A herbicidal composition, its preparation method and use

Abstract

The present application relates to a kind of herbicide composition and its preparation method and application.The active ingredient of the herbicide composition includes acetochlor, oxaziclomefone, 2,4-D isooctyl ester;Wherein, the mass ratio of acetochlor, oxaziclomefone, 2,4-D isooctyl ester is (1-60) :(1-25) :(1-35).The herbicide composition has good control effect on annual weeds in spring soybean field and spring corn field, and each active ingredient synergistic effect can significantly reduce the use dosage, and the dispersion effect is good, the weeding effect is excellent, has no influence on the following crops, is environment-friendly, high safety and stable system.

Description

A herbicidal composition, its preparation method and application Technical Field

[0001] This invention relates to the field of pesticide technology, and in particular to a herbicidal composition, its preparation method, and its application. Background Technology

[0002] Effective weed control methods for spring corn and soybean fields include spraying non-selective herbicides, pre-emergence herbicides, and post-emergence herbicides, which are applicable before sowing, before emergence, and after emergence, respectively, to achieve good weed control results. Pre-emergence herbicides applied after sowing and before emergence are effective against both emerging and non-emerging weeds, and the cost is acceptable. While non-selective herbicides like glyphosate require large dosages, post-emergence herbicides are mostly highly active, and both methods are more expensive than pre-emergence herbicides.

[0003] Acetochlor is a widely used herbicide, mainly used for field weed control. It can effectively control annual grass weeds and small-seeded broadleaf weeds, with a residual effect of up to 45 days. It can be decomposed by microorganisms in the soil and will not have a long-term cumulative impact on the soil. It is currently the herbicide product with the largest market share.

[0004] Mefenoxam exerts its herbicidal activity primarily by inhibiting the photosynthesis of sensitive plants. After application, the germination and seedling emergence of various sensitive weeds are unaffected, but after emergence, the leaves turn pale green, eventually leading to nutrient depletion and death. Symptoms include leaves turning from green to yellow or appearing scorched; the entire leaf may turn yellow, but pale green remnants often remain in the veins, indicating intermittent chlorosis.

[0005] 2,4-D isooctyl ester is a broad-spectrum herbicide commonly used in agricultural production and lawn maintenance. Its mechanism of action involves interfering with the acidic components within the plant, leading to cessation of plant growth and ultimately death. Currently, 2,4-D isooctyl ester is one of the most commonly used herbicides in the world, ranking among the top in usage in countries such as the United States, Canada, and Australia.

[0006] However, the control effect of using any one of the three herbicides alone or in simple mixtures of two of them is generally limited. Long-term use of a single herbicide can easily lead to increased herbicide resistance in weeds, making it difficult to guarantee efficacy. Increasing the dosage to ensure efficacy not only raises costs but also exacerbates environmental pollution, creating a vicious cycle.

[0007] In view of this, the present invention is proposed. Summary of the Invention

[0008] The problem the invention aims to solve

[0009] The technical problem to be solved by the present invention is to overcome the shortcomings of the prior art and provide a herbicidal composition, its preparation method and application. The herbicidal composition has a good control effect on annual weeds in spring soybean fields and spring corn fields. The synergistic effect of each active ingredient can significantly reduce the dosage. It has good dispersion effect, excellent weed control effect, no impact on subsequent crops, is environmentally friendly, has high safety and the system is stable.

[0010] Solution for solving the problem

[0011] To solve the above-mentioned technical problems, the present invention provides a herbicidal composition, characterized in that its active ingredients include acetochlor, metribuzin, and 2,4-D isooctyl ester; wherein the mass ratio of acetochlor, metribuzin, and 2,4-D isooctyl ester is (1-60):(1-25):(1-35).

[0012] Preferably, the mass ratio of acetochlor, metribuzin, and 2,4-D isooctyl ester is (20-50):(1-20):(10-30);

[0013] Preferably, the mass ratio of acetochlor, metribuzin, and 2,4-D isooctyl ester is (32-42):(1-10):(13-23);

[0014] Preferably, the mass ratio of acetochlor, metribuzin, and 2,4-D isooctyl ester is 37:5:18.

[0015] Preferably, the active ingredients of the herbicidal composition consist of acetochlor, metribuzin, and 2,4-D isooctyl ester.

[0016] Preferably, the formulation of the herbicidal composition is a dispersible oil suspension, emulsifiable concentrate, microemulsion, water emulsion, suspension emulsion, granules, wettable powder, water-dispersible granules, or microcapsule suspension.

[0017] Preferably, the herbicidal composition is in the form of an emulsifiable concentrate.

[0018] Preferably, the herbicidal composition further includes adjuvants.

