WO2023040894A1 - Stable agrochemical composition comprising two solid active components and one liquid active component and its preparation process - Google Patents

Stable agrochemical composition comprising two solid active components and one liquid active component and its preparation process Download PDF

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Publication number
WO2023040894A1
WO2023040894A1 PCT/CN2022/118727 CN2022118727W WO2023040894A1 WO 2023040894 A1 WO2023040894 A1 WO 2023040894A1 CN 2022118727 W CN2022118727 W CN 2022118727W WO 2023040894 A1 WO2023040894 A1 WO 2023040894A1
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Prior art keywords
composition
active component
total amount
percent
weight based
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PCT/CN2022/118727
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French (fr)
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Ying Xu
Xiaofeng Xu
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Adama Agan Ltd.
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Priority to JP2024516960A priority Critical patent/JP2024531780A/en
Priority to CN202280061845.4A priority patent/CN117940016A/en
Priority to IL311456A priority patent/IL311456A/en
Publication of WO2023040894A1 publication Critical patent/WO2023040894A1/en
Priority to CONC2024/0004249A priority patent/CO2024004249A2/en

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    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/18—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof
    • A01N37/22—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group —CO—N<, e.g. carboxylic acid amides or imides; Thio analogues thereof the nitrogen atom being directly attached to an aromatic ring system, e.g. anilides
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
    • A01N43/54—1,3-Diazines; Hydrogenated 1,3-diazines
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system

Definitions

  • the present disclosure relates to a stable agrochemical composition comprising two solid active components and one liquid active component and its preparation process. More specifically, the present disclosure relates to a stable agrochemical composition e.g., a suspo-emulsion (SE) comprising Penoxsulam, Pretilachlor, and a further solid active component, especially a solid safener, e.g., Fenclorim, and its preparation process.
  • SE suspo-emulsion
  • the present disclosure relates to a stable agrochemical composition e.g., a suspo-emulsion (SE) comprising Pretilachlor, Fenclorim, and a further solid active component selected from the group consisted of Penoxsulam, Pyrazosulfuron-ethyl, Bensulfuron methyl, Quinclorac, Oxyfluorfen, Oxadiazon, cyhalofop-butyl, Pyriminobac-methyl, Clomazone (Dimethazon) , Pyribenzoxim, Oxadiargyl, and Simetryn, and its preparation process.
  • SE suspo-emulsion
  • Two or more agrochemical active components with different mechanisms of action are generally combined to provide an expanded range of applications, such as weed spectrum, or to provide a synergy.
  • a safener is also be added to the agrochemical composition as an active component to protect the crops.
  • Fenclorim is generally used along with Pretilachlor in a ratio of 1: 2 to 1: 5 (e.g., 1: 3 or 1: 4) .
  • a agrochemical composition (specifically in this case a herbicidal composition) comprising three active components has to be formulated in which two active components are solid and one active component is liquid.
  • a suspo-emulsion SE is the usual choice, especially when at least one of the two solid active components is insoluble in water or the liquid active component.
  • an agrochemical composition comprising two solid active components and one liquid active component, e.g., a stable SE comprising two solid active components and on e liquid active component can be successfully prepared, e.g., from combining EC with SC by carefully selecting the active components in each of EC or SC, especially when the content of the oil phase is very high, e.g., at least 30 percent by weight based on the total amount of the composition, preferably at least 40 percent by weight based on the total amount of the composition, preferably at least 50 percent by weight based on the total amount of the composition, preferably at least 60 percent by weight based on the total amount of the composition.
  • the present disclosure provides a stable agrochemical composition comprising two solid active components and one liquid active component and its preparation process. More specifically, the present disclosure provides a stable agrochemical composition e.g., a suspo-emulsion comprising Penoxsulam, Pretilachlor, and a further solid active component, especially a solid safener, e.g., Fenclorim, and its preparation process.
