A ternary herbicidal suspoemulsion containing 2,4-dichlorophenoxyacetic acid isooctyl ester, terbuthylazine and acetochlor, its preparation method and application

Abstract

This invention provides a ternary herbicidal suspension emulsion containing 2,4-D isooctyl ester, terbutaline, and acetochlor. Its preparation components include: 2,4-D isooctyl ester, terbutaline, acetochlor, a dispersant; an emulsifier; a stabilizer; a dispersion medium; other adjuvants; and water. The stabilizer comprises vitamin E polyethylene glycol succinate and modified silica. This invention, through the specific ratio of 2,4-D isooctyl ester, terbutaline, and acetochlor, expands the weeding range and improves the weeding effect, offering advantages such as rapid and thorough weed control with low toxicity. The specific stabilizer used in this invention results in finer particle size and higher suspension rate during the grinding process. By selecting a suitable emulsifier and considering the characteristics of cornfields and the properties of the active ingredient, this invention achieves excellent weeding performance without affecting crop growth and development.

Description

Technical Field

[0001] This invention relates to the field of agricultural technology, and in particular to a ternary herbicidal suspension emulsion containing 2,4-D isooctyl ester, tert-butyl ester and acetochlor, its preparation method and application. Background Technology

[0002] Corn is a widely cultivated economic crop in my country. During spring sowing, it is often infested with a variety of weeds such as barnyard grass, foxtail grass, etc., which can cover more than 90% of the sown area in severe cases. Therefore, weed control is necessary.

[0003] Existing pesticide technologies and products targeting corn weeds are showing signs of weakness. Long-term use of single herbicides has led to severe herbicide resistance in some weeds nationwide, such as crabgrass, velvetleaf, field bindweed, horsetail, and black nightshade. It is reported that globally, 65 weed species and 233 biotypes have developed resistance to atrazine. Conventional application rates are insufficient to kill weeds, while excessive use can cause phytotoxicity to corn. Furthermore, many companies simply repeat existing formulations of atrazine, acetochlor, nicosulfuron, and mesotrione, with few new products appearing on the market.

[0004] Phenoxycarboxylic acid herbicides are a type of hormone-based herbicide. They are systemic and can be rapidly absorbed by the roots and leaves of plants and transported throughout the plant, resulting in excessively high hormone concentrations within the weeds, which in turn affects the plant's cell growth and metabolism.

[0005] Chinese patent CN112088887B discloses a herbicidal suspension emulsion for sedge crops, its preparation method, application, and administration method. By combining metolachlor, S-metolachlor, and propyzamide in a specific ratio, it demonstrates high efficacy against both emerging annual weeds and weeds already emerging at the time of application, and exhibits high safety for tiger peas. However, the metabolites of S-metolachlor migrate into soil, surface water, and groundwater after degradation. In early 2023, the French Agency for Food, Environment and Occupational Health and Safety (Anses) announced on its website that it had initiated a procedure to remove the active herbicide S-metolachlor from primary crop protection uses, aiming to reduce environmental pollution from this substance and its metabolites and gradually restore groundwater quality.

[0006] Chinese patent CN110352974A discloses a post-emergence early-stage herbicidal active composition and herbicide. Component A is quizalofop-P-ethyl or clethodim, component B is chlorpyrifos-methyl, and component C is acetochlor or metolachlor. It has the characteristics of high efficiency, safety, broad spectrum of weed control, stable efficacy under low temperature and drought conditions, and safety for major subsequent crops. However, quizalofop-P-ethyl requires an increased dosage to achieve better control when the weeds are older. When the weeds are too old or have already begun to head, the control effect of this herbicide is extremely poor. The control effect of quizalofop-P-ethyl is poor when applied during the flowering period of soybeans.

[0007] To address the shortcomings of existing technologies, this invention provides a suspension emulsion specifically designed for weed control in cornfields. It effectively removes weeds, is highly safe, has minimal impact on corn, and has a wide range of applications. Summary of the Invention

[0008] The first aspect of this invention provides a ternary herbicidal suspension emulsion containing 2,4-D isooctyl ester, terbutaline, and acetochlor, the preparation components of which include:

[0009] 2,4-D isooctyl ester;

[0010] Terbutinzine;

[0011] Acetochlor;

[0012] Dispersant;

[0013] Emulsifier;

[0014] Stabilizer;

[0015] Dispersion medium;

[0016] Other adjuvants;

[0017] water;

[0018] The stabilizers mentioned above include vitamin E polyethylene glycol succinate and modified silica.