[0019] Preferably, the additive is selected from one or more of the following: emulsifier, stabilizer, wetting and dispersing agent, solvent, water, cosolvent, antifreeze, preservative, penetrant, thickener, disintegrant, structure modifier, and carrier;

[0020] Preferably, the additive is selected from one or more of emulsifiers, cosolvents, stabilizers, and solvents.

[0021] Preferably, the herbicidal composition comprises, by weight percentage: 40-80% active ingredient, 1-10% cosolvent, 5-15% emulsifier, 1-10% stabilizer, and solvent replenishment to 100%;

[0022] Preferably, the herbicidal composition comprises, by weight percentage: 50-70% active ingredient, 3-8% cosolvent, 5-10% emulsifier, 1-5% stabilizer, and solvent replenishment to 100%;

[0023] Preferably, the herbicidal composition comprises, by weight percentage: 60% active ingredient, 5% cosolvent, 7% emulsifier, 3% stabilizer, and solvent replenishment to 100%;

[0024] Preferably, the herbicidal composition comprises, by weight percentage: 37% acetochlor, 5% metribuzin, 18% 2,4-D isooctyl ester, 5% solubilizer, 7% emulsifier, 3% stabilizer, and solvent to make up 100%.

[0025] Preferably, the co-solvent is selected from C 1-4 alcohol;

[0026] Preferably, the co-solvent is selected from one or more of methanol, ethanol, and isopropanol;

[0027] Preferably, the co-solvent is methanol.

[0028] Preferably, the emulsifier is selected from one or more of castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, modified block polyoxyethylene ether, isomeric alcohol polyoxyethylene ether, and octylphenol polyoxyethylene ether.

[0029] Preferably, the emulsifier is a mixture of castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, and modified block polyoxyethylene ether.

[0030] Preferably, the mass ratio of castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, and modified block polyoxyethylene ether is (1-5):(1-5):(1-5);

[0031] Preferably, the mass ratio of castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, and modified block polyoxyethylene ether is 3.3:1.7:2.0.

[0032] Preferably, the stabilizer is selected from one or more of aminobenzoic acid, triphenyl phosphate, p-nitrobenzoic acid, 2,6-di-tert-butyl-p-cresol, oil-soluble vitamin E, gallic acid ester, and epichlorohydrin;

[0033] Preferably, the stabilizer is epichlorohydrin.

[0034] Preferably, the solvent is selected from one or more of xylene, 150# solvent oil, 200# solvent oil, sec-butyl acetate, trimethylbenzene, dichloromethane, and water;

[0035] Preferably, the solvent is xylene.

[0036] Preferably, the herbicidal composition comprises, by weight percentage: 37% acetochlor, 5% metribuzin, 18% 2,4-D isooctyl ester, 7% emulsifier, 5% solubilizer, 3% stabilizer, and solvent to make up to 100%.

[0037] The present invention also provides a method for preparing the herbicidal composition as described in any of the preceding claims, characterized by comprising the following steps: adding a solvent in a reaction vessel by weight, then adding acetochlor and a co-solvent by weight, heating, stirring and dissolving, then adding acetochlor, 2,4-D isooctyl ester and a stabilizer by weight, stirring, adding an emulsifier by weight, and stirring to obtain the herbicidal composition.

[0038] Preferably, the heating temperature is 30–50°C;

[0039] Preferably, the heating temperature is 40°C.

[0040] The present invention also provides the application of the herbicidal composition as described in any of the preceding claims or the herbicidal composition prepared according to the method described above in the control of weeds in farmland;

[0041] Preferably, the farmland is a spring soybean field or a spring corn field;

[0042] Preferably, the weeds are annual weeds;

[0043] Preferably, the annual weed is an annual grassy weed or a broadleaf weed;

[0044] Preferably, the annual weeds are barnyard grass, foxtail grass, black nightshade, wild millet, crabgrass, goosegrass, lambsquarters, amaranth, or iron amaranth;

[0045] Preferably, the annual weed is barnyard grass, foxtail grass, black nightshade, or lambsquarters.

