A pesticide emulsifiable concentrate containing fluorine-containing acaricide, a preparation method and application thereof
By using a specific ratio of compound solvent and emulsifier, flufenoxuron emulsifiable concentrate was prepared, which solved the problem of high decomposition rate of active ingredients and achieved high stability and high efficiency in controlling mites.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- HAILIR PESTICIDES & CHEM GRP
- Filing Date
- 2026-03-03
- Publication Date
- 2026-06-05
AI Technical Summary
Existing flufenoxuron emulsifiable concentrates have high decomposition rates of active ingredients and poor stability, making it difficult to balance the physical stability of the formulation with its efficacy against the target.
By using a specific ratio of composite solvent and composite emulsifier, flufenoxuron emulsifiable concentrate was prepared, which reduced the decomposition rate of the active ingredient and improved the emulsification effect and stability.
It effectively reduces the decomposition rate of flufenoxuron emulsifiable concentrate, improves the wetting and spreading ability of diluted pesticide solutions, enhances the control efficacy against target mites, and remains stable under high-temperature storage.
Smart Images

Figure SMS_1 
Figure SMS_2
Abstract
Description
Technical Field
[0001] This invention belongs to the field of pesticide acaricide technology, and relates to a pesticide emulsifiable concentrate containing flufenoxuron, its preparation method and its application. Background Technology
[0002] Emulsifiable concentrates (ECs) of pesticides play a vital role in agricultural production. ECs have a simple composition, generally requiring only three components: the pesticide technical, an organic solvent, and an emulsifier. They can be prepared by slow stirring in a reaction vessel, requiring no complex equipment and resulting in relatively low processing costs. ECs exhibit high biological activity, with their active ingredients evenly distributed onto the crop surface along with the pesticide solution, providing good wetting and adhesion, leading to high control efficacy. Furthermore, ECs have good storage stability and are convenient to use.
[0003] The decomposition rate of pesticide active ingredients is a key technical indicator for evaluating the stability of pesticide formulations. The appearance and efficacy of pesticide formulations largely depend on the decomposition rate of the active ingredients, i.e., their stability. Emulsifiable concentrates (ECCs) generally require a decomposition rate of less than 5%. However, finding suitable conditions for the adjuvant system to stabilize the active ingredients and avoid significant decomposition of pesticide components is very difficult. To address the decomposition problem of active ingredients in ECCs, the selection and ratio of emulsifiers and solvents are crucial. Using specific emulsifiers and solvents can reduce the decomposition rate of active ingredients. In flufenoxuron EC formulations, the type and amount of emulsifiers and solvents not only determine the decomposition of the active ingredients but also the stability, wetting, and spreading properties of the diluted flufenoxuron EC solution. The performance of the diluted solution directly determines the efficacy of the flufenoxuron EC.
[0004] Good pesticide formulations must balance physical stability and efficacy against the target. How to achieve both low decomposition rate of active ingredient and good efficacy in the development of flufenoxuron emulsifiable concentrate is an important problem that needs to be solved. Summary of the Invention
[0005] To address the aforementioned issues, this invention provides a flufenoxuron emulsifiable concentrate prepared from a rational composite solvent and a composite emulsifier. It is primarily used for the control of mites and features a rational component system, low decomposition rate of active ingredients, good emulsification effect, and good low-temperature and thermal storage stability. It meets the quality standards for emulsifiable concentrate products and exhibits significant efficacy against target mites.
[0006] To achieve the above objectives, the present invention adopts the following technical solution: a pesticide emulsifiable concentrate containing flufenoxuron, wherein the emulsifiable concentrate is composed of the following components by weight percentage: flufenoxuron 1-50%, compound emulsifier 1-30%, and the balance being a compound solvent.
[0007] Furthermore, the emulsifiable concentrate is composed of the following components by weight percentage: 5-40% flufenoxuron, 12-25% compound emulsifier, and the balance being a compound solvent.
[0008] Furthermore, the emulsifiable concentrate contains 8% to 30% by weight of flufenoxuron.
[0009] Furthermore, the weight percentage of flufenoxuron in the emulsifiable concentrate is 10%, 12%, 15%, 18%, 20%, 21%, 24%, or 30%. Furthermore, the composite solvent comprises solvent A, rosin-based vegetable oil, and solvent B; solvent B is one or more of tricresylbenzene, propylene carbonate, or solvent oil.