[0019] In one embodiment of the present invention, the emulsifier comprises an amphoteric surfactant and a nonionic surfactant.

[0020] In one embodiment of the present invention, the amphoteric surfactant comprises alkyl betaine or biuret.

[0021] In one embodiment of the present invention, the nonionic surfactant includes Atlox4913 and Termu11284.

[0022] In one embodiment of the present invention, the dispersant includes polycarboxylate dispersants and polycarboxylate dispersants.

[0023] In one embodiment of the present invention, the polycarboxylate dispersant is AkzoAgrlian-700, and the polycarboxylate dispersant is Croda Metasoerse-550S and Dow Duramax D-518.

[0024] In one embodiment of the present invention, the dispersion medium includes one or more of modified castor oil, methyl oleate, and soybean oil.

[0025] In one embodiment of the present invention, other additives include defoamers, antifreeze agents, preservatives, and pH adjusters; wherein the defoamer is an organosilicon defoamer; and the antifreeze agent is selected from one or more of propylene glycol, ethylene glycol, polyethylene glycol 400, and glycerol.

[0026] The preservative is selected from one or more of potassium sorbate, sodium benzoate, isothiazolinone, and benzisothiazolinone.

[0027] A second aspect of the present invention provides the application of a ternary herbicidal suspension emulsion containing 2,4-D isooctyl ester, terbutaline and acetochlor in the control of annual weeds in spring maize fields.

[0028] A third aspect of the present invention provides a method for preparing a ternary herbicidal suspension emulsion containing 2,4-D isooctyl ester, terbutaline, and acetochlor, the method comprising:

[0029] Terbutaline suspension, 2,4-D isooctyl ester emulsifiable concentrate, and acetochlor emulsifiable concentrate are obtained by stirring, mixing, grinding, and / or high-speed shearing; finally, the emulsifiable concentrate is added to the suspension, and the suspension emulsion is obtained by grinding and / or high-speed shearing.

[0030] By adopting the above technical solution, the present invention has the following beneficial effects:

[0031] 1. This invention expands the weeding range and improves the weeding effect by compounding 2,4-D isooctyl ester, terbutaline, and acetochlor in a specific ratio, and has the advantages of fast weeding, thorough weeding and low toxicity.

[0032] 2. The present invention uses specific stabilizers to obtain finer particle sizes and higher suspension rates during the grinding process;

[0033] 3. By selecting a suitable emulsifier and taking into account the characteristics of cornfields and the properties of the active ingredient, this invention enables the product to have excellent herbicidal performance without affecting crop growth and development. Detailed Implementation

[0034] The technical solution of the present invention will be clearly and completely described below. Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0035] The first aspect of this invention provides a ternary herbicidal suspension emulsion containing 2,4-D isooctyl ester, terbutaline, and acetochlor, the preparation components of which include:

[0036] 2,4-D isooctyl ester

[0037] Terbutinzine

[0038] Acetochlor

[0039] Dispersant;

[0040] Emulsifier;

[0041] Stabilizer;

[0042] Dispersion medium;

[0043] Other adjuvants;

[0044] water;

[0045] The stabilizers mentioned above include vitamin E polyethylene glycol succinate and modified silica.

[0046] In a preferred embodiment of the present invention, the ternary herbicidal suspension emulsion containing 2,4-D isooctyl ester, terbutaline, and acetochlor comprises the following components:

[0047]

[0048]

[0049] Dispersant: Primarily wets the surface particles of solid pesticides, facilitating grinding and allowing for better dispersion of the pesticide's solid active ingredients in the continuous phase (water). It also improves the stability of the aqueous and oil phases within the overall system. In this invention, the dispersant comprises polycarboxylate dispersants and polycarboxylate dispersants; the polycarboxylate dispersant is AkzoAgrlian-700, and the polycarboxylate dispersants are Croda Metasoerse-550S and Dow Duramax D-518, with a ratio of Croda Metasoerse-550S to Dow Duramax D-518 of 8:1; and the mass ratio of the polycarboxylate dispersant to the polycarboxylate dispersant is 1:3.

[0050] Emulsifier: An emulsifier can reduce the surface tension between oil and water, allowing the emulsion phase to disperse better in water, reducing flocculation, and improving system stability. In this invention, the emulsifier comprises amphoteric surfactants and nonionic surfactants.

[0051] In this invention, the amphoteric surfactant is alkyl betaine or biuret; specifically, it is dodecyl betaine.

[0052] In this invention, the nonionic surfactants are Atlox4913 and Termu1 1284.

