A suspension-emulsion containing prochloraz and a method for preparing the same

Abstract

The present application belongs to the technical field of new pesticides, and particularly relates to a suspension emulsion containing prochloraz and a preparation method thereof. The suspension emulsion containing prochloraz comprises active components and agriculturally acceptable adjuvants. The active components are prochloraz and fluopyram, and the adjuvants comprise one or more of solvents, emulsifiers, dispersing wetting agents, antifoaming agents, antifreezing agents and thickening agents. The solvents are composed of isooctanol and other solvents in a certain proportion. The suspension emulsion of prochloraz and fluopyram is prepared by mixing prochloraz solid technical material after pretreatment with ground fluopyram suspension concentrate. The suspension emulsion prepared by the method has a particle size D95 of less than or equal to 3 um, excellent storage stability, and is suitable for use in different temperature water and high-concentration water.

Description

Technical Field

[0001] This invention belongs to the field of novel pesticide technology and provides a suspension emulsion containing imazalil and its preparation method. Background Technology

[0002] Imazalil is a highly effective, low-toxicity, broad-spectrum imidazole fungicide developed by Boots Co., Ltd. in the UK and officially marketed by Agerford in 1977. Its mechanism of action is the inhibition of ergosterol biosynthesis. It has some systemic conductivity and provides preventative, protective, and curative effects. It can be used to control many diseases of the stems, leaves, and ears of cereal crops, such as powdery mildew, Fusarium head blight, and leaf spot. It can also control rice bakanae disease and rice blast, and can be used for seed treatment. This product can also be used to control many pathogens of fruit trees, vegetables, mushrooms, turf, and ornamental plants. It has significant control effects against various ascomycete and deuteromycete diseases of crops, such as anthracnose and leaf spot. It can be sprayed before harvesting fruit trees and vegetables or used for post-harvest storage and soaking. It can be mixed with various fungicides, insecticides, and herbicides.

[0003] Fluopyram, a succinate dehydrogenase inhibitor developed by Bayer CropScience in Germany, is a systemic fungicide. Its efficacy is readily absorbed by plants and transported to new leaves and roots, providing protection for over 80 days. It also possesses both fungicidal and nematicidal properties. Fluopyram kills pathogens by inhibiting the activity of succinate dehydrogenase in the mitochondrial electron transport chain of pathogens, interfering with respiration and hindering energy production. It is less likely to induce resistance. It is primarily used on high-value crops such as tomatoes, cucumbers, watermelons, grapes, bananas, and strawberries, and is highly effective against more than ten diseases including powdery mildew, gray mold, leaf mold, anthracnose, and sclerotinia rot.

[0004] Suspension emulsions (SE) are water-based pesticide formulations. They consist of a water-insoluble solid active ingredient and an oily liquid active ingredient (or their solution), uniformly dispersed in water with adjuvants to form a highly suspended emulsion system. The active ingredient particle size is typically less than 5 μm, combining the characteristics of both suspension concentrates (SC) and concentrated emulsions (CE). Its core features are: (i) a two-phase dispersion system: simultaneously containing a solid phase (solid active ingredient) and an oil phase (liquid active ingredient), both stably dispersed in the aqueous phase; (ii) environmentally friendly: using water as a medium significantly reduces the use of organic solvents, lowering toxicity to the environment and animals; (iii) safe storage and transportation: non-flammable and non-explosive, aligning with the trend of green pesticide development; and (iv) efficacy advantages: can be compounded with various pesticides, and its concentrated emulsion portion not only promotes pesticide absorption but also prolongs pesticide retention.

[0005] Chinese invention patent CN104222118B describes examples 19-21 as suspensions of fluopyram and prochloraz, and examples 28-30 as emulsions of fluopyram and prochloraz. These combinations show good control effects against wheat powdery mildew, cucumber downy mildew, and tomato blight. However, the preparation method of these combinations is not detailed. Prochloraz technical grade (industrial purity approximately 97%) is a light brown waxy solid at room temperature, turns into a yellowish-brown liquid when heated to about 75°C, and solidifies upon cooling. If the purity is >99%, its melting point is around 50°C, making it difficult to dissolve in water or conventional surfactants. Suspensions and emulsions prepared using conventional methods with untreated prochloraz have poor stability and application performance.

