Herbicidal compositions, formulations and their applications

Abstract

The present invention relates to the field of agrochemical technology, specifically to herbicidal compositions, pharmaceuticals and their applications. A herbicidal composition, comprising component A and component B, component A being pyriminobac (ethyl 3-(2-chloro-4-fluoro-5-(3-methyl-2,6-dioxy-4-trifluoromethyl-3,6-dihydropyrimidin-1(2H)-yl)phenyl)-5-methyl-4,5-dihydroisoxazole-5-carboxylate), component B being selected from at least one of acetochlor, butachlor, metolachlor, dimethachlor, mesotrione, nicosulfuron, atrazine, terbuthylazine, s-metolachlor, and dimethenamid-P, and the weight ratio of component A to component B is 1:(1-80). The present invention screens and optimizes the types and contents of emulsifiers, solvents, etc., so that the aqueous emulsion obtained has stable quality and excellent performance, which is more helpful in exerting the efficacy. The aqueous emulsion is free from stratification, aggregation, coalescence and demulsification when stored at different temperatures, thus greatly improving the storage stability of the aqueous emulsion.The herbicidal composition of the present application is suitable for pre-emergence soil treatment of field crops.

Description

[Technical field]

[0001] The present invention relates to the field of agrochemical technology, specifically to herbicidal compositions, formulations and their applications. [Background technology]

[0002] Herbicides are indispensable for crop management. CN105052931A is a kind of aqueous emulsion that enhances herbicidal efficacy, which is prepared by using herbicidal active ingredients, environmentally friendly solvents, surfactants, synergists, stabilizers, antifreeze agents and water, and has the characteristics of being environmentally friendly and easy to decompose. However, with a single herbicidal active ingredient, it is prone to resistance, has a narrow herbicidal spectrum, and the performance of the aqueous emulsion that enhances herbicidal efficacy is very unstable under high and low temperature conditions, which limits its application. Summary of the Invention [Problem to be solved by the invention]

[0003] In view of the above technical problems, the present invention provides a herbicidal composition containing Pyriminobac (ethyl 3-(2-chloro-4-fluoro-5-(3-methyl-2,6-dioxy-4-trifluoromethyl-3,6-dihydropyrimidin-1(2H)-yl)phenyl)-5-methyl-4,5-dihydroisoxazole-5-carboxylate) and an aqueous emulsion prepared therefrom, which solves the stability problems existing in the current aqueous emulsions by selecting auxiliaries, and broadens the application scope of the aqueous emulsions. [Means for solving the problem]

[0004] In order to solve the above technical problems, the first aspect of the present invention provides a herbicidal composition, the composition comprising component A and component B, the component A being pyriminobac (ethyl 3-(2-chloro-4-fluoro-5-(3-methyl-2,6-dioxy-4-trifluoromethyl-3,6-dihydropyrimidin-1(2H)-yl)phenyl)-5-methyl-4,5-dihydroisoxazole-5-carboxylate), the component B being selected from at least one of acetochlor, butachlor, metolachlor, dimethachlor, mesotrione, nicosulfuron, atrazine, terbuthylazine, s-metolachlor, and dimethenamid-P, and the weight ratio of the component A to the component B is 1:(1-80).

[0005] In a preferred embodiment, when component B is at least one of acetochlor, butachlor, metolachlor, dimethenachlor, s-metolachlor, and dimethenamid-P, the weight ratio of component A to component B is 1:(20-60).

[0006] In a preferred embodiment, when component B is at least one of mesotrione and nicosulfuron, the weight ratio of component A to component B is 1:(1-10).

[0007] In a preferred embodiment, when component B is at least one of atrazine, terbuthylazine, and dimetrizone, the weight ratio of component A to component B is 1:(10-50).

