Nano soluble concentrate containing s-metolachlor as well as preparation method and application of nano soluble concentrate

Abstract

The invention discloses a nano soluble concentrate containing s-metolachlor, metribuzin and pendimethalin, and the nano soluble concentrate is specifically prepared from the following raw materials in percentage by weight: 25% of s-metolachlor, 25% of metolachlor, 25% of metolachlor, 5% of metolachlor, 5% of metolachlor and the balance of water. 10% of metribuzin / pendimethalin; 38% of a solvent; 5-20% of a dispersant; 13% of an emulsifier; a proper amount of a pH regulator; and the balance of solvent. The nano soluble concentrate provided by the invention is small in particle size, good in particle dispersity, simple in preparation process, easy to operate and good in repeatability.

Description

Technical Field

[0001] This invention relates to two herbicidal compound nano-soluble agents, their preparation methods, and applications. One agent consists of a herbicidal active ingredient composed of metolachlor and cypermethrin, and the other consists of a herbicidal active ingredient composed of metolachlor and pendimethalin. Background Technology

[0002] In current agricultural production, weeds are increasingly damaging crops, especially cash crops such as corn. They not only lead to a significant decrease in crop yield but also develop resistance due to the overuse of herbicides, gradually reducing the effectiveness of traditional herbicides. S-metolachlor, a commonly used herbicide, has good control effects on monocotyledonous and some dicotyledonous weeds, especially annual broadleaf weeds and grasses. However, its effectiveness against some perennial weeds and emerging weeds is not ideal. Metfluthrin, as a novel herbicide, has a good weed-killing spectrum, but precise dosage control is required in practical applications, and it needs to be used in combination with other ingredients to improve its integrated control effect. Pendimethalin, a selective pre-emergence soil-applied herbicide, is widely used on various crops such as vegetables, fruit trees, and grapes, and has a good control effect on dicotyledonous weeds, but its control effect on monocotyledonous weeds is unsatisfactory.

[0003] Therefore, to address the aforementioned problems, it is necessary to develop a new herbicide composition that combines the advantages of different herbicides, broadens the weed control spectrum, and improves the efficacy against weeds. This composition should be able to target both monocot and dicot weeds simultaneously, reducing the amount of herbicide used, delaying the development of herbicide resistance in weeds, and ensuring crop safety and yield. Through scientific formulation and innovative formulation technology, a novel herbicide that integrates the advantages of multiple herbicides can be developed to meet the needs of modern agricultural production. Summary of the Invention

[0004] The purpose of this invention is to provide a nano-soluble herbicidal compound containing metolachlor and pendimethalin / ammonium methyl ether as active ingredients, its preparation method, and its application. Obtained through a specific preparation process, this composition can effectively control both monocot and dicot weeds, broaden the weed control spectrum, and improve the weed control effect.

[0005] Specifically, the two compositions contain metolachlor and cypermethrin, or metolachlor and pendimethalin as active ingredients, respectively, with the weight ratio of the active ingredients being metolachlor:cypermethrin / pendimethalin = 1-8:1-8, and preferably the weight ratio being metolachlor:cypermethrin / pendimethalin = 5:2.

[0006] The active ingredient has a weight percentage of 20-60% in the herbicidal composition, preferably 35%. It also includes DMAC, 602#, EC 500#, and EC R12 as auxiliary ingredients.

[0007] The specific operating method is as follows:

[0008] a. Heat and stir the chlorpyrifos and metolachlor / dimethalin with a solvent at 60°C until clear.

[0009] b. Add dispersant and emulsifier, and heat and stir at 60°C until clear.

[0010] In some embodiments, the solvent includes DMF, DMAC, methanol, ethanol, etc. DMAC is preferred as it aids in the dissolution and dispersion of the active ingredient. The dispersant includes DISPER2215, DISPER2216, G-100A, D-60, DS-720, 602#, etc. 602# is preferred as it helps improve the dispersibility of the active ingredient in the composition. The emulsifier includes emulsifiable concentrate R351, emulsifiable concentrate 500#, and emulsifiable concentrate R12, etc. Emulsifiable concentrate 500# and emulsifiable concentrate R12 are preferred as they help form a stable soluble concentrate.