[0006] During further research on the preparation of prochloraz and fluopyram suspension emulsions, the inventors discovered the following problems: ① The product has high viscosity at room temperature, poor fluidity, poor emulsification and dispersion, and cannot be uniformly dispersed in water; ② The product has poor low-temperature performance, solidifying into lumps when stored below 5℃, and leaving a large number of undissolved particles after dilution with water; ③ Poor storage stability, easily separating into oil and solid phases when stored at 54℃; ④ Poor adaptability to dilution with water, unable to be uniformly dispersed in water below 30℃, affecting normal spraying use; ⑤ Poor stability when diluted with water at high concentrations, making it unsuitable for aerial spraying.

[0007] Therefore, developing a suspension emulsion that addresses the above issues, is highly fluid, easy to use, stable in storage, adaptable to different environments and water qualities, and can be diluted at high concentrations for aerial spraying, is essential for bringing prochloraz and fluopyram suspension emulsions to market. Summary of the Invention

[0008] To address the aforementioned shortcomings of existing technologies, this invention provides a suspension emulsion containing prochloraz and its preparation method. The prochloraz solid technical material is pretreated and then mixed with ground fluopyram suspension to obtain a prochloraz and fluopyram suspension emulsion. The suspension emulsion obtained by this method has a particle size D95≤3um, excellent storage stability, and is suitable for use in waters with different temperatures and qualities, as well as for high-concentration dilution.

[0009] After numerous experiments and gradual exploration, the inventor discovered that: The technical challenge in preparing prochloraz and fluopyram suspensions lies in the pre-preparation of the prochloraz oil phase. While prochloraz is soluble in some organic solvents, if the solidified prochloraz technical is added to an organic solvent before melting, it is difficult to completely dissolve at room temperature. Even when heated to 54°C, the prochloraz technical still cannot completely become a liquid. Furthermore, if the chosen solvent or emulsifier is unsuitable, even if prochloraz is completely melted at high temperature and then mixed with solvent and emulsifier, solid prochloraz will clearly precipitate within 24 hours at room temperature or low temperature. If the high-temperature melted prochloraz technical is directly added to an aqueous suspension, the prochloraz instantly becomes viscous and solidifies, and even with the addition of solvent and emulsifier at room temperature, it is difficult to melt into a homogeneous flowing liquid. According to the inventors' tests, if isooctanol is used to dissolve prochloraz technical (solid, 97.2% by mass), it takes more than 8 hours to dissolve 25 grams of prochloraz technical with 100 grams of isooctanol at room temperature (25±2°C), which cannot meet production requirements.

[0010] Especially in this invention, where the imazalil content is high and the solvents used are mismatched, the resulting suspension emulsion, even when forcibly mixed with the water phase by external force, is extremely unstable. The oil phase precipitates upon heating and solidifies entirely upon cooling. Therefore, the oil phase in this application's technical solution is a rational combination of isooctanol and organic solvents. Isooctanol is readily soluble in organic solvents and has a certain solubility for imazalil, serving not only as a solvent but also exhibiting cold-resistant and low-temperature-resistant properties. This solvent combination significantly improves the drawback of low-temperature agglomeration of the oil phase, representing a significant improvement over using isooctanol alone. Furthermore, the emulsifier selected for the oil phase, through the addition of the special auxiliary agent poly(ethylene oxide)-poly(propylene oxide) monobutyl ether, ensures both the overall emulsifying performance of the formulation and improves the overall stability of the suspension emulsion. Polyethylene oxide polypropylene oxide monobutyl ether is soluble in both water and organic solvents. When it comes into contact with an oil-water mixture, it will oriented like a bridge at the oil-water interface, with the lipophilic group inserted into the oil phase and the hydrophilic group extended into the water phase. This arrangement significantly reduces the interfacial tension between oil and water, making it easier for the oil to be dispersed into tiny droplets during stirring, rather than agglomerating into flakes. Therefore, it can bind the oil and water phases more firmly, and the structure is not easily destroyed.