[0053] Stabilizers: The stabilizers described in this invention include vitamin E polyethylene glycol succinate and modified silica.

[0054] The modified silica is prepared as follows: silica, sodium metabisulfite, sodium acrylate and water are ultrasonically mixed in proportion, the mixture is dried at a constant temperature, and the dried product is irradiated with an electron beam with an energy of 5-10 keV and a dose of 10-40 kGy for 5-10 min.

[0055] Preferably, the weight ratio of silicon dioxide, sodium metabisulfite, sodium acrylate, and water is 50:(1-3):(3-4):(100-300).

[0056] Preferably, the silica has a particle size of 0.1-0.15 μm and a specific surface area of ​​15-27 m². 2 / g, purchased from Shandong Boken Silicon Materials Co., Ltd., model BK94.

[0057] Dispersion medium: The dispersion medium includes one or more of modified castor oil, methyl oleate, and soybean oil.

[0058] Other additives: The other additives mentioned in this invention include defoamers, antifreeze agents, preservatives, and pH adjusters; wherein the defoamer is an organosilicon defoamer, specifically BYK-080 from BYK Corporation. The antifreeze agent is selected from one or more of propylene glycol, ethylene glycol, polyethylene glycol 400, and glycerol; specifically ethylene glycol.

[0059] The preservative is selected from one or more of potassium sorbate, sodium benzoate, isothiazolinone, and benzisothiazolinone; specifically, sodium benzoate.

[0060] The pH adjuster is sodium hydroxide.

[0061] A second aspect of the present invention provides the application of a ternary herbicidal suspension emulsion containing 2,4-D isooctyl ester, terbutaline and acetochlor in the control of annual weeds in spring maize fields.

[0062] A third aspect of the present invention provides a method for preparing a ternary herbicidal suspension emulsion containing 2,4-D isooctyl ester, terbutaline, and acetochlor, the method comprising:

[0063] Terbutaline suspension, 2,4-D isooctyl ester emulsifiable concentrate, and acetochlor emulsifiable concentrate are obtained by stirring, mixing, grinding, and / or high-speed shearing; finally, the emulsifiable concentrate is added to the suspension, and the suspension emulsion is obtained by grinding and / or high-speed shearing.

[0064] The present invention will be further explained below with reference to specific embodiments.

[0065] Example 1

[0066] This embodiment provides a ternary herbicidal suspension emulsion containing 2,4-D isooctyl ester, terbutaline, and acetochlor, the preparation components of which include:

[0067]

[0068] The dispersants are Croda Metasoerse-550S, Dow Duramax D-518, and Akzo Agrlian-700, with a mass ratio of 8:1:3.

[0069] The emulsifiers are dodecyl betaine, Atlox 4913 and Termu1 1284, in a mass ratio of 2:1:1.

[0070] The stabilizer comprises vitamin E polyethylene glycol succinate and modified silica in a mass ratio of 3:1.

[0071] The modified silica is prepared as follows: 50 parts by weight of silica, 2 parts by weight of sodium metabisulfite, 3 parts by weight of sodium acrylate and 200 parts by weight of water are ultrasonically mixed, the mixture is dried at a constant temperature, and the dried product is irradiated with an electron beam of 8 keV and a dose of 30 kGy for 10 min.

[0072] The silica has a particle size of 0.1-0.15 μm and a specific surface area of ​​15-27 m². 2 / g, purchased from Shandong Boken Silicon Materials Co., Ltd., model BK94.

[0073] The dispersion medium is methyl oleate. The defoamer is BYK-080 from BYK Corporation; the antifreeze is ethylene glycol; and the preservative is sodium benzoate.

[0074] A second aspect of the present invention provides a method for preparing the suspension emulsion:

[0075] S01 mixes tert-butylamine, stabilizer, nonionic surfactant, Croda Metasoerse-550S, Dow Duramax D-518 and water by grinding to obtain tert-butylamine suspension.

[0076] Zirconium beads were used as the grinding media, the grinding time was 2 hours, and the rotation speed was 1300 rpm.

[0077] S02 is prepared by grinding and stirring 2,4-dip isooctyl ester, acetochlor, dispersion medium and remaining emulsifier to obtain emulsifiable oil;

[0078] S03 involves mixing emulsifiable concentrate and suspending agent under high shear, then adding the remaining raw materials, and finally preparing the suspension emulsion through modulation and mixing.

[0079] The shear emulsification time was 30 minutes and the rotation speed was 2500 rpm.