  • a stable agrochemical composition e.g., a suspo-emulsion comprising Penoxsulam, Pretilachlor, and a further solid active component, especially a solid safener, e.g., Fenclorim, and its preparation process.
  • the present disclosure relates to a stable agrochemical composition e.g., a suspo-emulsion (SE) comprising Pretilachlor, Fenclorim, and a further solid active component selected from the group consisted of Penoxsulam, Pyrazosulfuron-ethyl, Bensulfuron methyl, Quinclorac, Oxyfluorfen, Oxadiazon, cyhalofop-butyl, Pyriminobac-methyl, Clomazone (Dimethazon) , Pyribenzoxim, Oxadiargyl, and Simetryn, and its preparation process.
  • SE suspo-emulsion
  • the present disclosure provides:
  • a stable agrochemical composition comprising:
  • a first active component which is solid at room temperature and insoluble in water at room temperature
  • the first active component is insoluble in the third active component at room temperature
  • the second solid active component has a solubility in the third liquid active component of from 1 to 33 g/100g at room temperature.
  • composition of any one of embodiments 1 to 11, wherein the composition further comprises an organic solvent with a content of 1 to 40 percent by weight based on the total amount of the composition.
  • composition of any one of embodiments 1 to 12, wherein the composition further comprises one or more additives selected from the group consisting of thickener, dispersant, wetting agent, emulsifier, antifreeze, antifoam, and bactericide.
  • a process for preparing the stable agrochemical composition of embodiments 1 to 19, comprising the steps of:
  • step a) comprises mixing the first active component, a first portion of water, and other optional additives to form a homogeneous suspension.
  • step a) further comprises milling the suspension until the mean particle size d90 is ⁇ 7 ⁇ m.
  • step b) comprises mixing the second and third active components, an optional organic solvent and other optional additives to form a clear liquid.
  • step c) the mixing of the SC with EC is conducted under a shear and the mean particle size d90 of the composition is ⁇ 7 ⁇ m based on all particles of all types.
  • step c) comprises c1) mixing the SC with a part of or all of the thickener to form a homogeneous suspension, and c2) mixing the suspension obtained in c1) with the EC.
  • Astable agrochemical composition prepared by a process comprise the steps of
  • the first active component is solid at room temperature and insoluble in water at room temperature
  • the second active component is solid at room temperature
  • the third active component is liquid at room temperature
  • the first active component is insoluble in the third active component at room temperature, and the second active component has a solubility in the third active component of from 1 to 33 g/100g at the room temperature.
  • step a) comprises mixing the first active component, a first portion of water, and other optional additives to form a homogeneous suspension.
  • step a) further comprises milling the suspension until the mean particle size d90 is ⁇ 7 ⁇ m.
  • step b) comprises mixing the second and third active components, an optional organic solvent and other optional additives to form a clear liquid.
  • composition comprises a thickener
  • step c) comprises c1) mixing the SC with the thickener to form a homogeneous suspension, and c2) mixing the suspension obtained in c1) with the EC.
  • composition further comprises an organic solvent with a content of 1 to 40 percent by weight based on the total amount of the composition.
  • composition further comprises one or more additives selected from the group consisting of thickener, dispersant, wetting agent, emulsifier, antifreeze, antifoam, and bactericide.
  • Fig. 1 shows a microscope photograph which was taken on the SE1 obtained in Example 1.
  • Pretilachlor is the common name for 2-chloro-N- (2, 6-diethylphenyl) -N- (2-propoxyethyl) acetamide with a structure of Its herbicidal activity is described in The Pesticide Manual, Fifteenth Edition, 2009. Pretilachlor is a liquid at room temperature with a melting point less of -20 °C.
  • Fenclorim is the common name for 4, 6-dichloro-2-phenylpyrimidine with a structure of Fenclorim is a solid at room temperature with a melting point of 96.9 °C and has a solubility in water of 2.5 mg/L at room temperature.