[0008] The inventors have found that after the active ingredients provided by Pyriminobac (ethyl 3-(2-chloro-4-fluoro-5-(3-methyl-2,6-dioxy-4-trifluoromethyl-3,6-dihydropyrimidin-1(2 H)-yl)phenyl)-5-methyl-4,5-dihydroisoxazole-5-carboxylate) and component B are mixed in a certain ratio, the unique mechanism of action of the two active ingredients can achieve synergistic effects without cross-resistance, broaden the herbicidal spectrum, improve the control effect, and play a role in compensating for the shortcomings of the low control effect of single-use agents against major weeds. At the same time, it can improve the sustained efficacy of each component of the composition, delay the occurrence of weed resistance, reduce the repeated use of pesticides, and reduce the amount and cost of use. It can be widely used in field crops.

[0009] A second aspect of the invention provides a herbicide composition formulation comprising a herbicide composition and a pesticidally acceptable adjuvant.

[0010] In a preferred embodiment, the formulation of the herbicidal composition is one selected from the group consisting of an emulsifiable concentrate, an aqueous emulsion, a microemulsion, a dispersible oil suspension, a suspoemulsion, a hydrate, and a water-dispersible granule.

[0011] In a more preferred embodiment, the weight percentage of the herbicidal composition in the herbicidal composition formulation is 1-90%.

[0012] In a more preferred embodiment, the formulation of the herbicidal composition is an aqueous emulsion, and the pesticidally acceptable adjuvants include at least one of a solvent, an emulsifier, a thickener, an antifreeze agent, an antifoam agent, a density adjuster, and a pH adjuster.

[0013] In the present invention, the raw materials for preparing the aqueous emulsion contain, by weight percentage, at least 1-60% of a herbicidal composition, 2-10% of an emulsifier, 1-5% of a thickener, 0.5-3% of an antifreeze agent, and a solvent to make up the remaining amount.

[0014] emulsifier An emulsifier is a compound that allows a liquid mixture of two or more mutually insoluble components to form a stable emulsion. Its mechanism of action is that during the emulsification period, the dispersed phase is dispersed in the continuous phase in the form of droplets (micron scale), and the emulsifier reduces the interfacial tension of each component in the mixed system and forms a stronger film on the surface of the droplets, or forms an electric double layer on the surface of the droplets due to the charge of the emulsifier, preventing the droplets from coagulating with each other and maintaining the emulsion in a uniform state. From the perspective of phase, the emulsion is still heterogeneous. The dispersed phase in the emulsion can be an aqueous phase or an oil phase, most of which is an oil phase. The continuous phase can be an oil phase or an aqueous phase, most of which is an aqueous phase. An emulsifier is a surfactant that has a hydrophilic group and a lipophilic group in the molecule. To express the hydrophilicity or lipophilicity of an emulsifier, the "hydrophilic-lipophilic balance value (HLB value)" is usually used, and the lower the HLB value, the higher the lipophilicity, and conversely, the higher the HLB value, the better the hydrophilicity. Different types of emulsifiers have different HLB values, and it is necessary to select an appropriate emulsifier to obtain a stable emulsion.

[0015] In the present invention, the emulsifier is at least one selected from alkylphenol ethoxylates, phenylethylphenol polyoxyethylene polyoxypropylene ethers, polyoxyethylene sorbitan monolaurate, polyoxyethylene sorbitan palmitate monoesters, polyoxyethylene sorbitan stearate monoesters, sorbitan oleate monoesters, sorbitan laurate, sorbitan monopalmitate, sorbitan stearate, castor oil polyoxyethylene ethers, alkylbenzenesulfonates, alkylnaphthalenesulfonates, and alkylsulfonates.

[0016] In a preferred embodiment, the emulsifier is a combination of castor oil polyoxyethylene ether, sorbitan monopalmitate and sodium dodecylbenzenesulfonate, in a weight ratio of (10-20):(1-5):1.

[0017] In a more preferred embodiment, the emulsifier is a combination of castor oil polyoxyethylene ether, sorbitan monopalmitate, and sodium dodecylbenzene sulfonate in a weight ratio of 16:3:1.