[0046] The effects of the invention

[0047] The herbicidal composition of this invention exhibits a synergistic effect among the three active ingredients: acetochlor, metribuzin, and 2,4-D isooctyl ester. Compared to the three single agents, this herbicidal composition demonstrates stronger control of annual weeds in spring soybean and spring corn fields, significantly reducing the dosage of active ingredients, thereby lowering costs, reducing environmental pollution, and improving crop safety. Furthermore, it exhibits a more significant synergistic effect within a suitable ratio range. Acetochlor and metribuzin effectively seal off undisturbed grasses and broadleaf weeds, while 2,4-D isooctyl ester effectively kills early-emerging broadleaf weeds, achieving comprehensive and thorough weed control through a single seal and kill. The compound formulation of acetochlor, metribuzin, and 2,4-D isooctyl ester in this invention has a residual effect of up to 60 days, a moderate duration of action, and no impact on subsequent crops, allowing for crop rotation the following year. The herbicidal composition of this invention incorporates the stabilizer epichlorohydrin, effectively preventing discoloration of acetochlor and thus enhancing the stability of the formulation system. Furthermore, this herbicidal composition abandons the conventional combination of anionic and nonionic emulsifiers, employing ternary nonionic emulsifiers with different HLB values. The emulsifiers are modified and feature a significant EO design, resulting in a composition with remarkable emulsification and dispersion effects upon entering water. This further improves wetting, spreading, and adsorption in the waxy layer of weeds, significantly enhancing the herbicidal effect. Attached Figure Description

[0048] Figure 1 shows the effect of the formulation shown in Example 1-1 (sampling tube on the right in the figure) and the formulation shown in Example 3-1 (sampling tube on the left in the figure) after the light stability test.

[0049] Figure 2 shows the emergence and growth of soybeans and the weed situation in the spring soybean field of the blank control group 30 days after the field efficacy test.

[0050] Figure 3 shows the emergence, growth, and weed situation of soybeans in spring soybean fields after applying "Fengsha No. 1" at a rate of 2250 ml / mu for 30 days following the field efficacy test.

[0051] Figure 4 shows the emergence and growth of corn seedlings and the weed situation in the spring corn field of the blank control group 30 days after the field efficacy test.

[0052] Figure 5 shows the emergence and growth of corn seedlings and the weed situation in a spring cornfield after applying "Fengsha No. 1" at a rate of 2250 ml / mu for 30 days following a field efficacy trial. Detailed Implementation

[0053] To make the technical solution and beneficial effects of the present invention more apparent and understandable, a detailed description is provided below by listing specific embodiments. The accompanying drawings are not necessarily drawn to scale, and local features may be enlarged or reduced to more clearly show the details of the local features; unless otherwise defined, the technical and scientific terms used herein have the same meanings as those in the technical field to which this application pertains.

[0054] The present invention provides a herbicidal composition, characterized in that its active ingredients include acetochlor, metribuzin, and 2,4-D isooctyl ester; wherein the mass ratio of acetochlor, metribuzin, and 2,4-D isooctyl ester is (1-60):(1-25):(1-35).

[0055] In some embodiments, the mass ratio of acetochlor, metribuzin, and 2,4-D isooctyl ester is (20-50):(1-20):(10-30).

[0056] In some embodiments, the mass ratio of acetochlor, metribuzin, and 2,4-D isooctyl ester is (32-42):(1-10):(13-23).

[0057] In some embodiments, the mass ratio of acetochlor, metribuzin, and 2,4-D isooctyl ester is 37:5:18.

[0058] In some embodiments, the active ingredient of the herbicidal composition consists of acetochlor, metribuzin, and 2,4-D isooctyl ester.

[0059] In some embodiments, the herbicidal composition is formulated as a dispersible oil suspension, emulsifiable concentrate, microemulsion, water emulsion, suspension emulsion, granules, wettable powder, water-dispersible granules, or microcapsule suspension.

[0060] In some embodiments, the herbicidal composition is in the form of an emulsifiable concentrate.

[0061] In some embodiments, the herbicidal composition further includes adjuvants.

[0062] In some embodiments, the additive is selected from one or more of emulsifiers, stabilizers, wetting and dispersing agents, solvents, water, cosolvents, antifreeze agents, preservatives, penetrants, thickeners, disintegrants, structure modifiers, and carriers.

[0063] In some embodiments, the additive is selected from one or more of emulsifiers, cosolvents, stabilizers, and solvents.

[0064] In some embodiments, the herbicidal composition comprises, by weight percentage: 40-80% active ingredient, 1-10% cosolvent, 5-15% emulsifier, 1-10% stabilizer, and solvent replenishment to 100%.

[0065] In some embodiments, the herbicidal composition comprises, by weight percentage: 50-70% active ingredient, 3-8% cosolvent, 5-10% emulsifier, 1-5% stabilizer, and solvent to make up 100%.

[0066] In some embodiments, the herbicidal composition comprises, by weight percentage: 60% active ingredient, 5% cosolvent, 7% emulsifier, 3% stabilizer, and solvent replenishment to 100%.

[0067] In some embodiments, the herbicidal composition comprises, by weight percentage: 37% acetochlor, 5% metribuzin, 18% 2,4-D isooctyl ester, 5% solubilizer, 7% emulsifier, 3% stabilizer, and solvent to make up 100%.

[0068] In some embodiments, the co-solvent is selected from C 1-4 alcohol.