[0011] The prochlorazin and fluopyram suspension emulsions prepared in this invention utilize a nonionic acrylic copolymer combined with an ionic or sterically hindered dispersing and wetting agent in the fluopyram suspension. When tiny droplets dispersed by external shearing and stirring in the oil phase encounter the suspension, they quickly form a microstructure similar to an "oil-in-water" structure under the action of multiple adjuvants. Microscopic observation reveals only the fine fluopyram active ingredient, without any trace of oil droplets. The possible reason is that the ionic adjuvant in the fluopyram suspension causes the droplet surface to carry the same charge, preventing the oil droplets from aggregating through the principle of "like charges repelling each other"; while the hydrophilic groups of the nonionic adjuvant bind with water molecules to form a tight hydration layer, which acts as a buffer to prevent the oil droplets from contacting each other. Therefore, the prochloraz and fluopyram suspension emulsions prepared by this invention have an aqueous continuous phase that maintains low-temperature fluidity and can be uniformly emulsified and dispersed at water temperatures of 5-30℃. During use, the carboxylic acid groups in the acrylic copolymer can form chemical adsorption with the surface of the drug solution and chelate calcium and magnesium ions in the water, thereby improving the dispersion stability of the drug solution and reducing flocculation. This ensures that the prochloraz and fluopyram suspension emulsions prepared by this invention can be used normally even in high-concentration diluted water or hard water, and are suitable for use in various methods such as mechanical spraying and aerial spraying.

[0012] Based on the above inventive concept, the specific technical solution of the present invention is as follows: A suspension emulsion containing prochloraz includes an active ingredient and agriculturally acceptable adjuvants; the active ingredient is prochloraz and fluopyram, and the adjuvants include one or more of solvents, emulsifiers, dispersants and wetting agents, defoamers, antifreeze agents, and thickeners; the solvent is composed of isooctanol and other solvents in a certain proportion.

[0013] As one specific implementation method, the mass ratio of isooctanol to other solvents is 5:1 to 1:5.

[0014] In a preferred embodiment, the other solvent is one or more of ethylene glycol diacetate, xylene, solvent oil 150#, and rosin-based vegetable oil.

[0015] As a further preferred embodiment, other solvents are ethylene glycol diacetate, xylene, and solvent oil 150#.

[0016] In the most preferred embodiment, the other solvent is ethylene glycol diacetate.

[0017] As one specific implementation method, the content of active ingredients is 30%-45% by weight, of which imazalil is 20%-40% and fluopyram is 1%-10% by weight.

[0018] As one specific implementation method, the weight ratio of imazalil to fluopyram is 2:1-30:1.

[0019] As a preferred embodiment, the weight ratio of imazalil to fluopyram is 3:1 to 8:1.

[0020] In the most preferred embodiment, the weight ratio of imazalil to fluopyram is 6:1 to 7:1.

[0021] As one specific implementation, the composition of the suspension emulsion by weight percentage is as follows: Imazalil 20%-40%; Fluopyram 1%-10%; Solvent 10%-20%; Emulsifier 6%-10%; Dispersant wetting agent 5%-10%; Defoamer 0.2%-0.5%; Antifreeze 4%-6%; Thickener 0.1%-2.0%; Add deionized water to make up the remaining amount.

[0022] In a preferred embodiment, the emulsifier is one or more of castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, phenethylphenol formaldehyde resin polyoxyethylene ether, phenethylphenol polyoxyethylene ether, and polyethylene oxide polyoxypropylene monobutyl ether.

