiazolinone, 2% ethylene glycol and 55.94% water to the preparation apparatus and disperse evenly.

[0216] G. The material system is ground using a wet grinding process to the target particle size, thus obtaining 35% metsulfuron-methyl aqueous suspension.

[0217] H. The 35% metsulfuron-methyl aqueous suspension is stored in a transfer container through a filter for later use.

[0218] (III) Mixed (17.5% isoxaflutole + 17.5% mesotrione) microcapsule suspension - suspension concentrate

[0219] I. Mix the 35% isoxaflutole microcapsule suspension prepared in step (I) and the 35% mesotrione aqueous suspension prepared in step (II) in a 1:1 ratio and stir evenly to obtain (17.5% isoxaflutole + 17.5% mesotrione) microcapsule suspension-suspension.

[0220] Comparative Example 2 (Isoxamethonium and metsulfuron-methyl in a weight ratio of 1:1)

[0221] Preparation of (17.5% isoxaflutole + 17.5% mesotrione) microcapsule suspension-suspension.

[0222] (I) Preparation of 35% isoxaflutole microcapsule suspension

[0223] A. Dissolve 36.46% isoxaflutole technical grade (of which isoxaflutole content is 96%) in 4.5% solvent oil 100#, then add 3.5% MDI and mix well to form the oil phase;

[0224] B. Mix 5% polycarboxylate, 0.05% xanthan gum, and 46.04% water under shear homogenization conditions to prepare the aqueous phase for later use;

[0225] C. Transfer the oil phase to the aqueous phase, use a high-speed shear emulsifier to shear to obtain an emulsion, and then slowly add 0.35% hexamethylenediamine while stirring continuously;

[0226] D. 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 and 0.1% methylisothiazolinone were added, and stirring was continued for 0.5 hours.

[0227] E. Finally, after maintaining the temperature for a certain period of time, cool down to 20-25℃ to prepare 35% isoxaflutole microcapsule suspension. Discharge and set aside.

[0228] (II) Preparation of 70% Methionil Wettable Powder

[0229] F. Mix 73.68% of metolachlor technical (of which metolachlor content is 95%) and polycarboxylate (solid powder 26.32%) evenly in the material system, and then pulverize it using air jet milling to the target particle size to obtain 70% metolachlor wettable powder.

[0230] (III) Mixed (17.5% isoxaflutole + 17.5% mesotrione) microcapsule suspension - suspension concentrate

[0231] I. Mix the 35% isoxaflutole microcapsule suspension prepared in step (I) and the 70% mesotrione wettable powder prepared in step (II) with water in a ratio of 2:1:1 and stir evenly to obtain (17.5% isoxaflutole + 17.5% mesotrione) microcapsule suspension-suspension.

[0232] Test Example 1

[0233] The samples of Examples 1-10 and Comparative Examples 1-2, as well as their heat storage and freeze-thaw samples, were tested in accordance with national standards.

[0234] The suspension rate was tested according to the method in GB / T14825-2023;

[0235] Persistent foaming performance was tested according to the method in GB / T28137-2011;

[0236] pH value was determined according to the method in GB / T 1601-2023;

[0237] The wet sieve test shall be performed in accordance with the method of GB / T 16150-1995;

[0238] The pourability shall be tested according to the method of GB / T31737-2015;

[0239] Thermal storage stability was tested according to GB / T 19136-2021.

[0240] The freeze-thaw stability test was conducted in four cycles between room temperature (20℃±2℃) and (-10℃±2℃), with each cycle consisting of 18 hours of freezing and 6 hours of thawing.

[0241] Spontaneous dispersion is detected using the MT160 method in the CIPAC framework.

[0242] The test results are shown in Table 1.

[0243] Table 1. Stability test results of formulations for Examples 1-10 and Comparative Examples 1-2

[0244]

[0245]

[0246] Note: In Table 1, the products of Comparative Examples 1 and 2 were flowable when freshly prepared; the heat storage stability of Comparative Examples 1 and 2 in Table 1 was unqualified, mainly due to the problem of sample paste formation after heat storage, which rendered the test meaningless; the freeze-thaw stability of Comparative Examples 1 and 2 was also unqualified, with unqualified items including: metsulfuron suspension rate, spontaneous dispersibility, and isoxaflutole encapsulation rate. Microscopic examination of freeze-thawed and room temperature samples clearly showed that metsulfuron underwent severe Austrones ripening, and the surface of isoxaflutole microcapsules showed many depressions and obvious wrinkles, no longer being smooth spheres.