[0018] In the present invention, the HLB value of the castor oil polyoxyethylene ether is 11-16.

[0019] In a more preferred embodiment, the castor oil polyoxyethylene ether has an HLB value of 13-14.

[0020] In the present invention, the source of castor oil polyoxyethylene ether is not particularly limited, and examples thereof include Jiahua Chemical Co., Ltd., and its grades are EL-30, EL-40, HEL-40, EL-60, etc.

[0021] In the present invention, the source of the sorbitan monopalmitate is not particularly limited, and may be Jiangsu Haian Petrochemical Plant, the model number of which is S-40.

[0022] In the present invention, the source of the sodium dodecylbenzenesulfonate is not particularly limited, and may be Langfang Pengcai Fine Chemical Plant, etc.

[0023] Aqueous emulsions are O / W emulsion systems, which are thermodynamically unstable but kinetically stable multi-phase systems. The present invention improves the physical stability of aqueous emulsions at high temperatures and low temperatures through optimal blending. The inventors believe that blending castor oil polyoxyethylene ether, sorbitan monopalmitate and sodium dodecylbenzenesulfonate allows the emulsifier molecules to be closely arranged on the oil-water interface membrane, increasing the membrane strength and improving the emulsion stability, especially when the weight ratio of the three is (10-20):(1-5):1, the best effect can be obtained. Increasing the content of sorbitan monopalmitate reduces the HLB value of the mixed emulsifier, which leads to poor high temperature storage stability of the aqueous emulsion. This is because Pyriminoback (3-(2-chloro-4-fluoro-5-(3-methyl-2,6-dioxy-4-trifluoromethyl-3,6-dihydropyrimidin-1(2 H)-yl)phenyl)-5-methyl-4,5-dihydroisoxazole-5-carboxylate) dissolves in liquid under high temperature conditions and has a strong tendency to aggregate. At the same time, when the emulsifier is distributed at the oil-water interface, the proportion of lipophilic emulsifier increases, and the pulling force from the oil phase becomes greater than the pulling force from the water phase. When droplets collide, the emulsifier molecules are pushed into the oil phase, the film strength at the interface decreases, and the droplets are concentrated and appear in the transparent oil layer. The inventor also found that the stability of the aqueous emulsion diluent can be improved by adding a certain amount of sodium dodecylbenzenesulfonate, since the system contains a large amount of the emulsifier castor oil polyoxyethylene ether, which is highly hydrophilic. The higher the hydrophilicity of the mixed emulsifier, the higher the solubility of the organic solvent in water, leading to precipitation of crystals of the active pharmaceutical ingredient. Adding a small amount of sodium dodecylbenzenesulfonate reduces the solubility of the solvent in water and at the same time increases the stability of the emulsion to a certain extent, but excessive reduction may reduce the high-temperature storage stability of the emulsion.

[0024] Thickener Also called gelling agents, they are substances that can increase the viscosity of latex or liquids, and are also called pastes when used in food. Thickeners can increase the viscosity of a system and maintain the system in a uniform and stable suspension or emulsion state or form a gel. Most thickeners also have an emulsifying effect. They are divided into two categories: natural and synthetic. Most natural thickeners are prepared from plants and seaweeds containing polysaccharide viscous substances such as starch, gum arabic, pectin, agar, gelatin, sodium alginate, carrageenan, and dextrin, while general-purpose gelatin, soluble starch, polysaccharide derivatives, etc. are used in cosmetics. Synthetic thickeners include carboxymethylcellulose, propylene glycol alginate, methylcellulose, sodium starch phosphate, sodium carboxymethylcellulose, sodium alginate, casein, sodium polyacrylate, polyoxyethylene, polyvinylpyrrolidone, etc.

[0025] In the present invention, the thickener is not particularly limited, and examples thereof include xanthan gum, sodium hydroxymethylcellulose, polyvinyl alcohol, magnesium aluminum silicate, sodium alginate, guar gum, and gelatin.