[0080] Example 2

[0081] This embodiment provides a ternary herbicidal suspension emulsion containing 2,4-D isooctyl ester, terbutaline, and acetochlor, the preparation components of which include:

[0082]

[0083] The dispersants are Croda Metasoerse-550S, Dow Duramax D-518, and Akzo Agrlian-700, with a mass ratio of 8:1:3.

[0084] The emulsifiers are dodecyl betaine, Atlox 4913 and Termu1 1284, in a mass ratio of 2:1:1.

[0085] The stabilizer is modified silica.

[0086] The modified silica is prepared as follows: 50 parts by weight of silica, 2 parts by weight of sodium metabisulfite, 3 parts by weight of sodium acrylate and 200 parts by weight of water are ultrasonically mixed, the mixture is dried at a constant temperature, and the dried product is irradiated with an electron beam of 8 keV and a dose of 30 kGy for 10 min.

[0087] The silica has a particle size of 0.1-0.15 μm and a specific surface area of ​​15-27 m². 2 / g, purchased from Shandong Boken Silicon Materials Co., Ltd., model BK94.

[0088] The dispersion medium is methyl oleate. The defoamer is BYK-080 from BYK Corporation; the antifreeze is ethylene glycol; and the preservative is sodium benzoate.

[0089] A second aspect of the present invention provides a method for preparing the suspension emulsion:

[0090] S01 mixes tert-butylamine, stabilizer, nonionic surfactant, Croda Metasoerse-550S, Dow Duramax D-518 and water by grinding to obtain tert-butylamine suspension.

[0091] Zirconium beads were used as the grinding media, the grinding time was 2 hours, and the rotation speed was 1300 rpm.

[0092] S02 is prepared by grinding and stirring 2,4-dip isooctyl ester, acetochlor, dispersion medium and remaining emulsifier to obtain emulsifiable oil;

[0093] S03 involves mixing emulsifiable concentrate and suspending agent under high shear, then adding the remaining raw materials, and finally preparing the suspension emulsion through modulation and mixing.

[0094] The shear emulsification time was 30 minutes and the rotation speed was 2500 rpm.

[0095] Example 3

[0096] This embodiment provides a ternary herbicidal suspension emulsion containing 2,4-D isooctyl ester, terbutaline, and acetochlor, the preparation components of which include:

[0097]

[0098]

[0099] The dispersants are Croda Metasoerse-550S, Dow Duramax D-518, and Akzo Agrlian-700, with a mass ratio of 8:1:3.

[0100] The emulsifiers are dodecyl betaine, Atlox 4913 and Termu1 1284, in a mass ratio of 2:1:1.

[0101] The stabilizer includes vitamin E polyethylene glycol succinate.

[0102] A second aspect of the present invention provides a method for preparing the suspension emulsion:

[0103] S01 mixes tert-butylamine, stabilizer, nonionic surfactant, Croda Metasoerse-550S, Dow Duramax D-518 and water by grinding to obtain tert-butylamine suspension.

[0104] Zirconium beads were used as the grinding media, the grinding time was 2 hours, and the rotation speed was 1300 rpm.

[0105] S02 is prepared by grinding and stirring 2,4-dip isooctyl ester, acetochlor, dispersion medium and remaining emulsifier to obtain emulsifiable oil;

[0106] S03 involves mixing emulsifiable concentrate and suspending agent under high shear, then adding the remaining raw materials, and finally preparing the suspension emulsion through modulation and mixing.

[0107] The shear emulsification time was 30 minutes and the rotation speed was 2500 rpm.

[0108] Example 4

[0109] This embodiment provides a ternary herbicidal suspension emulsion containing 2,4-D isooctyl ester, terbutaline, and acetochlor, the preparation components of which include:

[0110]

[0111]

[0112] The dispersants are Croda Metasoerse-550S, Dow Duramax D-518, and Akzo Agrlian-700, with a mass ratio of 8:1:3.

[0113] The emulsifiers are dodecyl betaine, Atlox 4913 and Termu1 1284, in a mass ratio of 2:1:1.

[0114] The stabilizer comprises vitamin E polyethylene glycol succinate and modified silica in a mass ratio of 3:1.

[0115] The modified silica is prepared as follows: 50 parts by weight of silica, 2 parts by weight of sodium metabisulfite, 3 parts by weight of sodium acrylate and 200 parts by weight of water are ultrasonically mixed, the mixture is dried at a constant temperature, and the dried product is irradiated with an electron beam of 8 keV and a dose of 30 kGy for 10 min.