[0069] In some embodiments, the co-solvent is selected from one or more of methanol, ethanol, and isopropanol.

[0070] In some embodiments, the cosolvent is methanol.

[0071] In some embodiments, the emulsifier is selected from one or more of castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, modified block polyoxyethylene ether, isomeric alcohol polyoxyethylene ether, and octylphenol polyoxyethylene ether.

[0072] In some embodiments, the emulsifier is a mixture of castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, and modified block polyoxyethylene ether.

[0073] In some embodiments, the mass ratio of castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, and modified block polyoxyethylene ether is (1-5):(1-5):(1-5).

[0074] In some embodiments, the mass ratio of castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, and modified block polyoxyethylene ether is 3.3:1.7:2.0.

[0075] In some embodiments, the stabilizer is selected from one or more of aminobenzoic acid, triphenyl phosphate, p-nitrobenzoic acid, 2,6-di-tert-butyl-p-cresol, oil-soluble vitamin E, gallic acid ester, and epichlorohydrin.

[0076] In some embodiments, the stabilizer is epichlorohydrin.

[0077] In some embodiments, the solvent is selected from one or more of xylene, 150# solvent oil, 200# solvent oil, sec-butyl acetate, trimethylbenzene, dichloromethane, and water.

[0078] In some embodiments, the solvent is xylene.

[0079] In some embodiments, the herbicidal composition comprises, by weight percentage: 37% acetochlor, 5% metribuzin, 18% 2,4-D isooctyl ester, 7% emulsifier, 5% solubilizer, 3% stabilizer, and solvent to make up to 100%.

[0080] In some embodiments, the herbicidal composition comprises, by weight percentage: 37% acetochlor, 5% metribuzin, 18% 2,4-D isooctyl ester, 3.3% castor oil polyoxyethylene ether, 1.7% fatty alcohol polyoxyethylene ether, 2% modified block polyoxyethylene ether, 5% methanol, 3% epichlorohydrin, and xylene to bring the total to 100%.

[0081] The present invention also provides a method for preparing the herbicidal composition as described in any of the preceding claims, characterized by comprising the following steps: adding a solvent in a reaction vessel by weight, then adding acetochlor and a co-solvent by weight, heating, stirring and dissolving, then adding acetochlor, 2,4-D isooctyl ester and a stabilizer by weight, stirring, adding an emulsifier by weight, and stirring to obtain the herbicidal composition.

[0082] In some embodiments, the heating temperature is 30–50°C.

[0083] In some embodiments, the heating temperature is 40°C.

[0084] In some embodiments, each stirring is performed until homogeneous.

[0085] The present invention also provides the application of the herbicidal composition as described in any of the preceding claims or the herbicidal composition prepared according to the method described above in the control of weeds in farmland;

[0086] In some embodiments, the farmland is a spring soybean field or a spring corn field.

[0087] In some embodiments, the weeds are annual weeds.

[0088] In some embodiments, the annual weed is an annual grass or broadleaf weed.

[0089] In some embodiments, the annual weeds are barnyard grass, foxtail grass, black nightshade, wild millet, crabgrass, goosegrass, lambsquarters, amaranth, or iron amaranth.

[0090] In some embodiments, the annual weed is barnyard grass, foxtail grass, black nightshade, or lambsquarters.

[0091] The acetochlor used in this application embodiment was purchased from Zhanhua Guochang Fine Chemical Co., Ltd. as 81.5% acetochlor emulsifiable concentrate.

[0092] The metribuzin used in the embodiments of this application was purchased from Harbin Huifeng Bio-Agrochemical Co., Ltd. as 70% metribuzin wettable powder.

[0093] The 2,4-D isooctyl ester used in the embodiments of this application was purchased from 87.5% 2,4-D isooctyl ester emulsifiable concentrate from Dalian Songliao Chemical Co., Ltd. in Liaoning Province.

[0094] The amounts of acetochlor, metribuzin, and 2,4-D isooctyl ester mentioned in the embodiments of this application are calculated based on the actual amount of active pharmaceutical ingredients added, converted to a percentage.

[0095] Unless otherwise stated, all materials used in the embodiments of this application can be purchased directly from the market.

[0096] As shown in this application, either the "Fengsha No. 1" or the "60% acetochlor-dip octyl ester emulsifiable concentrate" is the same as the "(37% acetochlor + 5% metribuzin + 18% 2,4-dip isooctyl ester) emulsifiable concentrate" described in this application.

[0097] The method of the present invention will be described below through specific embodiments. It should be understood that these embodiments are used to illustrate the basic principles, main features and advantages of the present invention, and the present invention is not limited to the scope of the following embodiments. The implementation conditions used in the embodiments can be further adjusted according to specific requirements, and the implementation conditions not specified are usually the conditions in conventional experiments.