[0026] In a preferred embodiment, the thickening agent is polyvinyl alcohol.

[0027] The inventor believes that when a certain amount of polyvinyl alcohol is added to the system as a thickener, the polyvinyl alcohol molecules are arranged in series around the surfactant micelles, forming a surfactant mixed film, improving the strength of the film, while at the same time reducing the tension of the oil-water interface and further improving the stability of the emulsion, while increasing the viscosity of the aqueous emulsion, reducing the stratification rate, and improving the physical stability of the emulsion at room temperature. This is because the higher the viscosity of the system, the greater the viscous resistance of the droplets moving in the continuous phase, the slower the moving speed, the lower the diffusion coefficient, and the slower the stratification, aggregation and concentration rate of the emulsion, resulting in higher stability. However, excessive thickeners should not be added. Otherwise, the fluidity of the aqueous emulsion will be poor, and the fluidity index of the product will be unqualified, which may affect the use of the product.

[0028] Antifreeze Deicers, also known as freeze inhibitors, are substances added to other liquids (usually water) to lower their freezing point and improve their deicing effect. They also melt ice crystals and inhibit their growth. They are primarily used in refrigeration systems for internal combustion engines, but are also used in air conditioning systems, solar energy systems, snow melting systems, and freeze drying.

[0029] In the present invention, the antifreeze agent is not particularly limited, and examples thereof include ethylene glycol, propylene glycol, glycerol, hexylene glycol, urea, and ammonium sulfate.

[0030] solvent

[0031] In the present invention, the solvent is a combination of an organic solvent and water.

[0032] In a preferred embodiment, the weight ratio of the organic solvent to the emulsifier is (2-5:1).

[0033] In a more preferred embodiment, the weight ratio of the organic solvent to the emulsifier is 3:1.

[0034] In the present invention, the organic solvent is at least one selected from the group consisting of hydrocarbon solvents, ketone solvents, ester solvents, alcohol solvents, and aromatic hydrocarbon solvents.

[0035] In a preferred embodiment, the organic solvent is a hydrocarbon solvent.

[0036] In a more preferred embodiment, the hydrocarbon solvent includes toluene, o-xylene, and solvent oil #150.

[0037] In a more preferred embodiment, the hydrocarbon solvent is Solvent Oil #150.

[0038] The inventors found that when the weight ratio of the solvent to the emulsifier is (2-5):1, the droplet distribution of the prepared aqueous emulsion becomes dense, the viscosity of the system increases, and the resistance to the movement of small droplets increases, and a sufficiently large amount of emulsifier forms a dense interfacial film at the oil-water interface of the small droplets, so that the small droplets are less likely to concentrate and demulsify, and the stability of the emulsion is improved. However, the addition of an excessive amount of solvent may cause phase inversion of the emulsion.

[0039] In addition, the inventor has found that when the lipophilic group of the emulsifier contains a double bond and the content of the hydrophilic group polyoxyethylene chain is within a reasonable range, the oil separation rate of the aqueous emulsion is reduced. The inventor believes that this is due to the aromatic hydrocarbon solvent containing a double bond. When the lipophilic group of the emulsifier also contains a double bond, the interaction between the lipophilic group and the oil molecules is strengthened, and under the pulling action of the shear of the channel of the liquid membrane, the relative movement of the lipophilic group and the oil molecules occurs, the driving effect on the oil molecules is enhanced, and the interfacial viscosity is also increased. Similarly, when the lipophilic group is longer, the interaction between adjacent oil molecules is also strengthened, the interfacial viscosity is improved, and the stability of the corresponding aqueous emulsion system is increased. When the polyoxyethylene polymerization number of the hydrophilic group of the active agent increases, the oxygen group contained in the hydrophilic group is easily hydrated, the stability of the film is reduced, and the polyoxyethylene curls in water, and its occupied area increases with the increase in the polymerization degree, the strength of the film is reduced, and the stability of the corresponding aqueous emulsion system is reduced. Therefore, when this system uses aromatic hydrocarbon as the solvent and castor oil polyoxyethylene ether, sorbitan monopalmitate and sodium dialkylbenzene sulfonate as the emulsifier, the stability of the prepared aqueous emulsion is the best.