  • composition refers, but is not limited to, a combination in any physical form, e.g., blend, solution, alloy, or the like.
  • active component refers, but is not limited to, any compounds which have an agricultural activity, for example, insecticidal activity, fungicidal activity, bactericidal activity, herbicidal activity, safening activity, protecting activity, etc. Therefore, the term “active component” comprises, but is not limited to, insecticide compound, fungicide compound, bactericide compound, herbicide compound, safener compound, acaricide compound, nematicide compound, bird repellent compound, and plant nutrient compound, etc.
  • herbicidal active component refers, but is not limited to, any compounds which have herbicidal activity, safening activity, or protecting activity, etc. Therefore, the term “herbicidal active component” comprises herbicide compound, safener compound, etc.
  • sucspo-emulsion means a mixture of water-insoluble active ingredients dispersed in an aqueous solution, where one (or more) of the active ingredients is in suspension form and one (or more) of the active ingredients is in emulsion form.
  • the formulation is intended for dilution into water prior to spray application. Mixtures of active ingredients are often used to provide a broader spectrum of control. Formulating the active ingredients together eliminates the need for tank mixing (which can lead to incompatibilities) .
  • suspo-emulsions are easy to handle and measure, dust free, non-flammable and offer good miscibility with water (see, “Manual on development and use of FAO and WHO specifications for pesticides” ) .
  • stable when used in connection with a composition means that the composition should satisfy the following stability requirements set forth for suspo-emulsion (SE) as recited in NY/T 2989-2016 (Guidelines on developing the specifications of pesticides for registration) : appearance, wet sieve test, dispersion stability, low temperature stability (only for appearance, wet sieve test, and dispersion stability) , and heat storage stability (only for appearance, wet sieve test, and dispersion stability) .
  • SE suspo-emulsion
  • the term "insoluble” means the solubility of a material (e.g., an active component) in a specified material (for example, water, the third active component, etc., ) is less than 0.1g/1000g at a specified temperature.
  • an "ultra-low naphthalene solvent” is a solvent with a naphthalene concentration of less than 0.1 wt %.
  • a "low naphthalene solvent” is a solvent with a naphthalene concentration of less than 1 wt %.
  • additive is defined as any substance that is not an active component but is added to the composition such as sticking agents, surfactants, synergists, buffers, acidifiers, defoaming agents, thickeners, etc.
  • safety refers to an agent that increases the tolerance of plants to herbicides without significantly affecting the effectiveness of the herbicide.
  • thickener refers to an agent that increases the viscosity of a liquid composition without substantially changing other properties of the composition.
  • agriculturally acceptable carrier means carriers of which are known and accepted in the art for the formation of formulations for agricultural or horticultural use.
  • surfactant refers to an agriculturally acceptable material which imparts emulsifiability, stability, spreading, wetting, dispersibility or other surface-modifying properties.
  • mean Particle size d90 means particle size distribution D90, which represents the particle diameter corresponding to 90%cumulative (from 0 to 100%) undersize particle size distribution.
  • room temperature means 23 ⁇ 2°C.
  • the present disclosure provides a stable agrochemical composition, comprising:
  • a first active component which is solid at room temperature and insoluble in water at room temperature
  • the first active component is insoluble in the third active component at room temperature, and the second active component has a solubility in the third active component of from 1 to 33 g/100g at room temperature.
  • the first active component is solid at room temperature and insoluble in water at room temperature.
  • the solubility of the first active component in water at room temperature is less than 0.1g/L, preferably less than 0.08g/L.
  • the first active component is slightly soluble to insoluble in the third active component at room temperature.
  • the solubility of the first active component in the third active component at room temperature is less than 1g/100g, preferably less than 0.2g/100g.
  • the second active component is solid at room temperature and the second active component has a solubility in the third active component of from 1 to 33 g/100g at room temperature.