[0023] As a more preferred embodiment, the emulsifier is one of polyethylene oxide polypropylene oxide monobutyl ether, castor oil polyoxyethylene ether, and phenethylphenol formaldehyde resin polyoxyethylene ether.

[0024] In a specific embodiment, the dispersing and wetting agent is one or more of the following: polycarboxylate dispersant, sulfate ester and its salt dispersant, phosphate ester and its salt dispersant, acrylic copolymer, polymer, separating powder, and sodium dodecyl sulfate.

[0025] Among them, the polycarboxylate dispersants and wetting agents are selected from SP-27001 (Jiangsu Qingyu), HDB-1011T (Chuzhou Debang), SP-SC3275 (Jiangsu Qingyu), and DS-68 (Desheng Fine Chemical); the sulfate esters and their salts are selected from DISPER RYD982 (Suzhou Rongyida); the phosphate esters and their salts are selected from DISPER RYD981 (Suzhou Rongyida), HDB-SC2020 (Chuzhou Debang), DS-3036 (Desheng Fine Chemical), and Soprophor SC (Rhodia); the polymers are selected from G5000 (Codex, UK), DISPER D1000 (Suzhou Rongyida), and HDB-1035 (Chuzhou Debang); and the acrylic copolymers are selected from WINST3791 (Shanghai Keying) and MK-2700 (Desheng Fine Chemical). More preferably, the dispersing and wetting agent is selected from WINST3791, DISPER RYD981, HDB-SC2020, DISPERD1000, DISPER RYD982, and SP-SC3275; most preferably, the dispersing and wetting agent is selected from WINST3791.

[0026] As a preferred embodiment, the defoamer is polydimethylsiloxane, such as Sag 1522.

[0027] Preferably, the thickener is one or more of xanthan gum, magnesium aluminum silicate, and organobentonite.

[0028] Preferably, the antifreeze is one or more of ethylene glycol, propylene glycol, and glycerol. More preferably, it is ethylene glycol.

[0029] In addition, and more importantly, the inventors have also provided a method for preparing the suspension emulsion, the specific steps of which are as follows: 1) Preparation of prochloraz stock solution: Heat prochloraz technical to 70℃-80℃ to completely melt it into liquid, add solvent and mix evenly, then add emulsifier and mix thoroughly to obtain prochloraz stock solution for later use. 2) Preparation of fluopyram suspension mother liquor: Dispersant, wetting agent, thickener, antifreeze and defoamer are added to fluopyram technical material, then a certain amount of deionized water is added, mixed evenly, and then put into a sand mill for grinding until the particle size D95≤3um. After grinding is completed, fluopyram suspension mother liquor is obtained. 3) Preparation of prochloraz and fluopyram suspension emulsion: The prochloraz mother liquor and the ground fluopyram mother liquor are sheared and stirred evenly to obtain a suspension emulsion containing prochloraz and fluopyram.

[0030] As a preferred embodiment, the shearing speed in step (3) is 1500±300 rpm, no oil droplets are observed under a microscope, and the particle size D95 is measured to be ≤3.0um.

[0031] As a preferred embodiment, the temperature during the grinding process in step (2) is controlled between 20-30°C.

[0032] The imazalil technical used in this application has a mass fraction of 97.2% and is a solid wax in its room temperature state at around 25°C.

[0033] The above method for preparing prochloraz and fluopyram suspension emulsions, although involving a mixture of oil and water phases, significantly improves production efficiency through pretreatment of prochloraz technical. Various combinations of oil and solid phase additives (especially solvents) enhance sample stability and versatility, allowing for use in different water qualities and temperatures. High-speed shearing ensures the oil phase forms sufficiently small droplets to be fully coated by the water phase, improving not only sample flowability but also low-temperature storage stability.

[0034] Compared with the prior art, the bactericide composition provided by the present invention can produce the following beneficial effects: 1. The imazalil and fluopyram suspension emulsion samples prepared by this invention have good fluidity at room temperature and low viscosity (around 500 mPa·s when tested at 25℃ with a No. 2 rotor at 30 revolutions), which facilitates production and packaging; the particle size is small, with D95≤3um.