[0116] The silica has a particle size of 20 μm and a specific surface area of ​​4-5 m². 2 / g, purchased from Ningbo Jinlei Nanotechnology Co., Ltd., model number JL-SiO2-W20.

[0117] The dispersion medium is methyl oleate. The defoamer is BYK-080 from BYK Corporation; the antifreeze is ethylene glycol; and the preservative is sodium benzoate.

[0118] A second aspect of the present invention provides a method for preparing the suspension emulsion:

[0119] S01 mixes tert-butylamine, stabilizer, nonionic surfactant, Croda Metasoerse-550S, Dow Duramax D-518 and water by grinding to obtain tert-butylamine suspension.

[0120] Zirconium beads were used as the grinding media, the grinding time was 2 hours, and the rotation speed was 1300 rpm.

[0121] S02 is prepared by grinding and stirring 2,4-dip isooctyl ester, acetochlor, dispersion medium and remaining emulsifier to obtain emulsifiable oil;

[0122] S03 involves mixing emulsifiable concentrate and suspending agent under high shear, then adding the remaining raw materials, and finally preparing the suspension emulsion through modulation and mixing.

[0123] The shear emulsification time was 30 minutes and the rotation speed was 2500 rpm.

[0124] Example 5

[0125] This embodiment provides a ternary herbicidal suspension emulsion containing 2,4-D isooctyl ester, terbutaline, and acetochlor, the preparation components of which include:

[0126]

[0127] The dispersants are Croda Metasoerse-550S, Dow Duramax D-518, and Akzo Agrlian-700, with a mass ratio of 8:1:3.

[0128] The emulsifiers are Atlox4913 and Termu1 1284 in a mass ratio of 1:1.

[0129] The stabilizer comprises vitamin E polyethylene glycol succinate and modified silica in a mass ratio of 3:1.

[0130] The modified silica is prepared as follows: 50 parts by weight of silica, 2 parts by weight of sodium metabisulfite, 3 parts by weight of sodium acrylate and 200 parts by weight of water are ultrasonically mixed, the mixture is dried at a constant temperature, and the dried product is irradiated with an electron beam of 8 keV and a dose of 30 kGy for 10 min.

[0131] The silica has a particle size of 0.1-0.15 μm and a specific surface area of ​​15-27 m². 2 / g, purchased from Shandong Boken Silicon Materials Co., Ltd., model BK94.

[0132] The dispersion medium is methyl oleate. The defoamer is BYK-080 from BYK Corporation; the antifreeze is ethylene glycol; and the preservative is sodium benzoate.

[0133] A second aspect of the present invention provides a method for preparing the suspension emulsion:

[0134] S01 mixes tert-butylamine, stabilizer, nonionic surfactant, Croda Metasoerse-550S, Dow Duramax D-518 and water by grinding to obtain tert-butylamine suspension.

[0135] Zirconium beads were used as the grinding media, the grinding time was 2 hours, and the rotation speed was 1300 rpm.

[0136] S02 is prepared by grinding and stirring 2,4-dip isooctyl ester, acetochlor, dispersion medium and remaining emulsifier to obtain emulsifiable oil;

[0137] S03 involves mixing emulsifiable concentrate and suspending agent under high shear, then adding the remaining raw materials, and finally preparing the suspension emulsion through modulation and mixing.

[0138] The shear emulsification time was 30 minutes and the rotation speed was 2500 rpm.

[0139] Example 6

[0140] This embodiment provides a ternary herbicidal suspension emulsion containing 2,4-D isooctyl ester, terbutaline, and acetochlor, the preparation components of which include:

[0141]

[0142] The dispersants are Croda Metasoerse-550S, Dow Duramax D-518, and Akzo Agrlian-700, with a mass ratio of 8:1:3.

[0143] The emulsifiers are dodecyl betaine, Atlox 4913 and Termu1 1284, in a mass ratio of 2:1:1.

[0144] The stabilizer comprises vitamin E polyethylene glycol succinate and modified silica in a mass ratio of 1:1.

[0145] The modified silica is prepared as follows: 50 parts by weight of silica, 2 parts by weight of sodium metabisulfite, 3 parts by weight of sodium acrylate and 200 parts by weight of water are ultrasonically mixed, the mixture is dried at a constant temperature, and the dried product is irradiated with an electron beam of 8 keV and a dose of 30 kGy for 10 min.

[0146] The silica has a particle size of 0.1-0.15 μm and a specific surface area of ​​15-27 m². 2 / g, purchased from Shandong Boken Silicon Materials Co., Ltd., model BK94.