[0247] As shown in Table 1, the isoxaflutole + mesotrione microcapsule suspension prepared by this invention passed all tests. The samples remained stable after heat storage and accelerated freeze-thaw storage, indicating good reproducibility of the preparation process, stable product quality, and good freeze-thaw stability. Compared to Comparative Examples 1-2, Examples 1-2 failed the freeze-thaw test, exhibiting numerous long, radial rod-shaped crystals under microscopic examination. While their phenotypes were consistent with the room-temperature comparative samples, they were slightly better. This indicates that ① the comparative products had poor stability over time, and low temperatures could mitigate the deterioration trend. ② The specific reason for the quality deterioration is that the adjuvants on the surface of the mesotrione particles in the microcapsule suspension-suspension agent, after being mixed into the microcapsule suspension-suspension agent, experienced desorption and migration into the water or onto the surface of the isoxaflutole microcapsules (Comparative Example 1), or were not effectively adsorbed (Comparative Example 2). Without the assistance of the adjuvants, mesotrione undergoes significant Austrones ripening, and the contact between mesotrione and the isoxaflutole capsule shell causes deformation of the microcapsule surface, thus affecting the encapsulation efficiency of isoxaflutole. Overall, the formulation of this invention has good stability and solves the problem of instability in the mixing of isoxaflutole and mesotrione.

[0248] Test Example 2

[0249] Field trial example: Herbal efficacy test of annual weeds in sugarcane fields

[0250] 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.

[0251] Five treatments were set up: Treatment 1: water spray, blank control; Treatment 2: Example 1; Treatment 3: Example 6; Treatment 4: Comparative Example 1; Treatment 5: Comparative Example 2. All samples were freshly prepared and could be diluted with water to meet the spraying requirements.

[0252] Based on field application registration data, the field application rate for each treatment was calculated to be 200g / mu.

[0253] The pesticide was applied once using a Gongnong-16 backpack manual sprayer, with the dosage of the formulation diluted in 30L of water per acre, and sprayed evenly. The weather was favorable during the trial period, with an average daily temperature of 18-23℃. There was no rain on the day of application, and no rain fell within 10 days after application.

[0254] 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.

[0255]

[0256] The 30-day fresh weight efficacy results are shown in Table 2.

[0257] Table 2 Results of the 30-day fresh weight control efficacy of each treatment on annual weeds.

[0258]

[0259] As shown in Table 2, under the same formulation and specifications, the examples all showed significant improvements over the comparative examples. The (isoxaflubenzuron + mesotrione) microcapsule suspension prepared according to the method of this invention achieved an overall control efficacy of over 90%, demonstrating superior efficacy compared to other (isoxaflubenzuron + mesotrione) microcapsule suspensions prepared by conventional methods. The reason for this is that while the (isoxaflubenzuron + mesotrione) microcapsule suspensions prepared in the comparative examples met the application requirements in terms of appearance, flowability, and other conventional physicochemical indicators, the internal active ingredients were in an unstable state, resulting in poor dispersion. This was particularly problematic for soil-sealing herbicides, where the active ingredient remained in a "waiting for weeds" state after spraying, leading to poor uniformity of distribution and consequently, lower control efficacy. Follow-up monitoring of sugarcane growth in each treatment plot showed no significant abnormalities, indicating that the drug combination covered by this invention has high safety for sugarcane and good application effects.

[0260] In summary, the (isoxamethonium + mesotrione) microcapsule suspension-suspension preparation method and the product prepared by the method protected by this invention have higher stability, fewer types of raw materials, and more stable efficacy, showing significant advantages.

[0261] 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 agent containing isoxaflutole and mesotrione, characterized in that, The mixture includes isoxaflutole microcapsule suspension and mesotrione suspension at a mass ratio of 1:(0.1~10); the weight ratio of isoxaflutole to mesotrione is (1~7):(1~40); wherein, The isoxaflutole microcapsule suspension comprises the following raw materials in parts by weight: 5-50 parts isoxaflutole, 2-10 parts solvent oil, 0.4-5 parts oil phase wall material, 1-6 parts polycarboxylate, 0-4 parts sodium lignosulfonate, 0-5 parts thickener, 0-10 parts preservative, 0-5 parts antifreeze, 0.1-1 parts aqueous phase wall material, 0-5 parts specific gravity adjuster, 0-1 parts preservative, and 25-80 parts water; the oil phase wall material is selected from one or more of MDI, HDI, TDI, and IPDI; the aqueous phase wall material is selected from one or more of diamine, triethylenetetramine, and tetraethylenepentamine. Mesotrione suspension concentrate comprises the following raw materials in parts by weight: 5-50 parts by weight of mesotrione, 1-6 parts by weight of polycarboxylate, 0-4 parts by weight of sodium lignosulfonate, 0-5 parts by weight of antifreeze and 45-96 parts by weight of water. In isoxaflutole microcapsule suspension and / or mesotrione suspension, the mass fraction of polycarboxylate and sodium lignin sulfonate is ≤8%.

2. The microcapsule suspension-suspension agent according to claim 1, characterized in that, The mixture includes isoxaflutole microcapsule suspension and mesotrione suspension at a mass ratio of 1:(0.5~10).

3. The microcapsule suspension-suspension agent according to claim 1, characterized in that, The mixture includes isoxaflutole microcapsule suspension and mesotrione suspension at a mass ratio of 1:(0.5~9).

4. The microcapsule suspension-suspension agent according to claim 1, characterized in that, The mixture includes isoxaflutole microcapsule suspension and mesotrione suspension at a mass ratio of 1:(1~9).