[0035] 2. The obtained imazalil and fluopyram suspension emulsions have good storage stability: after 14 days of hot storage at 54℃, there is no oil-water separation, no stickiness, no bottoming, no clumping, etc.; after 14 days of cold storage at 0℃, the fluidity is good and does not affect the emulsification and dispersion in water, and it can be used normally; after 14 days of freezing at -18℃, the fluidity is restored within 2 hours after returning to room temperature, and it is uniformly dispersed and emulsified in water without particles or oil separation.

[0036] 3. Excellent application performance, adaptable to different water temperatures and qualities. It can emulsify normally and disperse evenly in water at 5-10℃. It can also emulsify and disperse rapidly when diluted 100 times in soft or hard water at 15℃. It is widely used in all seasons in both the north and south. It has excellent suspension performance. Even after 200 times dilution or 20 times dilution, it remains in suspension for 2 hours without the deposition of original drug particles. It can be used for aerial spraying. Detailed Implementation

[0037] The following detailed description of the present invention through specific embodiments should not be construed as limiting the scope of the invention to the following examples. All technologies implemented based on the above-described content of the present invention fall within the scope of the present invention. All percentages below are by weight, all additives used are conventional additives in the art, and the preparation methods and equipment for the corresponding dosage forms are conventional processes and equipment in the art.

[0038] Example 1: 30% prochloraz·fluopyram suspension emulsion A prochloraz·fluopyram suspension emulsion (prochloraz and fluopyram by mass fractions of 25% and 5% respectively) has the following weight ratio: .

[0039] Example 2: 35% prochloraz·fluopyram suspension emulsion A prochloraz·fluopyram suspension emulsion (prochloraz and fluopyram by mass fractions of 28% and 7% respectively) has the following weight ratio: .

[0040] Example 3: 40% prochloraz·fluopyram suspension emulsion A prochloraz·fluopyram suspension emulsion (prochloraz and fluopyram by mass fractions of 35% and 5% respectively) has the following weight ratio: .

[0041] Example 4: 42% prochloraz·fluopyram suspension emulsion A suspension concentrate containing fluopyram and imazalil (imazalil and fluopyram by mass fractions of 36% and 6% respectively), with the following weight ratio: .

[0042] Example 5: 45% prochloraz·fluopyram suspension emulsion A suspension concentrate containing fluopyram and imazalil (imazalil and fluopyram by mass fractions of 40% and 5% respectively), with the following weight ratio: .

[0043] Comparative Example 1: 40% prochloraz·fluopyram suspension emulsion A prochloraz·fluopyram suspension emulsion (prochloraz and fluopyram by mass fractions of 35% and 5% respectively) has the following weight ratio: Compared to Example 3, the solvent used in the oil phase of Imazalil in Comparative Example 1 was ethylene glycol diacetate, without the addition of isooctanol.

[0044] Comparative Example 2: 40% prochloraz·fluopyram suspension emulsion A prochloraz·fluopyram suspension emulsion (prochloraz and fluopyram by mass fractions of 35% and 5% respectively) has the following weight ratio: The difference between Comparative Example 2 and Example 3 is that the ratio of isooctyl alcohol to ethylene glycol diacetate in Example 3 was adjusted from 1:2 to 1:14.

[0045] Experiment Example 1: The test was conducted using the following method: 1. The suspension rate of the active ingredient fluopyram was determined according to the method in GB / T14825-2023; 2. Thermal storage stability of pesticides: The samples were stored at (54±2)℃ for 14 days to test whether the samples had clumping or stratification, i.e., separation of oil phase and solid phase. 3. Cold storage stability: Store at (0±2)℃ for 14 days, mainly observe the state of the sample, whether it can flow, and whether there is crystallization or agglomeration; 4. Freezing stability: After storing at (-18±2)℃ for 7 days, observe the sample state after restoring to room temperature for 2 hours to check for flowability and the presence of crystallization or agglomeration. Examples 1-5 and Comparative Examples 1-2 were subjected to hot and cold storage experiments; specific data are shown in Table 1. Table 1. Stability Comparison of Examples and Comparative Examples By comparing the above Examples 1-5 with Comparative Examples 1-2, the suspension rate of the samples in Examples 1-5 can all be above 99%.