[0147] The dispersion medium is methyl oleate. The defoamer is BYK-080 from BYK Corporation; the antifreeze is ethylene glycol; and the preservative is sodium benzoate.

[0148] A second aspect of the present invention provides a method for preparing the suspension emulsion:

[0149] S01 mixes tert-butylamine, stabilizer, nonionic surfactant, Croda Metasoerse-550S, Dow Duramax D-518 and water by grinding to obtain tert-butylamine suspension.

[0150] Zirconium beads were used as the grinding media, the grinding time was 2 hours, and the rotation speed was 1300 rpm.

[0151] S02 is prepared by grinding and stirring 2,4-dip isooctyl ester, acetochlor, dispersion medium and remaining emulsifier to obtain emulsifiable oil;

[0152] S03 involves mixing emulsifiable concentrate and suspending agent under high shear, then adding the remaining raw materials, and finally preparing the suspension emulsion through modulation and mixing.

[0153] The shear emulsification time was 30 minutes and the rotation speed was 2500 rpm.

[0154] Example 7

[0155] This embodiment provides a ternary herbicidal suspension emulsion containing 2,4-D isooctyl ester, terbutaline, and acetochlor, the preparation components of which include:

[0156]

[0157] The dispersants are Croda Metasoerse-550S, Dow Duramax D-518, and Akzo Agrlian-700, with a mass ratio of 8:1:3.

[0158] The emulsifiers are dodecyl betaine, Atlox 4913 and Termu1 1284, in a mass ratio of 2:1:1.

[0159] The stabilizer comprises vitamin E polyethylene glycol succinate and modified silica in a mass ratio of 3:1.

[0160] The modified silica is prepared as follows: 50 parts by weight of silica, 2 parts by weight of sodium metabisulfite, 3 parts by weight of sodium acrylate and 200 parts by weight of water are ultrasonically mixed, the mixture is dried at a constant temperature, and the dried product is irradiated with an electron beam of 8 keV and a dose of 30 kGy for 10 min.

[0161] The silica has a particle size of 0.1-0.15 μm and a specific surface area of ​​15-27 m². 2 / g, purchased from Shandong Boken Silicon Materials Co., Ltd., model BK94.

[0162] The dispersion medium is methyl oleate. The defoamer is a polyether defoamer, specifically a GPE type polyether defoamer; the antifreeze is ethylene glycol; and the preservative is sodium benzoate.

[0163] A second aspect of the present invention provides a method for preparing the suspension emulsion:

[0164] S01 mixes tert-butylamine, stabilizer, nonionic surfactant, Croda Metasoerse-550S, Dow Duramax D-518 and water by grinding to obtain tert-butylamine suspension.

[0165] Zirconium beads were used as the grinding media, the grinding time was 2 hours, and the rotation speed was 1300 rpm.

[0166] S02 is prepared by grinding and stirring 2,4-dip isooctyl ester, acetochlor, dispersion medium and remaining emulsifier to obtain emulsifiable oil;

[0167] S03 involves mixing emulsifiable concentrate and suspending agent under high shear, then adding the remaining raw materials, and finally preparing the suspension emulsion through modulation and mixing.

[0168] The shear emulsification time was 30 minutes and the rotation speed was 2500 rpm.

[0169] Performance testing

[0170] 1. Suspension rate: The suspension rate was determined in accordance with GB / T14825-2006 "Method for Determination of Suspension Rate of Pesticides"; the lowest suspension rate of the three active ingredients was taken as the suspension rate value of the entire system.

[0171] 2. The determination of thermal storage stability shall be carried out in accordance with GB / T19136-2003 Method for Determination of Thermal Storage Stability of Pesticides; the determination of low temperature stability shall be carried out in accordance with GB / T19137-2003 Method for Determination of Low Temperature Stability of Pesticides.

[0172] 3. Dispersion stability test: Add 0.5 mL of the suspension to hard water and observe the dispersion of the suspension in the water.

[0173] Superior grade: Automatically dispersed, with no visible particles / oily substances precipitated;

[0174] Good grade: Can disperse automatically, with a small amount of particles / oil precipitated;

[0175] Inferior grade: Cannot disperse automatically, with obvious particle / oily substances precipitated.

[0176] Table 1 Performance Test Results

[0177]

[0178]

[0179] "-" indicates that the suspension rate does not meet the standard and is low.