[0040] water

[0041] In the present invention, the water is deionized water, distilled water, purified water, or the like.

[0042] The inventors believe that the water used in this system cannot be tap water, because tap water contains various inorganic ions, which increases the density difference between the water phase and the oil phase, resulting in a high centrifugal stratification rate.

[0043] In the present invention, the method for preparing the aqueous emulsion is as follows. (1) The herbicidal composition is dissolved in an organic solvent, an emulsifier is added, and the mixture is stirred uniformly to obtain an oil phase. (2) Mix the thickener and antifreeze with water to obtain the aqueous phase. (3) Under high-shear conditions, the oil phase is slowly added to the aqueous phase and shear is continued for 20-60 min.

[0044] A third aspect of the present invention is to provide the application of the herbicidal composition in pre-emergence soil treatment of field crops.

[0045] The present invention will be described in detail below by examples.It should be noted that the following examples are only used to further illustrate the present invention, and are not construed as limiting the scope of protection of the present invention.Some non-essential improvements and adjustments made by those skilled in the art according to the above content of the present invention shall still fall within the scope of protection of the present invention. Effect of the Invention

[0046] The present invention provides a herbicidal composition and an aqueous emulsion containing the herbicidal composition, the beneficial effects of which are as follows:

[0047] 1. Pyriminobac (ethyl 3-(2-chloro-4-fluoro-5-(3-methyl-2,6-dioxy-4-trifluoromethyl-3,6-dihydropyrimidin-1(2 H)-yl)phenyl)-5-methyl-4,5-dihydroisoxazole-5-carboxylate) combined with acetochlor, butachlor, metolachlor, dimethachlor, mesotrione, nicosulfuron, atrazine, terbutazone, terbuthylazine, s-metolachlor, and dimethenamid-P has a unique mechanism of action that does not cause cross-resistance, achieves synergistic effects, broadens the herbicidal spectrum, improves the control effect, and compensates for the shortcomings of low control effect of single-use agents against major weeds. At the same time, it improves the sustained effect of each component of the composition, delays the occurrence of weed resistance, reduces repeated use of pesticides, and reduces the amount and cost of use. It can be applied to pre-emergence soil treatment of field crops.

[0048] 2. Through screening and optimizing the types and contents of emulsifiers, solvents, etc., the obtained aqueous emulsion has stable quality and excellent performance, which is more conducive to the exertion of pharmaceutical efficacy. This aqueous emulsion does not undergo stratification, aggregation, coalescence and demulsification when stored at different temperatures, so the storage stability of the aqueous emulsion is greatly improved. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0049] Example 1

[0050] Example 1 provides an aqueous emulsion of a herbicidal composition, the preparation of which contains the following components by weight: 51% herbicidal composition, 4% emulsifier, 2% thickener, 1% antifreeze, 12% organic solvent, and water to make up the remainder.

[0051] The herbicidal composition is a combination of Pyriminobac (ethyl 3-(2-chloro-4-fluoro-5-(3-methyl-2,6-dioxy-4-trifluoromethyl-3,6-dihydropyrimidin-1(2H)-yl)phenyl)-5-methyl-4,5-dihydroisoxazole-5-carboxylate) and acetochlor, with a weight ratio of 1:50. The emulsifier is a combination of castor oil polyoxyethylene ether, sorbitan monopalmitate and sodium dodecylbenzenesulfonate, with a weight ratio of 16:3:1. The castor oil polyoxyethylene ether is purchased from Jiahua Chemical Co., Ltd., with grade EL-30. The sorbitan monopalmitate is purchased from Jiangsu Haian Petrochemical Plant, with model number S-40. The sodium dodecylbenzenesulfonate is purchased from Langfang Pengcai Fine Chemical Co., Ltd. The thickening agent is polyvinyl alcohol, the antifreeze is glycerol, and the organic solvent is solvent oil # 150. The water is deionized water.