[0010] Furthermore, the mass ratio of solvent A to solvent B in the composite solvent is 5:1 to 1:2.
[0011] Furthermore, the mass ratio of solvent A to solvent B in the composite solvent is 4:1 to 1:1.
[0012] Furthermore, the mass ratio of solvent A to solvent B in the composite solvent is 40:35, 44:31, 40:20, 45:19.5, 45:15.5, 43:14, 42:12, or 44:11. Furthermore, the composite emulsifier includes polyoxyethylene ethers and sulfonates.
[0013] Furthermore, the polyoxyethylene ethers are one or more of lauryl alcohol polyoxyethylene ether, isotridecyl alcohol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, and triphenylethylphenol polyoxyethylene ether, and the sulfonates are sodium alkyl aryl sulfonate, calcium dodecylbenzene sulfonate, and sodium naphthalene sulfonate formaldehyde condensate.
[0014] Furthermore, the content of the composite emulsifier in the emulsifiable concentrate is 13% to 25%; the content of polyoxyethylene ethers in the emulsifiable concentrate is 10.5% to 17%; and the content of sulfonates in the emulsifiable concentrate is 2% to 10%. Furthermore, the mass ratio of polyoxyethylene ethers to sulfonates in the emulsifier is 2:1 to 10:1.
[0015] This invention also discloses the application of the emulsifiable concentrate described above in the prevention and control of agricultural, forestry, and horticultural mites.
[0016] Furthermore, the harmful mites mentioned are spider mites and malariae mites; The spider mite pests mentioned are *Tetranychus citrus*, *Tetranychus carmine*, *Tetranychus two-spotted*, *Tetranychus squarrosa*, *Tetranychus hawthorn*, *Tetranychus truncatus*, and *Tetranychus maculata*; the gall mite pests mentioned are *Tetranychus citrus*, *Tetranychus lycopersicum*, and *Tetranychus gracilis*.
[0017] The present invention also discloses a method for preparing an emulsifiable concentrate containing flufenoxuron, wherein metered flufenoxuron and a composite solvent are added to a mixing vessel to dissolve them, a composite emulsifier is added, the solvent is added to make up the difference, the mixture is stirred evenly, and then filtered to obtain the final product.
[0018] The present invention has the following advantages: The flufenoxam emulsifiable concentrate of this invention effectively reduces the decomposition rate of flufenoxam emulsifiable concentrate products through the mixed use of specific emulsifiers and specific solvents, resulting in good emulsification effect and high stability during high-temperature storage. The diluted flufenoxam emulsifiable concentrate of this invention has a smaller particle size and better wetting and spreading ability, thereby improving the control efficacy against target mites. Detailed Implementation
[0019] To better understand the essence of the present invention, the following detailed description of the present invention is provided in conjunction with embodiments. The contents mentioned in the embodiments are not intended to limit the present invention. The following description is only used to explain the present invention. Any modifications, substitutions or improvements made without departing from the spirit and principles of the present invention shall fall within the scope of protection claimed by the present invention.
[0020] Formulation preparation example: The following preparation methods are as follows: add the measured amount of flufenoxuron, wetting and penetrating agent, stabilizer and solvent into the mixing vessel to dissolve them, then add the emulsifier, make up the amount with solvent, stir evenly, and filter to obtain the final product.
[0021] Preparation Example 1: 10% Flufenoxam Emulsifiable Concentrate Formula composition: 10% flufenoxuron, 13% isotridecyl alcohol polyoxyethylene ether (1306, Wanhua Chemical), 2% calcium dodecylbenzenesulfonate (Nongru 500, Jiangsu Zhongshan Chemical), 40% rosin-based vegetable oil (ND-60, Jinan Fuer Chemical), and 35% trimethylbenzene.
[0022] Comparative Example 1-1: 10% Flufenoxam Emulsifiable Concentrate Formula composition: 10% flufenoxuron, 13% isotridecyl alcohol polyoxyethylene ether (1306, Wanhua Chemical), 2% calcium dodecylbenzenesulfonate (Nongru 500, Jiangsu Zhongshan Chemical), and 75% rosin-based vegetable oil (ND-60, Jinan Fuer Chemical).
[0023] Comparative Examples 1-2: Fluorosulfuron 10%, isotridecyl alcohol polyoxyethylene ether (1306, Wanhua Chemical) 13%, calcium dodecylbenzenesulfonate (Nongru 500, Jiangsu Zhongshan Chemical) 2%, and trimethylbenzene 75%.