[0180] In this invention, the suspension emulsion undergoes grinding and modulation processes during preparation. However, due to the presence of multiple phases in the system, such as phase transfer between the emulsifier and dispersant, the amount of emulsifier or dispersant in the other phase may be insufficient. This invention uses vitamin E polyethylene glycol succinate as a stabilizer, which can achieve a finer particle size during grinding, resulting in a higher overall suspension rate. However, smaller particle sizes are prone to aggregation, leading to a decrease in suspension rate. Furthermore, 2,4-D isooctyl ester requires acidic conditions for optimal efficacy, while terbutaline is relatively stable in neutral, weakly acidic, and weakly alkaline media, but easily hydrolyzes in acidic or alkaline media. To address this, the inventors discovered that using an amphoteric emulsifier can improve these conditions, and adding modified silica can simultaneously improve both issues. The results show that using vitamin E polyethylene glycol succinate as a stabilizer, combined with modified silica, results in high overall system stability and a high suspension rate.

[0181] Field trials and tests:

[0182] Field efficacy trial of 83% 2,4-D isooctyl ester·terbutaline·acetochlor suspension emulsion for controlling annual weeds in spring maize fields.

[0183] Experimental crop: Spring maize

[0184] Target plants for control: annual weeds

[0185] Test period: (May 26, 2022 - October 10, 2022)

[0186] Table 2 Test reagents:

[0187]

[0188]

[0189] Application method and water volume: The test agent was applied to the soil after spring corn sowing but before the seedlings emerged, when the weeds had sprouted but not yet emerged from the soil. On a sunny day with a wind force of less than level 3, the agent was diluted with 750L of water per hectare for soil spraying.

[0190] Test target situation

[0191] Echinochloa crus-galli (L) Beauv, Eriochloa villosa (Thunb.) Kunth, Chenopodium album L, Amaranthus retroflexus L, Polygonum bungeanum Turcz., Acalypha australis L., Commelina communis L., Rorippa globosa (Leyss) Bess, Humulus scandens (Lour) Merr., Cirsium arvense var. integrifolium, Kochia scoparia (L) Schrad., Ambrosia trifida L., Xanthium sibiricum Patrin., Abutilontheophrasti Medi, Solanum nigrum L., Amethystea caerulea L., etc.

[0192] Crop: Spring maize; Variety: Jidan 63; Application time: 3 days after maize sowing.

[0193] The black soil has an organic matter content of 2.3% and a neutral pH value.

[0194] Weather conditions on the day of application: 5-11 am on May 26, 2022, light rain, northerly wind at level 2, cloudy, 11-14℃, the weather conditions are conducive to the efficacy of the pesticide.

[0195] Table 3. Experimental Results:

[0196]

[0197]

[0198] Conclusion: The appropriate dosage of 83% 2,4-D isooctyl ester·terbutaline·acetochlor suspension emulsion, applied as a soil spray after sowing and before emergence of spring maize, is 1120.5 g / hm² for fields with low weed populations in the previous year. 2 (Dosage of active ingredient): For fields with a high weed population, the dosage can be appropriately increased to 1369.5 g / hm². 2 When diluted with 750L of water and sprayed on the soil, it can effectively control weeds such as barnyard grass, crabgrass, velvetleaf, lambsquarters, and black nightshade. It also has a good control effect on other broadleaf weeds (hope, thistle, knotweed, etc.) and is safe for corn.

[0199] Survey Methods

[0200] Using the absolute value survey method, a 0.25m artificially constructed [structure / method] was employed. 2 Using iron frames, three points were surveyed in each community, with points randomly selected. The types and quantities of weeds whose heart leaves had not died were recorded.

[0201] Methods for calculating drug efficacy

[0202] The number of plants or fresh weight of each treatment and the control efficacy were calculated according to formula (1):

[0203]

[0204] In the formula:

[0205] E—Prevention and control effect, expressed as a percentage (%)

[0206] PT—Number or fresh weight of remaining weeds in the treatment area, expressed in plants or grams (g);

[0207] CK—Number of weed plants or fresh weight in the blank control area, in units of plants or grams (g).

[0208] The results were analyzed using biological statistical methods (DMRT method).

[0209] Direct impact on crops

[0210] Visually observe the biological traits of corn leaves, such as leaf color, growth, tasseling, and plant height, at 1, 5, 10, 20, 30, and 40 days after application. If any pesticide damage is found, record the symptoms.

[0211] The specific methods for classifying pesticide damage are as follows:

[0212] Level 1: The crop is growing normally and shows no signs of damage;

[0213] Level 2: Slight pesticide damage to crops, with damage less than 10%;

[0214] Level 3: Moderate pesticide damage to crops, which can recover later and will not affect yield;

[0215] Level 4: Severe pesticide damage to crops, difficult to recover from, resulting in reduced yield.