[0011] In some embodiments, the method for preparing the herbicidal composition includes the following steps:

[0012] Step 1: Mix metolachlor and cypermethrin or pendimethalin in a predetermined ratio, add DMAC, and then heat and stir at 60°C until clear to form a preliminary mixed solution.

[0013] Step 2: Mix 602#, EC 500# and EC R12 in a predetermined ratio, add them to the initial mixed solution obtained in step a, and continue heating and stirring at 60°C until clear to form the final herbicide composition.

[0014] In some embodiments, the heating and stirring in step 1 is performed using a mechanical stirrer, and the stirring speed can be controlled between 100-1000 rpm. Preferably, it is 500 rpm.

[0015] The heating and stirring in step 2 are also carried out using a mechanical stirrer, and the stirring speed can be controlled between 100-1000 rpm. Preferably, it is 500 rpm.

[0016] In some embodiments, the temperature is controlled at 50-70°C, preferably 60°C, during the preparation of the herbicidal composition to ensure the stability of the active ingredients and the uniformity of the composition.

[0017] The compositions of the present invention can be converted into conventional formulations such as emulsifiable concentrates, wettable powders, granules, soluble powders, water-dispersible granules, suspensions, emulsions, microemulsions, emulsions, powders, coarse powders, soluble concentrates, pastes, and water surface floaters.

[0018] The application method depends on the specific use, and in all cases, their dispersion must be as fine and uniform as possible.

[0019] These formulations can be prepared using known processes, including but not limited to mixing, emulsification, ball milling, and sand milling, to ensure the homogeneity and stability of the formulation. The final soluble concentrate should be a clear or slightly turbid liquid with good thermal storage stability, cold storage stability, formulation stability, dilution stability, and sustained foaming properties.

[0020] The herbicidal composition of the present invention can be widely used for pre- or post-emergence weed control in dryland areas, and is especially suitable for weed control in fields of various crops such as soybeans, corn, corn-soybean intercropping, cotton, and wheat.

[0021] Compared with existing technologies, the two nano-soluble liquid agents of the present invention have the following advantages:

[0022] (1) It has a broad spectrum of weed control and can effectively control both monocot and dicot weeds.

[0023] (2) The preparation process is simple and easy to scale up.

[0024] (3) It has excellent solubility and stability, making it easy to use in the field.

[0025] The following examples are used to illustrate the preparation method of the present invention, but do not limit the scope of the present invention.

[0026] Example 1: 35% S-metolachlor·methrin nano-soluble liquid

[0027]

[0028] Weigh out the active ingredient, dissolve it in the solvent, then add the emulsifier and dispersant, and stir until homogeneous to obtain 35% metolachlor·methrin nano-soluble liquid.

[0029] Figure 1 This is a particle size distribution diagram of the 35% metolachlor-methoxychloride·methoxychloride nano-soluble liquid prepared in Example 1 of this invention. Figure 1 The average particle size is 58.98 nm.

[0030] Example 2: 35% S-metolachlor·pentyl soluble liquid

[0031]

[0032] Weigh out the active ingredient, dissolve it in the solvent, then add the emulsifier and dispersant, and stir until homogeneous to obtain 35% metolachlor·pentylene nano-soluble liquid.

[0033] Figure 2 This is a particle size distribution diagram of the 35% metolachlor·pentazine nano-soluble liquid agent prepared in Example 2 of the present invention. Figure 2 The average particle size is 53.57 nm.

[0034] Example of herbicide bioactivity assay:

[0035] 1. Test reagents

[0036] (1) 35% metolachlor·methrin soluble liquid

[0037] (2) 35% S-metolachlor·pentyl soluble liquid

[0038] (3) 960 g / L metolachlor EC (control agent)

[0039] (4) 480 g / L metribuzin suspension (control formulation)

[0040] (5) 330 g / L pendimethalin emulsifiable concentrate (control reagent)

[0041] (6) 40% sulfonylpyrazole suspension (control agent)

[0042] (7) 20% pyrimethanil (control agent)

[0043] (8) 25% thifensulfuron wettable powder (control formulation)

[0044] 2. Experimental methods and results

[0045] A pot experiment was conducted using 180 mm × 140 mm plastic pots filled with a 1:1 volume ratio of vermiculite and potting soil. Soil moisture was appropriately regulated and maintained within the range of 30-45%. Selected weed seeds were evenly sown in each pot and then covered with a thin layer of soil. A measured amount of the test solution was applied to the soil surface using a sprayer, with a spray volume set at 529 liters / ha. The effects were evaluated at 10 and 20 days after the treatment, including photographic recording (10 days) and observation of weed growth (20 days).