[0098] Example 1-1

[0099] First, add 212.2 kg of xylene to the reaction vessel, followed by 50.0 kg of (100% acetochlor) and 50.0 kg of methanol. Heat to 40±5℃ and stir until completely dissolved and homogeneous. Then add 370.0 kg of (100% acetochlor), 180.0 kg of (100% 2,4-D isooctyl ester, and 30.0 kg of epichlorohydrin. Stir thoroughly until homogeneous. Finally, add 33.0 kg of castor oil polyoxyethylene ether, 17.0 kg of fatty alcohol polyoxyethylene ether, and 20.0 kg of modified block polyoxyethylene ether. Stir until homogeneous to obtain (37% acetochlor + 5% acetochlor + 18% 2,4-D isooctyl ester) emulsifiable concentrate, namely "Fengsha No. 1".

[0100] The formulation of the emulsifiable concentrate (37% acetochlor + 5% metribuzin + 18% 2,4-D isooctyl ester) is shown in Table 1.

[0101] Table 1

[0102] Acetochlor 37%, metribuzin 5%, 2,4-D isooctyl ester 18%, castor oil polyoxyethylene ether 3.3%, fatty alcohol polyoxyethylene ether 1.7%, modified block polyoxyethylene ether 2.0%, methanol 5.0%, epichlorohydrin 3.0%, xylene to 100%. surface

[0103] Examples 1-2

[0104] First, add 342.0 kg of xylene to the reaction vessel, followed by 40.0 kg of 100% acetochlor and 50.0 kg of methanol. Heat to 40±5℃ and stir until completely dissolved and homogeneous. Then add 296.0 kg of 100% acetochlor, 144.0 kg of 100% 2,4-D isooctyl ester and 30.0 kg of epichlorohydrin. Stir thoroughly until homogeneous. Finally, add 33.0 kg of castor oil polyoxyethylene ether, 17.0 kg of fatty alcohol polyoxyethylene ether and 20.0 kg of modified block polyoxyethylene ether, and stir until homogeneous to obtain the final product.

[0105] Examples 1-3

[0106] First, add 278.4 kg of xylene to the reaction vessel, followed by 45.0 kg of 100% acetochlor and 50.0 kg of methanol. Heat to 40±5℃ and stir until completely dissolved and homogeneous. Then add 333.0 kg of 100% acetochlor, 162.0 kg of 100% 2,4-D isooctyl ester and 30.0 kg of epichlorohydrin. Stir thoroughly until homogeneous. Finally, add 33.0 kg of castor oil polyoxyethylene ether, 17.0 kg of fatty alcohol polyoxyethylene ether and 20.0 kg of modified block polyoxyethylene ether, and stir until homogeneous to obtain the final product.

[0107] Examples 1-4

[0108] First, add 238.4 kg of xylene to the reaction vessel, followed by 45.0 kg of 100% acetochlor and 50.0 kg of methanol. Heat to 40±5℃ and stir until completely dissolved and homogeneous. Then add 370.0 kg of 100% acetochlor, 162.0 kg of 100% 2,4-D isooctyl ester and 30.0 kg of epichlorohydrin. Stir thoroughly until homogeneous. Finally, add 33.0 kg of castor oil polyoxyethylene ether, 17.0 kg of fatty alcohol polyoxyethylene ether and 20.0 kg of modified block polyoxyethylene ether, and stir until homogeneous to obtain the final product.

[0109] Examples 1-5

[0110] First, add 234.8 kg of xylene to the reaction vessel, followed by 50.0 kg of 100% acetochlor and 50.0 kg of methanol. Heat to 40±5℃ and stir until completely dissolved and homogeneous. Then add 370.0 kg of 100% acetochlor, 162.0 kg of 100% 2,4-D isooctyl ester and 30.0 kg of epichlorohydrin. Stir thoroughly until homogeneous. Finally, add 33.0 kg of castor oil polyoxyethylene ether, 17.0 kg of fatty alcohol polyoxyethylene ether and 20.0 kg of modified block polyoxyethylene ether, and stir until homogeneous to obtain the final product.

[0111] Example 2-1

[0112] First, add 212.2 kg of xylene to the reaction vessel, followed by 50.0 kg of 100% acetochlor and 50.0 kg of methanol. Heat to 40±5℃ and stir until completely dissolved and homogeneous. Then add 370.0 kg of 100% acetochlor, 180.0 kg of 100% 2,4-D isooctyl ester and 30.0 kg of epichlorohydrin. Stir thoroughly until homogeneous. Finally, add 43.0 kg of castor oil polyoxyethylene ether, 22.0 kg of fatty alcohol polyoxyethylene ether and 5.0 kg of modified block polyoxyethylene ether, and stir until homogeneous to obtain the final product.