5. The microcapsule suspension-suspension agent according to claim 1, characterized in that, The weight ratio of isoxaflutole to mesotrione is (1~7):(1~9).

6. The microcapsule suspension-suspension agent according to claim 1, characterized in that, The weight ratio of isoxaflutole to mesotrione is (1~2):(1~4).

7. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In the isoxaflutole microcapsule suspension, the weight ratio of isoxaflutole to oil phase wall material is 1:(0.05~0.5).

8. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In the isoxaflutole microcapsule suspension, the weight ratio of isoxaflutole to oil phase wall material is 1:(0.08~0.5).

9. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In the isoxaflutole microcapsule suspension, the weight ratio of isoxaflutole to oil phase wall material is 1:(0.08~0.2).

10. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In the isoxaflutole microcapsule suspension, isoxaflutole is 5-45 parts by weight.

11. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In the isoxaflutole microcapsule suspension, isoxaflutole is 17-40 parts by weight.

12. The microcapsule suspension-suspension agent according to claim 10, characterized in that, In the isoxaflutole microcapsule suspension, the polycarboxylate and sodium lignosulfonate are 3 to 8 parts by weight.

13. The microcapsule suspension-suspension agent according to claim 10, characterized in that, In the isoxaflutole microcapsule suspension, the polycarboxylate and sodium lignosulfonate are 4-6 parts by weight.

14. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In isoxaflutole microcapsule suspensions, the oil phase wall material accounts for 3-5%.

15. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In isoxaflutole microcapsule suspensions, the oil phase wall material accounts for 3-4.5%.

16. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In the isoxaflutole microcapsule suspension, the aqueous phase wall material is 0.1 to 1.0 parts by weight.

17. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In isoxaflutole microcapsule suspension, the solvent oil is 3-10 parts by weight.

18. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In the isoxaflutole microcapsule suspension, the solvent oil is 3-5 parts by weight.

19. The microcapsule suspension-suspension agent according to claim 17, characterized in that, In the isoxaflutole microcapsule suspension, the solvent oil is one or more of solvent oil 100#, solvent oil 150#, and solvent oil 200#.

20. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In the isoxaflutole microcapsule suspension, the thickener is 0.05 to 0.1 parts by weight.

21. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In the isoxaflutole microcapsule suspension, xanthan gum is used as the thickener.

22. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In the isoxaflutole microcapsule suspension, the preservative content is 0.1 to 0.2 parts by weight.

23. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In isoxaflutole microcapsule suspension, the preservative is a thiazolinone preservative.

24. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In isoxaflutole microcapsule suspension, the preservative is methylisothiazolinone.

25. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In isoxaflutole microcapsule suspension, the specific gravity adjuster is 3 to 5 parts by weight.

26. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In isoxaflutole microcapsule suspension, the specific gravity regulator is anhydrous calcium chloride.

27. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In isoxaflutole microcapsule suspension, the antifreeze agent is ethylene glycol.

28. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In the isoxaflutole microcapsule suspension, water is added to bring the total weight to 100 parts.

29. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In the aqueous suspension of metolachlor, the amount of metolachlor is 20-50 parts by weight.

30. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In the metolachlor aqueous suspension, metolachlor is present in 30-40 parts by weight.

31. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In the mesotrione aqueous suspension, the thickener is 0.05 to 0.1 parts by weight.

32. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In the metolachlor aqueous suspension, the thickener is xanthan gum.

33. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In the aqueous suspension of metolachlor, the preservative content is 0.1 to 0.2 parts by weight.

34. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In the metolachlor aqueous suspension, the preservative is a thiazolinone preservative.

35. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In the aqueous suspension of metolachlor, the preservative is methylisothiazolinone.

36. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In mesotrione aqueous suspension, the antifreeze content is 1-3%.

37. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In the aqueous suspension of metolachlor, the antifreeze agent is ethylene glycol.

38. The microcapsule suspension-suspension agent according to any one of claims 1 to 6, characterized in that, In the metolachlor aqueous suspension, water is added to bring the total to 100 parts by weight.

39. A method for preparing a microcapsule suspension-suspension agent according to any one of claims 1 to 38, characterized in that, Includes the following steps: 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 metolachlor aqueous suspension: The terbutaline, dispersant, thickener, preservative, antifreeze and water are mixed and wet-milled to the target particle size to obtain metolachlor aqueous suspension. 3) Mix the materials from steps 1) and 2) to obtain microcapsule suspension-suspension agent.

40. The application of a microcapsule suspension-suspension agent according to any one of claims 1 to 38, or a microcapsule suspension-suspension agent prepared by the preparation method according to claim 39, in the control of weeds in farmland before crop planting, or after sowing and before seedling emergence, or during the crop growth period.

41. The application according to claim 40, characterized in that, The weeds include broadleaf weeds and / or grass weeds.

42. The application according to claim 40, characterized in that, The weeds are selected from at least one of the following: goosegrass, crabgrass, lambsquarters, and amaranth.

Citation Information

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