[0046] Comparative Example 1 had a particle size of D95=7.6um and a significantly reduced suspension rate. Its storage stability under various conditions was very different from that of Example 3. The suspension rate of para-dichlorophenamine was significantly reduced, indicating that the oil phase emulsification and dispersion performance was poor when isooctanol solvent was not used.

[0047] Compared with Example 3, Comparative Example 2 changed the ratio of isooctanol to ethylene glycol diacetate, and the particle size was larger. Microscopic observation showed that small oil droplets appeared in the formulation, indicating that the ratio of solvents not only affects the storage stability of the formulation, but also affects the overall particle size change and suspension rate of the formulation.

[0048] Example 2: The dispersion and suspension properties of a formulation in water are important indicators for evaluating its application performance. This test consists of two steps: (1) Emulsification and dispersion performance in different water temperatures and water qualities. The agent was diluted 100 times with soft water at 8℃, 15℃ and 30℃ and standard hard water, respectively, and the complete and uniform emulsification and dispersion were observed. The specific data are shown in Table 2.

[0049] (2) Suspension performance in different water temperatures and qualities. The reagent was diluted 100 times with soft water at 15℃ and 30℃ and standard hard water, respectively, and placed in a 100ml stoppered graduated cylinder for 2 hours. Flocculation, stratification, and sedimentation were observed. The reagent was diluted 20 times with standard hard water at 15℃ and 30℃, and placed in a 100ml stoppered graduated cylinder for 2 hours. Stratification, sedimentation, and oil separation were observed. Water stability experiments were conducted on Examples 1-5 and Comparative Examples 1-2. Specific data are shown in Table 3. Table 2 Comparison of emulsification and dispersion properties of the examples and comparative examples Table 3. Comparison of water stability in the examples and comparative examples Through the above comparative experiments, Examples 1-5 all exhibited excellent suspension performance in water at both temperatures within 2 hours. Comparative Examples 1 and 2, due to poor low-temperature performance, showed incomplete emulsification and dispersion in low-temperature water, resulting in varying degrees of precipitation or floating oil after standing for 2 hours. These performance comparisons demonstrate that the type and ratio of solvent in the prochloraz oil phase significantly affect the storage stability and dilution performance of the prochloraz·fluopyram suspension.

[0050] Application Example 1: Comparative test on the control effect of prochloraz·fluopyram suspension emulsion on wheat scab.

[0051] Test Location: Shandong Jingbo Agricultural Chemical Technology Co., Ltd. Bio-testing Base Test subject: Wheat scab Test materials: formulation samples for both the example and comparative examples.

[0052] Experimental Design: Environmental conditions were consistent across all treatments during the experiment, with sunny weather. All experimental plots were of the same size, with a plot area of ​​20 m². 2 (10 meters long, 2 meters wide). Eight treatments were set up, including examples and comparative examples, with four replicates for each treatment and intervals between treatments. The dosage was 13g of active ingredient per acre (based on two technical grade pesticides), and the water consumption per plot was 1.5 liters (i.e., 750 liters / hectare). Foliar spraying was applied at the early stage of wheat disease. A five-point sampling method was used, with five points randomly selected from each plot, and 100 ears surveyed at each point.

[0053] The control effect was calculated according to the "Guidelines for Field Efficacy Testing of Pesticides" (GB / T 17980.30).