[0113] Example 2-2

[0114] First, add 212.2 kg of xylene to the reaction vessel, followed by 50.0 kg of 100% acetochlor and 50.0 kg of methanol. Heat to 40±5℃ and stir until completely dissolved and homogeneous. Then add 370.0 kg of 100% acetochlor, 180.0 kg of 100% 2,4-D isooctyl ester and 30.0 kg of epichlorohydrin. Stir thoroughly until homogeneous. Finally, add 13.0 kg of castor oil polyoxyethylene ether, 17.0 kg of fatty alcohol polyoxyethylene ether and 40.0 kg of modified block polyoxyethylene ether, and stir until homogeneous to obtain the final product.

[0115] Example 2-3

[0116] First, add 212.2 kg of xylene to the reaction vessel, followed by 50.0 kg of 100% acetochlor and 50.0 kg of methanol. Heat to 40±5℃ and stir until completely dissolved and homogeneous. Then add 370.0 kg of 100% acetochlor, 180.0 kg of 100% 2,4-D isooctyl ester and 30.0 kg of epichlorohydrin. Stir thoroughly until homogeneous. Finally, add 23.0 kg of castor oil polyoxyethylene ether, 12.0 kg of fatty alcohol polyoxyethylene ether and 35.0 kg of modified block polyoxyethylene ether, and stir until homogeneous to obtain the final product.

[0117] Examples 2-4

[0118] First, add 262.2 kg of xylene to the reaction vessel, then add 50.0 kg of (100% concentration) acetochlor, heat to 40±5℃, and stir until completely dissolved and homogeneous. Add 370.0 kg of (100% concentration) acetochlor, 180.0 kg of (100% concentration) 2,4-D isooctyl ester and 30.0 kg of epichlorohydrin, and stir thoroughly until homogeneous. Add 23.0 kg of castor oil polyoxyethylene ether, 12.0 kg of fatty alcohol polyoxyethylene ether and 35.0 kg of modified block polyoxyethylene ether, and stir until uniform.

[0119] Example 3-1

[0120] First, add 212.2 kg of xylene to the reaction vessel, followed by 50.0 kg of 100% acetochlor and 50.0 kg of methanol. Heat to 40±5℃ and stir until completely dissolved and homogeneous. Then add 370.0 kg of 100% acetochlor and 180.0 kg of 100% 2,4-D isooctyl ester and stir thoroughly until homogeneous. Finally, add 33.0 kg of castor oil polyoxyethylene ether, 17.0 kg of fatty alcohol polyoxyethylene ether, and 20.0 kg of modified block polyoxyethylene ether and stir until homogeneous to obtain the final product.

[0121] Example 3-2

[0122] First, add 212.2 kg of xylene to the reaction vessel, followed by 50.0 kg of 100% acetochlor and 50.0 kg of methanol. Heat to 40±5℃ and stir until completely dissolved and homogeneous. Then add 370.0 kg of 100% acetochlor, 180.0 kg of 100% 2,4-D isooctyl ester and 30.0 kg of BHT (2,6-di-tert-butyl-p-cresol). Stir thoroughly until homogeneous. Finally, add 33.0 kg of castor oil polyoxyethylene ether, 17.0 kg of fatty alcohol polyoxyethylene ether and 20.0 kg of modified block polyoxyethylene ether, and stir until homogeneous to obtain the final product.

[0123] Example 3-3

[0124] First, add 212.2 kg of xylene to the reaction vessel, followed by 50.0 kg of 100% acetochlor and 50.0 kg of methanol. Heat to 40±5℃ and stir until completely dissolved and homogeneous. Then add 370.0 kg of 100% acetochlor, 180.0 kg of 100% 2,4-D isooctyl ester and 30.0 kg of oil-soluble vitamin E, and stir thoroughly until homogeneous. Finally, add 33.0 kg of castor oil polyoxyethylene ether, 17.0 kg of fatty alcohol polyoxyethylene ether and 20.0 kg of modified block polyoxyethylene ether, and stir until homogeneous to obtain the final product.

[0125] Examples 3-4

[0126] First, add 212.2 kg of xylene to the reaction vessel, followed by 50.0 kg of 100% acetochlor and 50.0 kg of methanol. Heat to 40±5℃ and stir until completely dissolved and homogeneous. Then add 370.0 kg of 100% acetochlor, 180.0 kg of 100% 2,4-D isooctyl ester and 30.0 kg of gallic acid. Stir thoroughly until homogeneous. Finally, add 33.0 kg of castor oil polyoxyethylene ether, 17.0 kg of fatty alcohol polyoxyethylene ether and 20.0 kg of modified block polyoxyethylene ether, and stir until homogeneous to obtain the final product.