[0024] Comparative Examples 1-3: Fluorosulfuron 10%, isotridecyl alcohol polyoxyethylene ether (1306, Wanhua Chemical) 13%, calcium dodecylbenzenesulfonate (Nongru 500, Jiangsu Zhongshan Chemical) 2%, rosin-based vegetable oil (ND-60, Jinan Fuer Chemical) 37%, and trimethylbenzene 38%.
[0025] Preparation Example 2: 12% Flufenoxam Emulsifiable Concentrate Formula composition: 12% flumethrin, 10.5% isotridecyl alcohol polyoxyethylene ether (1306, Wanhua Chemical), 2.5% sodium naphthalene sulfonate formaldehyde condensate, 44% rosin-based vegetable oil (ND-60, Jinan Fuer Chemical), and 31% No. 200 solvent oil.
[0026] Comparative Example 2-1: 12% Flufenoxam Emulsifiable Concentrate Formula composition: Fluorosulfuron 12%, isotridecyl alcohol polyoxyethylene ether (1306, Wanhua Chemical) 10.5%, sodium naphthalene sulfonate formaldehyde condensate (dispersant NNO, Jinan Sante Chemical) 2.5%, rosin-based vegetable oil (ND-60, Jinan Fuer Chemical) 36%, No. 200 solvent oil (Jinan Liyang Chemical) 39%.
[0027] Comparative Example 2-2: 12% Flufenoxam Emulsifiable Concentrate Formula composition: Fluorosulfuron 12%, isotridecyl alcohol polyoxyethylene ether (1306, Wanhua Chemical) 10.5%, sodium naphthalene sulfonate formaldehyde condensate (dispersant NNO, Jinan Sante Chemical) 2.5%, rosin-based vegetable oil (ND-60, Jinan Fuer Chemical) 61%, No. 200 solvent oil (Jinan Liyang Chemical) 14%.
[0028] Preparation Example 3: 15% Flufenoxam Emulsifiable Concentrate Formula composition: 15% flufenoxuron, 15% triphenylethylphenol polyoxyethylene ether (Nongru 601, Nanjing Taihua), 10% calcium dodecylbenzenesulfonate (Nongru 500, Jiangsu Zhongshan Chemical), 40% rosin-based vegetable oil (ND-60, Jinan Fuer Chemical), and 20% propylene carbonate.
[0029] Control Example 3-1: 15% Fludioxon Emulsifiable Concentrate Formula composition: 15% flufenoxuron, 15% triphenylethylphenol polyoxyethylene ether (Nongru 601, Nanjing Taihua), 10% calcium dodecylbenzenesulfonate (Nongru 500, Jiangsu Zhongshan Chemical), and 60% rosin-based vegetable oil (ND-60, Jinan Fuer Chemical).
[0030] Comparative Example 3-2: 15% Fludioxon Emulsifiable Concentrate Formula composition: 15% flufenoxuron, 15% triphenylethylphenol polyoxyethylene ether (agricultural emulsion 601, Nanjing Taihua), 10% calcium dodecylbenzenesulfonate (agricultural emulsion 500, Jiangsu Zhongshan Chemical), and 60% propylene carbonate.
[0031] Preparation Example 4: 18% Flufenoxam Emulsifiable Concentrate Formula composition: 18% flufenoxuron, 14% lauryl alcohol polyoxyethylene ether (AEO-9, Nanjing Taihua), 3.5% calcium dodecylbenzenesulfonate (agricultural emulsion No. 500, Jiangsu Zhongshan Chemical), 45% rosin-based vegetable oil (ND-60, Jinan Fuer Chemical), and 19.5% No. 200 solvent oil (Jinan Liyang Chemical).
[0032] Comparative Example 4-1: 18% Flufenoxam Emulsifiable Concentrate Formula composition: 18% flufenoxuron, 14% lauryl alcohol polyoxyethylene ether (AEO-9, Nanjing Taihua), 3.5% calcium dodecylbenzenesulfonate (Nongru 500, Jiangsu Zhongshan Chemical), and 64.5% rosin-based vegetable oil (ND-60, Jinan Fuer Chemical).
[0033] Comparative Example 4-2: 18% Flufenoxam Emulsifiable Concentrate Formula composition: Fluorosulfuron 18%, Lauryl alcohol polyoxyethylene ether (AEO-9, Nanjing Taihua) 14%, Calcium dodecylbenzenesulfonate (Agricultural Emulsion No. 500, Jiangsu Zhongshan Chemical) 3.5%, Solvent oil No. 200 (Jinan Liyang Chemical) 64.5%.