[0054] 1. Disease Grading Standards During the survey, the area affected by the disease should be classified into grades (0-7) according to the proportion of the entire ear of grain. Level 0: Disease-free throughout the entire ear of grain; Level 1: Infected ear area / total ear area < 1 / 4; Level 3: Infected ear area / Total ear area = 1 / 4 - 1 / 2; Level 5: Infected ear area / Total ear area = 1 / 2 - 3 / 4; Level 7: Infected ear area / total ear area > 3 / 4. 2. Key performance indicator calculation formula: Disease incidence rate (%) = (Number of diseased ears / Total number of ears surveyed) × 100 Disease index = [∑(number of diseased ears at each level × corresponding level value) / (total number of ears surveyed × 7)] × 100 Control efficacy (%) = (Disease index in blank control area - Disease index in drug-treated area) / Disease index in blank control area × 100 Table 4. Control efficacy of prochloraz·fluopyram suspension emulsion against wheat scab. .

[0055] Application Example 2: Comparative Test of the Control Effect of Prochloraz·Fluoropyram Suspension Emulsion on Tomato Anthracnose Test location: Dongyang Village, Chengdong Subdistrict, Boxing County, Shandong Province Test subject: Tomato anthracnose Test materials: formulation samples for both the example and comparative examples.

[0056] Experimental Design: This experiment used open-field tomato cultivation, ensuring uniform crop growth. Environmental conditions were consistent across all treatments during the experiment, with sunny weather. All experimental plots were the same size, with a plot area of ​​20m². 2 (10 meters long, 2 meters wide). Eight treatments were set up, including examples and comparative examples, with four replicates for each treatment and intervals between treatments. The dosage was 15g of active ingredient per acre (based on two technical grade pesticides), and the water consumption per plot was 1.5 liters (i.e., 750 liters / hectare). Foliar spraying was carried out at the early stage of tomato fruit surface disease: five random sampling points were taken from each plot, with three plants investigated at each point, and six leaves investigated from top to bottom on each plant.

[0057] Grading method: Grade 0: No lesions; Grade 1: The lesion area accounts for less than 5% of the total leaf surface area; Grade 3: Lesions cover 6%-10% of the total leaf surface area; Level 5: Lesions cover 11%-25% of the total leaf surface area; Level 7: Lesions cover 26%-50% of the total leaf surface area. Level 9: The lesion area accounts for more than 51% of the total leaf area.

[0058] Methods for calculating drug efficacy Disease index = [∑(number of diseased leaves at each level × corresponding level value) / (total number of leaves surveyed × 9)] × 100 Control efficacy (%) = [1 - (Disease index before application in the blank control area × Disease index after application in the treated area) / (Disease index after application in the blank control area × Disease index before application in the treated area)] × 100 Table 5. Control efficacy of prochloraz·fluopyram suspension emulsion against tomato anthracnose. Through the above two application examples, the efficacy of Examples 1-5 against wheat scab and tomato anthracnose reached its optimal state 14 days after application, with control efficiencies approaching or exceeding 90%, indicating that prochloraz and fluopyram suspension emulsions exhibited excellent control efficacy at this time. In contrast, the suspension emulsions in Comparative Examples 1 and 2 had high viscosity, uneven dispersion, and poor emulsification, resulting in larger droplets that easily slipped, affecting crop absorption and translocation. Furthermore, the high amount of active ingredient precipitation led to low pesticide utilization and poor efficacy.

[0059] Based on the comprehensive evaluation of the above formulation performance test examples and application effects, the formulation and preparation method of the prochloraz·fluopyram suspension emulsion provided by this invention have high production efficiency, excellent formulation stability and application effects, are green and environmentally friendly, are stable in storage, are not prone to clumping, and have wide applications. It has broad reference value for promoting the compound products of prochloraz and fluopyram.

[0060] This invention demonstrates and describes the basic principles, product characteristics, and advantages of the method for preparing prochloraz·fluopyram suspension emulsion. This invention is not limited to the above embodiments; various changes and modifications can be made without departing from the scope of this invention, and all such changes are claimed to be included within the scope of protection.