[0127] Example 1: Indoor Combined Toxicity Test

[0128] Indoor formulation screening (combined toxicity) tests were conducted on Examples 1-1 to 1-5, and the results are shown in Table 2.

[0129] Table 2

[0130]

[0131] Example 2: Stability Performance Test

[0132] Storage tests were conducted on Examples 1-1, 2-1, 2-2, 2-3, and 2-4, including cold storage at 0±2℃, heat storage at 54±2℃, and emulsion stability tests, to observe the stability of the formulations. The results are shown in Table 3.

[0133] Table 3

[0134] Example Cold Storage Hot Storage Emulsion Stability Surface Tension (mN / m) 1-1 No crystallization Pass Emulsion Stability Pass 29.38 2-1 No crystallization Pass Primary Emulsion Pass, Emulsion Stability Fail 33.65 2-2 No crystallization Pass Both Primary Emulsion and Emulsion Stability Fail 40.23 2-3 No crystallization Pass Both Primary Emulsion and Emulsion Stability Fail 38.76 2-4 Bottom crystallization Pass Emulsion Stability Pass surface

[0135] Example 3: Stability Performance Test

[0136] Storage tests were conducted on Examples 1-1, 3-1, 3-2, 3-3, and 3-4, including cold storage at 0±2℃, heat storage at 54±2℃, and emulsion stability tests, to observe the stability of the formulations. The results are shown in Table 4.

[0137] Table 4

[0138]

[0139]

[0140] Example 4: Field Efficacy Test

[0141] 1. Location: Xiangyang Farm, Northeast Agricultural University, Harbin, Heilongjiang Province; the plots are arranged as shown in Table 5.

[0142] Table 5. Layout of the residential area

[0143]

[0144] 2. Drugs and dosages: as shown in Table 6.

[0145] Table 6 Experimental Design of Test Reagents

[0146]

[0147] 3. Application date: May 13, 2016

[0148] 4. Number of applications: 1 time

[0149] 5. Field Management: Sowing was carried out on May 12, 2016; only normal field management was required during the trial period; no irrigation or other pest control was carried out; manual weeding was carried out twice in the manually weeded areas on May 28 and June 13. After the trial, all weeds in the field were removed manually.

[0150] 6. Weed survey:

[0151] First survey: 15 days after application (May 28, 2016), weed control efficacy was visually assessed;

[0152] Second survey: 30 days after application (June 13, 2016), the number of surviving weeds and their fresh weight were investigated.

[0153] Two surveys were conducted.

[0154] 7. Weed survey

[0155] Survey methods: The weed survey adopted the estimated value survey method and the absolute value survey method.

[0156] Absolute value survey method: The number of weeds was investigated, and three points were sampled along the diagonal of each plot, with each point measuring 0.25m. The fresh weight of weeds in the survey area was also measured 30 days after the application of the pesticide.

[0157] Estimated value survey method: The following grading criteria are used for the survey:

[0158] Level 1: No grass

[0159] Level 2: Equivalent to 0-2.5% of the blank control area.

[0160] Level 3: Equivalent to 2.6%-5% of the blank control.

[0161] Level 4: Equivalent to 5.1%-10% of the blank control.

[0162] Level 5: Equivalent to 10.1%-15% of the blank control.

[0163] Level 6: Equivalent to 15.1%-25% of the blank control.

[0164] Level 7: Equivalent to 25.1%-35% of the blank control.

[0165] Level 8: Equivalent to 35.1%-67.5% of the blank control.

[0166] Level 9: Equivalent to 67.6%-100% of the blank control.

[0167] Weed symptoms: After application, the number of weeds in the treated area was significantly less than that in the control area, and the amount of pesticide applied was positively correlated with the weed control effect. The weeds in the control area grew vigorously.

[0168] Herbicide efficacy calculation method: Follows the guidelines for field efficacy trials of pesticides (I). The formula for calculating herbicide efficacy is as follows:

[0169]

[0170] Note: PT - Number of remaining weeds (or fresh weight) in the treatment area.

[0171] The number (or fresh weight) of surviving weeds in the CK-blank control area.

[0172] 8. Crop Survey

[0173] Number of surveys: Three surveys in total.

[0174] First survey: 15 days after application (May 28, 2016);

[0175] Second survey: 30 days after application (June 13, 2016);

[0176] Third survey: Soybean harvest time (September 30, 2016).

[0177] Survey Methodology: The pesticide damage was classified and graded for each plot according to the pesticide damage grading method.

[0178] Grade 1: Soybeans are growing normally, with no signs of pesticide damage.

[0179] Level 2: Slight pesticide damage to soybeans, less than 10%

[0180] Level 3: Moderate pesticide damage to soybeans; recovery is possible and yield will not be affected.