[0034] Preparation Example 5: 20% Flufenoxam Emulsifiable Concentrate Formula composition: 20% flufenoxuron, 13% fatty alcohol polyoxyethylene ether (AEO-7, Jilin Petrochemical), 6.5% sodium alkyl aryl sulfonate, 45% rosin-based vegetable oil (ND-60, Jinan Fuer Chemical), and 15.5% propylene carbonate.
[0035] Control Example 5-1: 20% Flufenoxam Emulsifiable Concentrate Formula composition: 20% flufenoxuron, 13% fatty alcohol polyoxyethylene ether (AEO-7, Jilin Petrochemical), 6.5% sodium alkyl aryl sulfonate, and 60.5% rosin-based vegetable oil (ND-60, Jinan Fuer Chemical).
[0036] Control Example 5-2: 20% Flufenoxam Emulsifiable Concentrate Formula composition: 20% flufenoxuron, 13% fatty alcohol polyoxyethylene ether (AEO-7, Jilin Petrochemical), 6.5% sodium alkyl aryl sulfonate, and 60.5% propylene carbonate.
[0037] Preparation Example 6: 21% Flufenoxam Emulsifiable Concentrate Formula composition: Fluorosulfuron 21%, Triphenylethylphenol Polyoxyethylene Ether (Agricultural Emulsion 601, Nanjing Taihua) 17%, Calcium Dodecylbenzene Sulfonate (Agricultural Emulsion 500, Jiangsu Zhongshan Chemical) 5%, Rosin-based Vegetable Oil (ND-60, Jinan Fuer Chemical) 43%, No. 200 Solvent Oil (Jinan Liyang Chemical) 14%.
[0038] Control Example 6-1: 21% Flufenoxam Emulsifiable Concentrate Formula composition: Fluorosulfuron 21%, Triphenylethylphenol Polyoxyethylene Ether (Agricultural Emulsion 601, Nanjing Taihua) 17%, Calcium Dodecylbenzene Sulfonate (Agricultural Emulsion 500, Jiangsu Zhongshan Chemical) 5%, Rosin-based Vegetable Oil (ND-60, Jinan Fuer Chemical) 26%, No. 200 Solvent Oil (Jinan Liyang Chemical) 31%.
[0039] Comparative Example 6-2: 21% Flufenoxam Emulsifiable Concentrate Formula composition: Fluorosulfuron 21%, Triphenylethylphenol Polyoxyethylene Ether (Agricultural Emulsion 601, Nanjing Taihua) 17%, Calcium Dodecylbenzene Sulfonate (Agricultural Emulsion 500, Jiangsu Zhongshan Chemical) 5%, Rosin-based Vegetable Oil (ND-60, Jinan Fuer Chemical) 48%, No. 200 Solvent Oil (Jinan Liyang Chemical) 9%.
[0040] Preparation Example 7: 24% Flufenoxam Emulsifiable Concentrate Formula composition: Fluorosulfuron 24%, Lauryl alcohol polyoxyethylene ether (AEO-9, Nanjing Taihua) 15%, Calcium dodecylbenzenesulfonate (Agricultural Emulsion No. 500, Jiangsu Zhongshan Chemical) 7%, Rosin-based vegetable oil (ND-60, Jinan Fuer Chemical) 42%, Trimethylbenzene (Jiangsu Hualun) 12%.
[0041] Control Example 7-1: 24% Flufenoxam Emulsifiable Concentrate Formula composition: Fluorosulfuron 24%, Lauryl alcohol polyoxyethylene ether (AEO-9, Nanjing Taihua) 15%, calcium dodecylbenzenesulfonate (Nongru 500, Jiangsu Zhongshan Chemical) 7%, rosin-based vegetable oil (ND-60, Jinan Fuer Chemical) 54%.
[0042] Comparative Example 7-2: 24% Flufenoxam Emulsifiable Concentrate Formula composition: Fluorosulfuron 24%, Lauryl alcohol polyoxyethylene ether (AEO-9, Nanjing Taihua) 15%, calcium dodecylbenzenesulfonate (Nongru 500, Jiangsu Zhongshan Chemical) 7%, tricresylbenzene (Jiangsu Hualun) 54%.