[0046] To ensure data reliability, each treatment was repeated four times. The experiments were conducted in a controlled indoor environment to eliminate the influence of environmental variables. The experimental results are shown in Table 1, which details the control efficacy against various weeds.

[0047] Table 1. Results of herbicidal bioactivity determination of the nano-soluble liquid formulation of the herbicidal composition of the present invention.

[0048]

[0049]

[0050] The data in Table 1 show that different agents and dosages have varying effects on the control of barnyard grass, foxtail grass, amaranth, and purslane.

[0051] (1) The 35% S-metolachlor·methrin nano-soluble liquid and the 35% S-metolachlor·pentyl nano-soluble liquid showed 100% control efficacy against barnyardgrass, foxtail grass, amaranth and purslane at all tested dosages (100 times to 400 times).

[0052] (2) 960 g / L metolachlor EC at doses of 60 ml / mu and 80 ml / mu showed 100% control efficacy against all tested weeds.

[0053] (3) At a dosage of 55 ml / mu, the 480 g / L metribuzin suspension showed 100% control efficacy against barnyardgrass, foxtail, and purslane, but only 93.26% control efficacy against amaranth. At a dosage of 82.5 ml / mu, the control efficacy against all tested weeds was 100%.

[0054] (4) At a dosage of 150 ml / mu, 330 g / L pendimethalin EC showed a control efficacy of 97.79% against crabgrass, 97.58% against foxtail grass, 64.21% against amaranth, and 100% against purslane. At a dosage of 225 ml / mu, the control efficacy was 100% against crabgrass, 97.96% against foxtail grass, 13.16% against amaranth, and 100% against purslane.

[0055] (5) 40% sulfopyrazole suspension at dosages of 25 ml / mu and 30 ml / mu had 100% control efficacy against barnyardgrass, foxtail grass and amaranth, and 100% control efficacy against purslane at dosage of 25 ml / mu and 97.63% at dosage of 30 ml / mu.

[0056] (6) At a dosage of 10 ml / mu, 20% pyrimethanil showed a control efficacy of 53.46% against barnyardgrass, 88.39% against foxtail grass, 86.32% against amaranth, and 100% against purslane. At a dosage of 30 ml / mu, the control efficacy was 34.56% against barnyardgrass, 90.44% against foxtail grass, 21.58% against amaranth, and 100% against purslane.

[0057] (7) At a dosage of 6 g / mu, 25% thifensulfuron wettable powder showed a control efficacy of 31.48% against barnyardgrass, 88.29% against foxtail grass, 83.89% against amaranth, and 100% against purslane. At a dosage of 8 g / mu, the control efficacy was 100% against barnyardgrass, 28.48% against foxtail grass, 46.84% against amaranth, and 100% against purslane.

[0058] (8) Compound preparations:

[0059] ①The combination of 960 g / L metolachlor EC + 480 g / L metolachlor SC showed 100% control efficacy against barnyardgrass, foxtail, and purslane in all tested ratios. However, the control efficacy against amaranth was 95.26% in the ratio of 35 ml / mu metolachlor + 70 ml / mu metolachlor, and 87.37% in the ratio of 35 ml / mu metolachlor + 35 ml / mu metolachlor.

[0060] ②The combination of 960 g / L metolachlor EC + 330 g / L pendimethalin EC showed 100% control efficacy against barnyardgrass, foxtail, and purslane in all tested ratios, but the control efficacy against amaranth was only 32.89% when the ratio of metolachlor 70 ml / mu + pendimethalin 90 ml / mu was used.