[0216] Level 5: Severe pesticide damage to crops, irreversible, resulting in significant yield reduction or complete crop failure.

[0217] Impact on crop growth

[0218] After application of the pesticide, the effects of each treatment on corn seedling emergence, leaf color, growth, jointing, tasseling, and yield were observed.

[0219] In autumn, the fresh weight of grains in the middle row of each plot was measured, converted into yield per hectare, and the yield increase rate was calculated.

[0220] The corn yield increase rate is calculated according to formula (2):

[0221]

[0222] In the formula:

[0223] Y —Production increase rate, in percentage (%);

[0224] Y—Target herbicide treatment yield, in kilograms (kg);

[0225] Y0—Yield of the control area, in kilograms (kg).

[0226] The results were analyzed using biological statistical methods (DMRT method).

[0227] Table 4. Investigation on the effects of 83% 2,4-D isooctyl ester·terbutaline·acetochlor suspension emulsion on crop yield.

[0228]

[0229]

[0230] Prevention and control effect: The survey data were statistically analyzed using the DPS data processing system software. The specific results are shown in Tables 5 and 6.

[0231] Table 5. Weed control efficacy (%) of 83% 2,4-D isooctyl ester·terbutaline·acetochlor suspension emulsion in spring maize fields—20 days after application.

[0232]

[0233] Note: 1. Others include broadleaf weeds such as hops, thistle, and knotweed; 2. The significant difference in the table is the 5% significance of the weed count, and the same applies to the following tables.

[0234] Table 6. Control efficacy (%) of 83% 2,4-D isooctyl ester·terbutaline·acetochlor suspension emulsion against annual weeds in spring maize fields — 40 days after application

[0235]

[0236]

[0237] It was also found that using other crops was not as effective as using corn.

[0238] Finally, it should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention, and not to limit them; although the present invention has been described in detail with reference to the foregoing embodiments, those skilled in the art should understand that modifications can still be made to the technical solutions described in the foregoing embodiments, or equivalent substitutions can be made to some or all of the technical features; and these modifications or substitutions do not cause the essence of the corresponding technical solutions to deviate from the scope of the technical solutions of the embodiments of the present invention.

Claims

1. A ternary herbicidal suspoemulsion concentrate comprising 2,4-D isooctyl, terbuthylazine and acetochlor, characterized in that, Its preparation components include: 2,4-D isooctyl ester 10%; Terbuthylazine 20%; Acetochlor 53%; Dispersant 1.5%; Emulsifier 2%; Stabilizer 0.7%; Dispersion medium 1%; Other adjuvants 1%; Water balance; The dispersant is Croda Metasoerse-550S, Dow Duramax D-518, and Akzo Agrlian-700, with a mass ratio of 8:1:3; The emulsifiers are dodecyl betaine, Atlox 4913 and Termu1 1284, in a mass ratio of 2:1:1; The stabilizer comprises vitamin E polyethylene glycol succinate and modified silica in a mass ratio of 3:1; The modified silica is prepared as follows: 50 parts by weight of silica, 2 parts by weight of sodium metabisulfite, 3 parts by weight of sodium acrylate and 200 parts by weight of water are ultrasonically mixed, the mixture is dried at a constant temperature, and the dried product is irradiated with an electron beam of 8 keV and a dose of 30 kGy for 10 min. The particle size of the silica is 0.1-0.15 μm, and the specific surface area is 15-27 m 2 / g, purchased from Shandong BoKen Silicon Material Co., Ltd., model BK94; The dispersion medium is methyl oleate; the defoamer is BYK-080 from BYK Corporation; the antifreeze is ethylene glycol; and the preservative is sodium benzoate. The method for preparing the suspension emulsion: S01 Terbutaline suspension is obtained by grinding together terbutaline, stabilizer, nonionic surfactant, Croda Metasoerse-550S, Dow Duramax D-518 and water. Zirconium beads were used as the grinding media, the grinding time was 2 hours, and the rotation speed was 1300 rpm. S02 is prepared by grinding and stirring 2,4-dip isooctyl ester, acetochlor, dispersion medium and remaining emulsifier to obtain emulsifiable oil; S03 involves mixing emulsifiable concentrate and suspending agent under high shear, then adding the remaining raw materials, and finally preparing the suspension emulsion through modulation and mixing. The shear emulsification time was 30 min, and the rotation speed was 2500 rpm.

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