[0043] Preparation Example 8: 30% Flufenoxam Emulsifiable Concentrate Formula composition: 30% flumethrin, 13% fatty alcohol polyoxyethylene ether (AEO-7, Jilin Petrochemical), 2% sodium naphthalene sulfonate formaldehyde condensate (dispersant NNO, Jinan Sante Chemical), 44% rosin-based vegetable oil (ND-60, Jinan Fuer Chemical), and 11% propylene carbonate.
[0044] Control Example 8-1: 30% Flufenoxam Emulsifiable Concentrate Formula composition: 30% flumethrin, 13% fatty alcohol polyoxyethylene ether (AEO-7, Jilin Petrochemical), 2% sodium naphthalene sulfonate formaldehyde condensate (dispersant NNO, Jinan Sante Chemical), 48% rosin-based vegetable oil (ND-60, Jinan Fuer Chemical), and 7% propylene carbonate.
[0045] Control Example 8-2: 30% Flufenoxam Emulsifiable Concentrate Formula composition: 30% flumethrin, 13% fatty alcohol polyoxyethylene ether (AEO-7, Jilin Petrochemical), 2% sodium naphthalene sulfonate formaldehyde condensate (dispersant NNO, Jinan Sante Chemical), 27% rosin-based vegetable oil (ND-60, Jinan Fuer Chemical), and 28% propylene carbonate.
[0046] Example 1: Determination of main performance indicators of each formulation preparation example and control example.
[0047] 1. Emulsion stability test: Refer to GB / T 1603-2001 "Determination of stability of pesticide emulsions".
[0048] 2. Determination of storage stability and thermal decomposition rate: Refer to GB / T 19136-2021 "Determination of thermal storage stability of pesticides" and GB / T 19137-2003 "Determination of low temperature stability of pesticides".
[0049] 3. Test method for emulsification and dispersibility: Use a syringe to slowly add 1 mL of emulsifiable oil into a beaker containing hard water from a height of 2 cm above the water surface, and observe the emulsification and dispersibility. Criteria for determining the emulsified dispersion state in water: Level 1: It can disperse quickly, automatically, and evenly, and with slight stirring, it becomes a blue or pale white transparent emulsion; Level 2: It can automatically disperse as a white cloud, and when stirred slightly, it becomes a blue, translucent emulsion; Grade III: Filamentous dispersion, turns into a blue, opaque emulsion after stirring; Grade IV: It sinks as white microspheres and becomes a white, opaque emulsion after stirring; Level 5: It sinks in the form of oil droplets, emulsifies when stirred, and separates into layers when stirring stops.
[0050] Table 1. Results of determination of main performance indicators of flufenoxuron emulsifiable concentrate deal with Emulsion stability Emulsification and dispersibility Low temperature stability Content % before thermal storage Content after heat storage % thermal storage degradation rate % Preparation Example 1 qualified Level 1 qualified 10.15 10.03 1.18 Compare with Example 1-1 qualified Level 4 Unqualified 10.23 9.36 8.50 Compare with Examples 1-2 Unqualified Level 4 Unqualified 10.11 9.15 9.50 Compare with Examples 1-3 qualified Level 3 qualified 10.23 9.57 6.45 Preparation Example 2 qualified Level 1 qualified 12.13 11.89 1.98 Compare with Example 2-1 Unqualified Level 3 Unqualified 12.35 11.51 6.80 Compare with Example 2-2 qualified Level 2 Unqualified 12.06 11.42 5.31 Preparation Example 3 qualified Level 1 qualified 15.19 14.88 2.04 Compare with Example 3-1 qualified Level 3 qualified 15.22 13.92 8.54 Compare with Example 3-2 Unqualified Level 4 Unqualified 15.06 13.53 10.16 Preparation Example 4 qualified Level 1 qualified 18.11 17.68 2.37 Compare with Example 4-1 Unqualified Level 4 Unqualified 18.23 16.63 8.78 Compare with Example 4-2 Unqualified Level 5 Unqualified 18.15 16.32 10.08 Preparation Example 5 qualified Level 1 qualified 20.13 19.85 1.39 Compare with Example 5-1 qualified Level 5 Unqualified 20.21 18.52 8.36 Compare with Example 5-2 Unqualified Level 5 Unqualified 20.18 18.24 9.61 Preparation Example 6 qualified Level 1 qualified 21.31 20.76 2.58 Compare with Example 6-1 Unqualified Level 3 Unqualified 21.26 19.38 8.84 Compare with Example 6-2 qualified Level 2 qualified 21.18 19.55 7.70 Preparation Example 7 qualified Level 1 qualified 24.23 23.41 3.38 Compare with Example 7-1 Unqualified Level 4 Unqualified 24.15 22.15 8.28 Compare with Example 7-2 Unqualified Level 5 Unqualified 24.03 21.37 11.07 Preparation Example 8 qualified Level 1 qualified 30.12 29.18 3.12 Compare with Example 8-1 Unqualified Level 4 Unqualified 30.15 28.12 6.73 Compare with Example 8-2 Unqualified Level 4 Unqualified 30.31 28.05 7.46 Table 1 shows the experimental data results. The emulsifiable concentrates of different contents of flufenoxuron in Preparation Examples 1-8 all contain specific emulsifiers and specific composite solvent formulations. After the heat storage test, the heat storage decomposition rate is less than 5%, which is significantly lower than that of the control example. Moreover, the emulsions of Preparation Examples 1-8 have good stability and the emulsification and dispersibility are all Grade 1, meeting the quality standards of composite emulsifiable concentrate products.