[0052] The aqueous emulsion was prepared as follows. (1) The herbicidal composition is dissolved in an organic solvent, an emulsifier is added, and the mixture is stirred uniformly to obtain an oil phase. (2) Mix the thickener and antifreeze with water to obtain the aqueous phase. (3) Under high-speed shear conditions, the oil phase is slowly added to the aqueous phase, and the shear is continued for 40 min. Example 2

[0053] Example 2 provides an aqueous emulsion of a herbicidal composition, the preparation raw material of the emulsion includes the following components by weight: 30% herbicidal composition, 3% emulsifier, 1% thickener, 0.5% antifreeze agent, 15% organic solvent, and water to make up the remaining amount.

[0054] The herbicidal composition is a combination of Pyriminobac (ethyl 3-(2-chloro-4-fluoro-5-(3-methyl-2,6-dioxy-4-trifluoromethyl-3,6-dihydropyrimidin-1(2 H)-yl)phenyl)-5-methyl-4,5-dihydroisoxazole-5-carboxylate) and s-metolachlor, with a weight ratio of 1:50. The emulsifier is a combination of castor oil polyoxyethylene ether, sorbitan monopalmitate and sodium dodecylbenzenesulfonate, with a weight ratio of 10:1:1. The castor oil polyoxyethylene ether is purchased from Jiahua Chemical Co., Ltd., with grade EL-30. The sorbitan monopalmitate is purchased from Jiangsu Haian Petrochemical Plant, with model number S-40. The sodium dodecylbenzenesulfonate is purchased from Langfang Pengcai Fine Chemical Co., Ltd. The thickening agent is polyvinyl alcohol, the antifreeze is glycerol, the organic solvent is solvent oil #150, and the water is deionized water.

[0055] The aqueous emulsion was prepared as follows. (1) The herbicidal composition is dissolved in an organic solvent, an emulsifier is added, and the mixture is stirred uniformly to obtain an oil phase. (2) Mix the thickener and antifreeze with water to obtain the aqueous phase. (3) Under high-speed shear conditions, the oil phase is slowly added to the aqueous phase, and the shear is continued for 40 min. Example 3

[0056] Example 3 provides an aqueous emulsion of a herbicidal composition, the preparation raw material of the emulsion comprises the following components by weight: 12% herbicidal composition, 8% emulsifier, 5% thickener, 3% antifreeze agent, 24% organic solvent, and water to make up the remainder.

[0057] The herbicidal composition is a combination of Pyriminobac (ethyl 3-(2-chloro-4-fluoro-5-(3-methyl-2,6-dioxy-4-trifluoromethyl-3,6-dihydropyrimidin-1(2H)-yl)phenyl)-5-methyl-4,5-dihydroisoxazole-5-carboxylate) and Nicosulfuron, with a weight ratio of 1:5. The emulsifier is a combination of castor oil polyoxyethylene ether, sorbitan monopalmitate and sodium dodecylbenzenesulfonate, with a weight ratio of 20:5:1. The castor oil polyoxyethylene ether is purchased from Jiahua Chemical Co., Ltd., with grade EL-30. The sorbitan monopalmitate is purchased from Jiangsu Haian Petrochemical Plant, with model number S-40. The sodium dodecylbenzenesulfonate is purchased from Langfang Pengcai Fine Chemical Co., Ltd. The thickening agent is polyvinyl alcohol, the antifreeze is glycerol, the organic solvent is solvent oil #150, and the water is deionized water.