[0061] In summary, both the 35% S-metolachlor·methrin nano-soluble liquid and the 35% S-metolachlor·pendimethalin nano-soluble liquid demonstrated excellent performance, achieving 100% control of all weeds at all tested dosages. Compound formulations also showed high efficacy in most cases, especially when S-metolachlor was mixed with methrin or pendimethalin. The efficacy of other agents varied depending on the weed species and dosage.

[0062] Based on the above herbicidal bioactivity determination, the present invention further subjected the two nano-soluble liquid agents to gradient dilution. The results showed that the 35% S-metolachlor·pendimethalin nano-soluble liquid agent and the 35% S-metolachlor·methrin nano-soluble liquid agent still exhibited good herbicidal activity under the condition of dilution of 1125 times, and the average fresh weight inhibition rate of weed control could reach more than 85%.

[0063] In summary, the nano-soluble liquid formulations containing 35% S-metolachlor and metolachlor, and 35% S-metolachlor and pendimethalin provided by this invention, have demonstrated excellent weed-control effects through carefully designed experimental verification. These nano-soluble formulations not only have significant advantages in particle size control, dispersibility, and slow-release performance, but also possess simple and easy-to-implement preparation processes with good operability and repeatability, making them suitable for large-scale production.

[0064] In the herbicidal bioactivity test, both single-agent and compound formulations showed high control efficacy against weeds such as crabgrass, foxtail, amaranth, and purslane. In particular, the 35% S-metolachlor·methrin and 35% S-metolachlor·pendimethalin nano-soluble liquid formulations achieved or nearly achieved 100% control efficacy at different concentrations, demonstrating their potential for field weed control.

[0065] Furthermore, the nano-soluble liquid formulation of this invention exhibits excellent solubility and stability, which not only improves the efficiency of herbicide use but also helps reduce the amount of pesticides used, thereby reducing environmental impact. Through scientific formulation and innovative formulation technology, this invention has successfully developed a novel herbicide that integrates the advantages of multiple herbicides, meeting the needs of sustainable development in modern agriculture.

[0066] Although the present invention has been described through specific embodiments, those skilled in the art can make appropriate modifications or improvements based on the spirit of the invention to adapt to different application needs and conditions. These modifications or improvements all fall within the scope of protection of the present invention. Therefore, the present invention is not only theoretically innovative, but also has broad applicability and commercial prospects in practical applications. Attached Figure Description

[0067] Figure 1 Particle size distribution of 35% metolachlor·methrin nano-soluble liquid.

[0068] Figure 2 Particle size distribution of 35% metolachlor·pentylene nano-soluble liquid.

[0069] Figures 3-1 to 3-6 Results of bioactivity assay of 35% metolachlor·pendimethalin nano-soluble liquid at different dilution ratios (500x, 750x, 1125x, 1688x, 2531x, 3797x).

[0070] Figures 3-7 to 3-12 Results of bioactivity assay of 35% metolachlor·methrin nano-soluble liquid at different dilution ratios (500x, 750x, 1125x, 1688x, 2531x, 3797x).

Claims

1. Two herbicidal compositions, characterized in that... The active ingredients are metolachlor and cypermethrin, and metolachlor and pendimethalin, respectively, with a weight ratio of metolachlor:cypermethrin / pendimethalin = 1-8:1-8.

2. The herbicidal composition according to claim 1, characterized in that... The preferred weight ratio of the active ingredients is metolachlor: methamidophos / pentazocine = 5:

2.

3. The herbicidal composition according to claim 1 or 2, characterized in that... The active ingredient accounts for 20-60% by weight in the herbicidal composition.

4. The herbicidal composition according to claim 3, characterized in that the active ingredient has a preferred weight percentage content of 35% in the herbicidal composition.

5. The herbicidal composition according to claim 4, wherein, The herbicidal composition formulations are emulsifiable concentrates, wettable powders, granules, soluble powders, water-dispersible granules, suspension emulsions, and soluble solutions.

6. The herbicidal composition according to claim 5, wherein, The herbicidal composition is preferably a soluble formulation.

7. The two pesticide nano-soluble agents according to claims 1-6, characterized in that, The particle size is 0-300nm, preferably less than or equal to 100nm.

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