[0051] Example 2: Determination of wetting and spreading performance indicators.
[0052] Test instruments: Surface tension meter (Krusse GmbH, Germany), NDJ-1 viscometer (Shanghai Balance Instrument Factory), JC2000C series drop contact angle meter (Shanghai Zhongchen Digital Technology Equipment Co., Ltd.).
[0053] Test reagents: Preparation Examples 1, 2, 6, and 8, and Control Examples 1-3, 2-1, 2-2, 6-1, 6-2, 8-1, and 8-2 were diluted 1000 times with standard hard water to prepare corresponding solutions, with distilled water as a blank control.
[0054] 1. Measurement of surface tension and viscosity of the drug solution.
[0055] The surface tension of the treated solution was measured using a surface tension meter in accordance with the national standard GB / T 5549-2010, and the viscosity was measured using a viscometer. Each treatment was repeated 5 times, and the average value was taken.
[0056] 2. Contact angle measurement.
[0057] Use a 1-10 μL pipette to transfer 2 μL of the prepared solution onto the citrus leaves. After standing for about 30 seconds, use a contact angle meter to measure the contact angle formed between the solution and the leaf surface. Repeat each treatment 3 times and take the average value.
[0058] The experimental results are shown in the table below: Table 2 Results of Wetting and Spreadability Tests deal with Surface tension (mN / m) Viscosity (Pa / s) Contact angle / ° Preparation Example 1 37.15 0.9131 17 Preparation Example 2 36.90 0.9150 20 Preparation Example 6 36.50 0.9172 16 Preparation Example 8 35.14 0.9208 17 Compare with Examples 1-3 54.56 0.8854 64 Compare with Example 2-2 57.29 0.8862 57 Compare with Example 6-2 48.97 0.8951 46 Compare with Example 8-2 50.71 0.8876 69 distilled water 70.26 0.8844 74 The wetting and retention capacity of the pesticide solution is closely related to its surface tension and contact angle on the target leaf. As shown in the table above, the surface tension and contact angle of preparations 1, 2, 6, and 8 are significantly lower than those of the control example and distilled water. This indicates that the reasonable formulation of this invention can reduce the surface tension and contact angle of the pesticide solution on plant leaves or insect surfaces, thereby improving the wetting, spreading, and adhesion of the pesticide solution.
[0059] Example 3: Field efficacy test for controlling citrus paronychia.
[0060] The experiment was conducted in a citrus orchard in Mosha Town, Xinping County, Yuxi City, Yunnan Province. The soil type, fertilization and cultivation system of the experimental area were basically consistent with the local citrus cultivation practices. The planted variety was Mogu mandarin orange, and the citrus trees were growing well and were 7 years old.
[0061] Experimental target: Citrus paronychia.
[0062] Experimental design: All experimental plots were randomly arranged into blocks, with 2 trees per plot and 4 replicates. Guard rows were set between each plot.
[0063] Application time: The experiment was conducted during the peak occurrence of citrus paronychia. A backpack electric sprayer (SX-MD15DA 15L) was used to spray the leaves on both sides of the canopy once evenly.