[0058] The aqueous emulsion was prepared as follows. (1) The herbicidal composition is dissolved in an organic solvent, an emulsifier is added, and the mixture is stirred uniformly to obtain an oil phase. (2) Mix the thickener and antifreeze with water to obtain the aqueous phase. (3) Under high-speed shear conditions, the oil phase is slowly added to the aqueous phase, and the shear is continued for 40 min. Example 4

[0059] The difference between Example 4 and Example 1 is that the emulsifier does not contain castor oil polyoxyethylene ether. Example 5

[0060] The difference between Example 5 and Example 1 is that nonylphenol polyoxyethylene ether is used instead of the castor oil polyoxyethylene ether, which is purchased from Nantong Runfeng Petrochemical Co., Ltd. Example 6

[0061] The difference between Example 6 and Example 1 is that the emulsifier does not contain sorbitan monopalmitate. Example 7

[0062] The difference between Example 7 and Example 1 is that the emulsifier does not contain sodium dodecylbenzenesulfonate. Example 8

[0063] The difference between Example 8 and Example 1 is that the thickening agent is xanthan gum. Example 9

[0064] The difference between Example 9 and Example 1 is that the solvent is dimethylformamide. Example 10

[0065] The difference between Example 10 and Example 1 is that the weight ratio of the solvent to the emulsifier is 10:1. Example 11

[0066] The difference between Example 11 and Example 1 is that the herbicidal composition is a combination of Pyriminobac (ethyl 3-(2-chloro-4-fluoro-5-(3-methyl-2,6-dioxy-4-trifluoromethyl-3,6-dihydropyrimidin-1(2H)-yl)phenyl)-5-methyl-4,5-dihydroisoxazole-5-carboxylate) and acetochlor, the weight ratio is 1:30. (Performance test)

[0067] 1. High temperature storage stability test: The aqueous emulsion is placed in the same graduated test tube with a well-sealed stopper and stored in a water bath for 14 days. After high temperature storage, if the system is homogeneous and the water separation rate is less than 10%, it is considered to be passed; otherwise, it is considered to be failed.

[0068] 2. Freeze-thaw stability test: Place the aqueous emulsion in a stoppered graduated test tube, freeze in a refrigerator at -10℃ for 18 hours, then place in the refrigerator. Repeat this process three times to observe whether the oil precipitates. If there is any precipitation of the oil phase, it is considered to be a failure, otherwise it is considered to be a pass.

[0069] 3. Emulsion stability test: The aqueous emulsion is diluted 200 times with 342 ppm standard hard water, and left to stand in a 30°C thermostatic water bath for 1 hour before being removed. The emulsion is observed for separation; if there is no oil film on the top and no sediment on the bottom, the stability is deemed to have passed; otherwise, it is deemed to have failed. The performance test results of the examples are shown in Table 1. [Table 1]

[0070] 4. Control effect test: Sample: 95% Pyriminovac (3-(2-chloro-4-fluoro-5-(3-methyl-2,6-dioxy-4-trifluoromethyl-3,6-dihydropyrimidin-1(2H)-yl)phenyl)-5-methyl-4,5-dihydroisoxazole-5-carboxylate ethyl) drug substance, 81.5% acetochlor emulsifiable concentrate Crops: Corn: Common varieties grown on a large scale in the market (Tiezhan 505, Kejujia 2323) weed: Annual weeds such as velvet, pigweed, morning glory, amaranth, day cherries, wild watermelon seedlings, sedge, tsingle-leaved radish, Japanese laurel, Japanese laurel, cowpea, wild millet, green foxtail, catkin, horseweed, barnyard grass, sparrow, wild oats, wheatgrass, Japanese knotweed, and green foxtail. Chemical application method: Add 45 kg of water per mu and spray on the soil (sow corn and weed seeds together, spray 24 hours after sowing). Test result statistics and analysis: ED of the test drug 50 / ED 90 Calculating values Calculate with DPS statistical analysis software Calculation of cotoxicity factor:

number

[0071] 5.Tabata Efficacy Test: Test Drugs: Example 1 Herbicidal composition aqueous emulsion Control: 10% Pyriminoback (3-(2-chloro-4-fluoro-5-(3-methyl-2,6-dioxy-4-trifluoromethyl-3,6-dihydropyrimidin-1(2H)-yl)phenyl)-5-methyl-4,5-dihydroisoxazole-5-carboxylate ethyl) aqueous emulsion (Nantong Jiangshan Agricultural Chemical Co., Ltd.), 81.5% Acetochlor emulsifiable concentrate (Nantong Jiangshan Agricultural Chemical Co., Ltd.) Test Crops: Corn (variety: Soyokumo No. 11) Target for control: Annual weeds (mainly horseweed, cowweed, horseweed, radish, radish, etc.) Test Method: Area division: 20m 2 ,are randomly arranged, and each treatment is repeated three times. Usage: Before and after sowing corn, spray evenly on the ground surface with 45kg of water per mu, and spray once before sowing corn. Survey, recording and measurement methods Weather Data: The weather on the day of the test was clear and sunny with a light breeze. Temperatures were normal during the test, and the test drug was effective as normal. Field management data: Base fertilizer 45%, chemical fertilizer 50kg / mu. Other field management such as disease prevention and top dressing is done according to normal management. Weed survey: Visually observe the overall weed control effect on the 7th, 10th, 15th, 30th, and 45th days after application of the test chemical. Survey method: Visual inspection. How to calculate efficacy: Record the percentage of relative control based on visual observations. Crop survey: The germination status of corn is visually observed after sowing, and the number of seedlings is counted three times, 4, 7, and 12 days after sowing. The growth status of corn is observed 32 and 47 days after sowing. Research method: 20 plants were set up for each treatment to observe the stability of different application rates on corn. The results of the investigation into the effectiveness of the test drugs against weeds are as follows: [Table 3] The results of the investigation into the safety of the test drugs on agricultural crops are as follows: [Table 4]

[0072] The above examples are merely illustrative of some features of the methods described herein. The appended claims are intended to claim the broadest possible scope, and the examples described herein are intended to describe embodiments selected according to all possible combinations of examples. It is therefore the applicant's intention that the appended claims are not limited by the selection of examples that illustrate the features of the invention. Any numerical ranges used in the claims include subranges contained therein, and variations within these ranges, if possible, are to be construed as being included within the scope of the appended claims.

Claims

1. A herbicidal composition formulation comprising a herbicidal composition and a pesticidally acceptable adjuvant, The herbicidal composition comprises a component A and a component B, the component A being (ethyl 3-(2-chloro-4-fluoro-5-(3-methyl-2,6-dioxy-4-trifluoromethyl-3,6-dihydropyrimidin-1(2H)-yl)phenyl)-5-methyl-4,5-dihydroisoxazole-5-carboxylate), the component B being at least one selected from acetochlor, nicosulfuron, and s-metolachlor, and the weight ratio of the component A to the component B being 1:(20-60); The formulation of the herbicidal composition is an aqueous emulsion, and the agriculturally acceptable adjuvant includes at least one of a solvent, an emulsifier, a thickener, an antifreeze agent, an antifoaming agent, a density adjuster, and a pH adjuster; The emulsifier is a combination of castor oil polyoxyethylene ether, sorbitan monopalmitate and sodium dodecylbenzenesulfonate, and the weight ratio thereof is (10-20):(1-5):

1.

2. The herbicidal composition formulation according to claim 1, characterized in that the weight percentage of the herbicidal composition in the herbicidal composition formulation is 1-90%.

3. The herbicidal composition formulation according to claim 1, characterized in that the solvent is a combination of an organic solvent and water, and the weight ratio of the organic solvent to the emulsifier is (2-5):

1.

4. The herbicidal composition formulation according to claim 3, wherein the organic solvent is at least one selected from the group consisting of hydrocarbon solvents, ketone solvents, ester solvents, alcohol solvents, and aromatic hydrocarbon solvents.

5. The application of the herbicidal composition formulation according to any one of claims 1 to 4, characterized in that it is used for pre-emergence soil treatment of field crops.

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