Claims

1. A suspension emulsion containing prochloraz, comprising an active ingredient and agriculturally acceptable adjuvants; said active ingredient being prochloraz and fluopyram, said adjuvants comprising one or more of solvents, emulsifiers, dispersants, wetting agents, defoamers, antifreeze agents, and thickeners, characterized in that, The solvent is composed of isooctanol and other solvents in a certain proportion.

2. The suspension emulsion according to claim 1, characterized in that: The mass ratio of isooctanol to other solvents is 5:1 to 1:5; the other solvents are one or more of ethylene glycol diacetate, xylene, solvent oil 150#, and rosin-based vegetable oil; preferably, the other solvents are ethylene glycol diacetate, xylene, and solvent oil 150#; most preferably, the other solvents are ethylene glycol diacetate.

3. The suspension emulsion according to claim 1, characterized in that: The content of active ingredients is 30%-45% by weight, of which imazalil is 20%-40% and fluopyram is 1%-10% by weight.

4. The suspension emulsion according to claim 1, characterized in that: The weight ratio of prochloraz to fluopyram is 2:1-30:1; preferably, the weight ratio of prochloraz to fluopyram is 3:1-8:1; preferably, the weight ratio of prochloraz to fluopyram is 6:1-7:

1.

5. The suspension emulsion according to claim 1, characterized in that, The composition of the suspension emulsion, by weight percentage, is as follows: Imazalil 20%-40%; Fluopyram 1%-10%; Solvent 10%-20%; Emulsifier 6%-10%; Dispersant wetting agent 5%-10%; Defoamer 0.2%-0.5%; Antifreeze 4%-6%; Thickener 0.1%-2.0%; Add deionized water to make up the remaining amount.

6. The suspension emulsion according to claim 1 or 5, characterized in that: The emulsifier is one or more of castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, phenethylphenol formaldehyde resin polyoxyethylene ether, phenethylphenol polyoxyethylene ether, and polyethylene oxide polyoxypropylene monobutyl ether; preferably, the emulsifier is one of polyethylene oxide polyoxypropylene monobutyl ether, castor oil polyoxyethylene ether, and phenethylphenol formaldehyde resin polyoxyethylene ether.

7. The suspension emulsion according to claim 1 or 5, characterized in that: The dispersing and wetting agent is one or more of the following: polycarboxylic acid dispersant, sulfate ester dispersant, phosphate ester dispersant, acrylic copolymer, polymer, separating powder, and sodium dodecyl sulfate.

8. The suspension emulsion according to claim 1 or 5, characterized in that: The defoamer is polydimethylsiloxane; the thickener is one or more of xanthan gum, magnesium aluminum silicate, and organobentonite; and the antifreeze is one or more of ethylene glycol, propylene glycol, and glycerol.

9. The method for preparing the suspension emulsion containing imazalil according to claim 1, characterized in that, The specific preparation steps are as follows: 1) Preparation of prochloraz stock solution: Heat prochloraz technical to 70℃-80℃ to completely melt it into liquid, add solvent and mix evenly, then add emulsifier and mix thoroughly to obtain prochloraz stock solution for later use. 2) Preparation of fluopyram suspension mother liquor: Dispersant, wetting agent, thickener, antifreeze and defoamer are added to fluopyram technical material, then a certain amount of deionized water is added, mixed evenly, and then put into a sand mill for grinding until the particle size D95≤3um. After grinding is completed, fluopyram suspension mother liquor is obtained. 3) Preparation of prochloraz and fluopyram suspension emulsion: The prochloraz mother liquor and the ground fluopyram mother liquor are sheared and stirred to mix evenly, thus obtaining a suspension emulsion containing prochloraz and fluopyram.

10. The method for preparing the suspension emulsion containing imazalil according to claim 9, characterized in that: In step (3), the shearing speed is 1500±300 rpm, no oil droplets are observed under a microscope, and the particle size D95 is measured to be ≤3.0um; preferably, the temperature is controlled between 20-30℃ during the grinding process in step (2).

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