[0064] Experimental Investigation: The initial insect population was assessed before treatment, and the insect population was surveyed at 3, 10, 14, and 21 days after application. Two trees were planted per plot. On each tree, 20 leaves were randomly selected from five directions (east, west, south, north, and center) to collect the total number of live mites on both the upper and lower surfaces. The average number of mites per leaf was calculated to determine the control efficacy. Following application, the safety of each pesticide treatment on new shoots, tender leaves, and young fruit was visually observed during efficacy surveys.
[0065] Methods for calculating drug efficacy:
[0066] Results and analysis of field efficacy trials: Table 3 Results of field efficacy trials for controlling *Pseudomonas citrus* deal with Dilution factor 3 days after medication 3 days after medication 10 days after medication 10 days after medication 14 days after medication 14 days after medication 21 days after medication 21 days after medication / / Reduction rate Prevention efficacy (%) Reduction rate Prevention efficacy (%) Reduction rate Prevention efficacy (%) Reduction rate Prevention efficacy (%) Preparation Example 1 1500 82.81 83.39 82.23 85.57 83.38 87.87 85.10 90.23 Preparation Example 2 2000 74.29 75.16 72.88 77.97 74.29 81.24 76.27 84.44 Preparation Example 3 2500 74.85 75.71 74.85 79.57 75.44 82.07 76.32 84.47 Preparation Example 4 3000 73.37 74.27 70.92 76.38 75.00 81.75 74.65 83.37 Preparation Example 5 3000 79.49 80.18 78.72 82.71 80.77 85.96 81.28 87.72 Preparation Example 6 3200 78.13 78.87 75.68 80.24 79.36 84.94 78.13 85.66 Preparation Example 7 3500 85.42 85.91 85.94 88.58 85.68 89.55 88.54 92.48 Preparation Example 8 4500 82.37 82.96 81.36 84.86 83.38 87.87 84.63 89.92 Compare with Examples 1-3 1500 63.35 64.59 62.78 69.77 61.65 72.01 52.27 68.70 Compare with Example 2-1 2000 63.02 64.28 60.70 68.07 61.16 71.65 55.58 70.87 Compare with Example 2-2 2000 66.08 67.23 64.34 71.03 67.08 75.97 58.35 72.68 Compare with Example 6-1 3200 61.61 62.91 59.35 66.98 57.74 69.15 46.77 65.09 Compare with Example 6-2 3200 67.90 68.99 63.93 70.70 66.05 75.22 55.70 70.94 Compare with Example 8-1 4500 65.66 66.82 61.54 68.76 64.01 73.73 56.59 71.53 Compare with Example 8-2 4500 64.55 65.75 61.67 68.87 61.10 71.60 52.45 68.81 Water comparison / -3.51 / -23.11 / -37.00 / -52.46 / Field efficacy trials showed that the compound emulsifiable concentrate formulation of this invention has a good control effect on citrus red spider mite. Among them, the emulsifiable concentrates of preparations 1-8 have a significantly better control effect on citrus red spider mite than the control example. The control efficacy is greater than 83% 21 days after application, and the effect lasts for a long time.
[0067] Example 4: Field efficacy test for controlling pepper spider mite.
[0068] Experimental site: Chili fields in Weijia Village, Liushan Town, Linqu County, Weifang City, Shandong Province. The experimental site is flat, with medium to high soil fertility and convenient irrigation and drainage.
[0069] Experimental crop: chili pepper.
[0070] Experimental target: a mixed population of two-spotted spider mites and truncated spider mites.
[0071] Experimental design: Treatments were carried out according to the experimental design concentration, with water treatment as the control. Each treatment was repeated 4 times and randomly arranged.
[0072] Experimental method: When the two mixed populations of pepper spider mites entered the initial peak stage, 20 mite-infested leaves were marked in each plot. The number of adult and nymphal mites was recorded as the base population. Then, conventional spraying was carried out using a 3WBD-20 electric sprayer. The number of live mites was collected on the 1st, 3rd and 7th day after the application, and the mite population reduction rate and control effect were calculated.