[0181] Level 4: Severe pesticide damage to soybeans, difficult to recover from, resulting in reduced yield.

[0182] Level 5: Severe pesticide damage to soybeans, irreversible, resulting in significant yield reduction or complete crop failure.

[0183] Side effects observation: No effect on non-target organisms.

[0184] Crop yield and quality: Yield measurement results showed that 60% acetazine-dextrose emulsifiable concentrate (i.e., "Fengsha No. 1") had no effect on soybean yield. The results are shown in Table 7.

[0185] Table 7. Effects of 60% Ethyl Acetate·Zyrazine·October Emulsifiable Oil on Soybean Yield

[0186]

[0187] Table 8 shows the visual control efficacy of 60% ethyl acetate-azine-dextrose emulsifiable concentrate against annual weeds in soybean fields 15 days after application. As can be seen from Table 8, 15 days after application, the visual control efficacy of 60% ethyl acetate-azine-dextrose emulsifiable concentrate against weeds reached over 85%, with good efficacy against annual weeds such as barnyard grass, foxtail, lambsquarters, and black nightshade.

[0188] Table 8

[0189]

[0190] Tables 9 and 10 show the plant control efficacy (%) and fresh weight control efficacy (%) of 60% ethyl acetate-dextrose emulsifiable concentrate against annual weeds in soybean fields 30 days after application. Tables 9 and 10 indicate that 60% ethyl acetate-dextrose emulsifiable concentrate showed good plant control efficacy against annual weeds 30 days after application, at a dosage of 1800-2250 g a.i. / hm². 2 The plant control efficacy against barnyard grass was 92.0%–93.5%, against foxtail grass 90.4%–91.8%, against lambsquarters 92.1%–94.6%, and against black nightshade 91.5%–95.8%; the fresh weight control efficacy against barnyard grass was 84.5%–88.5%, against foxtail grass 84.4%–90.9%, against lambsquarters 90.3%–94.6%, and against black nightshade 90.9%–96.1%.

[0191] Table 9

[0192]

[0193] Note: Duncan multiple comparisons, lowercase letters indicate the 0.05 level, and uppercase letters indicate the 0.01 level.

[0194] Table 10

[0195]

[0196] Note: Duncan multiple comparisons, lowercase letters indicate the 0.05 level, and uppercase letters indicate the 0.01 level.

[0197] It should be understood that the above embodiments are exemplary and are not intended to encompass all possible implementations included in the claims. Various modifications and changes can be made to the above embodiments without departing from the scope of this disclosure. Similarly, the various technical features of the above embodiments can be arbitrarily combined to form other embodiments of the present invention that may not be explicitly described. Therefore, the above embodiments only illustrate several implementations of the present invention and do not limit the scope of protection of this patent.

Claims

1. A herbicidal composition, characterized in that, The herbicidal composition comprises, by weight percentage: 37% acetochlor, 5% metribuzin, 18% 2,4-D isooctyl ester, 7% emulsifier, 5% co-solvent, 3% stabilizer, and solvent to 100%; the co-solvent is selected from methanol; the emulsifier is selected from a mixture of castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, and modified block polyoxyethylene ether, wherein the mass ratio of castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, and modified block polyoxyethylene ether is 3.3:1.7:2.0; the stabilizer is selected from epichlorohydrin; and the solvent is selected from xylene.

2. A method for preparing the herbicidal composition as described in claim 1, characterized in that, The process includes the following steps: adding solvent to a reaction vessel according to weight, then adding acetochlor and co-solvent according to weight, heating, stirring to dissolve, then adding acetochlor, 2,4-D isooctyl ester and stabilizer according to weight, stirring, adding emulsifier according to weight, and stirring to obtain the final product.

3. The method as described in claim 2, characterized in that, The heating temperature is 30~50℃.

4. The method as described in claim 3, characterized in that, The heating temperature is 40°C.

5. The application of the herbicidal composition according to claim 1 or the herbicidal composition prepared by any one of claims 2-4 in the control of weeds in farmland.

6. The application as described in claim 5, characterized in that, The farmland in question is either a spring soybean field or a spring corn field.

7. The application as described in claim 5, characterized in that, The weeds mentioned are annual weeds.

8. The application as described in claim 7, characterized in that, The annual weeds are annual grasses or broadleaf weeds.

9. The application as described in claim 8, characterized in that, The annual weeds mentioned are barnyard grass, foxtail grass, black nightshade, wild millet, crabgrass, goosegrass, lambsquarters, amaranth, or iron amaranth.

10. The application as described in claim 9, characterized in that, The annual weeds mentioned are barnyard grass, foxtail grass, black nightshade, or lambsquarters.

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