[0073] Methods for calculating drug efficacy:
[0074] Results and analysis of field efficacy trials: Table 4 Results of field efficacy trials for controlling pepper spider mites deal with Dosage of active ingredient (g / hectare) 1 day after medication 1 day after medication 3 days after medication 3 days after medication 7 days after medication 7 days after medication / / Reduction rate Prevention efficacy (%) Reduction rate Prevention efficacy (%) Reduction rate Prevention efficacy (%) Preparation Example 1 35 84.04 84.41 86.07 87.69 88.31 90.90 Preparation Example 2 35 83.41 83.79 84.60 86.40 83.89 87.46 Preparation Example 6 35 83.78 84.15 84.03 85.89 83.78 87.38 Preparation Example 8 35 85.19 85.52 85.88 87.53 85.88 89.01 Compare with Examples 1-3 35 67.15 67.89 69.30 72.89 67.87 74.99 Compare with Example 2-1 35 65.99 66.76 66.44 70.36 65.08 72.82 Compare with Example 6-2 35 69.70 70.39 70.44 73.90 70.94 77.38 Compare with Example 8-1 35 68.98 69.68 69.91 73.42 68.29 75.31 Water comparison / -2.31 / -13.22 / -28.47 / Field efficacy trials showed that the compound emulsifiable concentrate formulation of this invention has a good control effect on red spider mites in peppers. Among them, the emulsifiable concentrates of Preparation Example 1, Preparation Example 2, Preparation Example 6, and Preparation Example 8 have significantly better control effects on red spider mites in citrus peppers than Control Examples 1, 2, 6, and 8, with a control efficacy of more than 87% 7 days after application.
[0075] Experiments show that the flufenoxuron emulsifiable concentrate described in this invention exhibits good control efficacy against target mites. The emulsifiable concentrate formulation prepared in this invention demonstrates significant efficacy and a rational component system. Through the rational formulation using composite solvents and composite emulsifiers, it achieves good emulsification, low degradation rate of active ingredients, and good low-temperature and thermal stability. It can reduce the surface tension of the pesticide solution and the contact angle of the pesticide solution on plant leaves or insect surfaces, improving the wetting, spreading, and adhesion of the pesticide solution. Furthermore, no phytotoxicity was observed in the experiments with the compounded pesticide.
Claims
1. A pesticide emulsifiable concentrate containing flufenoxuron, characterized in that, The emulsifiable concentrate is composed of the following components by weight percentage: 1-50% flufenoxuron, 1-30% compound emulsifier, and the balance being a compound solvent.
2. The emulsifiable concentrate according to claim 1, characterized in that, The emulsifiable concentrate is composed of the following components by weight percentage: 5-40% flufenoxuron, 12-25% compound emulsifier, and the balance being a compound solvent; Preferably, the emulsifiable concentrate contains 8% to 30% by weight of flufenoxuron; More preferably, the emulsifiable concentrate contains 10% to 30% by weight of flufenoxuron.
3. The emulsifiable concentrate according to claim 1, characterized in that, The composite solvent comprises solvent A, rosin-based vegetable oil, and solvent B; solvent B is one or more of tricresylbenzene, propylene carbonate, or solvent oil.
4. The emulsifiable concentrate according to claim 3, characterized in that, The mass ratio of solvent A to solvent B in the composite solvent is 5:1 to 1:
2.
5. The emulsifiable concentrate according to claim 4, characterized in that, The mass ratio of solvent A to solvent B in the composite solvent is 4:1 to 1:
1.
6. The emulsifiable concentrate according to claim 1, characterized in that, The composite emulsifier includes polyoxyethylene ethers and sulfonates.
7. The emulsifiable concentrate according to claim 5, characterized in that, The polyoxyethylene ethers are one or more of lauryl alcohol polyoxyethylene ether, isotridecyl alcohol polyoxyethylene ether, fatty alcohol polyoxyethylene ether, and triphenylethylphenol polyoxyethylene ether, and the sulfonates are sodium alkyl aryl sulfonate, calcium dodecylbenzene sulfonate, and sodium naphthalene sulfonate formaldehyde condensate.
8. The application of the emulsifiable concentrate according to any one of claims 1-7 in the control of agricultural, forestry, and horticultural mites.
9. The application according to claim 8, characterized in that, The harmful mites mentioned are spider mites and malariae mites. The spider mite pests mentioned are *Tetranychus citrus*, *Tetranychus carmine*, *Tetranychus two-spotted*, *Tetranychus squarrosa*, *Tetranychus hawthorn*, *Tetranychus truncatus*, and *Tetranychus maculata*; the gall mite pests mentioned are *Tetranychus citrus*, *Tetranychus lycopersicum*, and *Tetranychus gracilis*.
10. The emulsifiable concentrate according to claim 1, characterized in that, The preparation method is as follows: add the metered flufenoxuron and composite solvent into the mixing tank to dissolve them, then add the composite emulsifier, make up the amount with solvent, stir evenly, and filter to obtain the final product.