  • the solubility of the second active component in the third active component at room temperature may be 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 12.1, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, or 33 g/100g, or any ranges formed by selecting any two solubilities mentioned above as the two limits, for example, the solubility of the second active component in the third active component at room temperature may be 2 to 30 g/100g, or 5 to 25 g/100g.
  • the second active component has a solubility in the third active component of from 2 to 28 g/100g, 5 to 20 g/100g, 7 to 18 g/100g, 8 to 15 g/100g, 9 to 14 g, or 11 to 13 /100g at room temperature.
  • the second active component has a solubility in the third active component of 12.1 g/100g at room temperature.
  • the solubility of the second solid active component in the third liquid active component at room temperature is important to understand why in some cases a stable agrochemical composition comprising the three active components, especially a stable SE comprising the three active components can not be formulated.
  • a stable agrochemical composition comprising the three active components, especially a stable SE comprising the three active components may not be formulated at all or may not be obtained through the conventional route mentioned before, in some cases also depending on the amounts of the second active component and the third active component.
  • solubility of the second solid active component in the third liquid active component is high enough, and the amounts of the second active component and the third active component are such that the second active component is dissolved totally in the third active component no matter at room temperature or 54°C, a stable SE will be easily formulated through the conventional route mentioned before.
  • solubility of the second solid active component in the third liquid active component is small enough, and also considering the amounts of the second active component and the third active component, those skilled in the art will not even think of formulating a SE through the conventional route mentioned before.
  • the third active component is liquid at room temperature.
  • the first active component, the second active component and the third active component may be independently selected from the group consisting of insecticide compounds, fungicide compounds, bactericide compounds, herbicide compounds, safener compounds, acaricide compounds, nematicide compounds, bird repellent compounds, and plant nutrient compounds.
  • all the first active component, the second active component and the third active component are selected from the herbicidal active components.
  • both the first and third active components are herbicide compounds, and the second active component is a safener.
  • the first active component is a triazolopyrimidine sulfonamide herbicide compound
  • the third liquid active component is an acetanilide herbicide compound
  • the second active component is a safener compound e.g., a phenylpyrimidine safener compound.
  • the first active component is a herbicidal compound which is neither Pretilachlor nor a safener compound
  • the third liquid active component is Pretilachlor
  • the second active component is Fenclorim.
  • the first active component is any one selected from the group consisted of Penoxsulam, Pyrazosulfuron-ethyl, Bensulfuron methyl, Quinclorac, Oxyfluorfen, Oxadiazon, cyhalofop-butyl, Pyriminobac-methyl, Clomazone (Dimethazon) , Pyribenzoxim, Oxadiargyl, and Simetryn, the third liquid active component is Pretilachlor, and the second active component is Fenclorim. Most preferably, the first active component is Penoxsulam, the third liquid active component is Pretilachlor, and the second active component is Fenclorim.
  • the content of the first active component may be 0.02 to 40 percent by weight based on the total amount of the composition.
  • the content of the first active component may be 0.02, 0.03, 0.04, 0.05, 0.06, 0.07, 0.08, 0.09, 0.1, 0.11, 0.12, 0.13, 0.14, 0.15, 0.16, 0.17, 0.18, 0.19, 0.2, 0.25, 0.3, 0.35, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, 1.1, 1.2, 1.3, 1.34, 1.4, 1.5, 1.6, 1.7, 1.8, 1.9, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40 percent by weight based on the total amount of the composition, or any ranges formed by selecting any two contents mentioned above as the two limits, for example
  • the content of the first active component may be 0.04 to 20 percent by weight based on the total amount of the composition. More preferably, the content of the first active component may be 0.08 to 10 percent by weight based on the total amount of the composition. More preferably, the content of the first active component may be 0.1 to 8 percent by weight based on the total amount of the composition. For example, the content of the first active component may be 0.1, 1.2 or 8 percent by weight based on the total amount of the composition.
  • the content of the first active component may be 0.1 to 10 percent by weight based on the total amount of the composition.
  • the content of the first active component may be 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, 1.1, 1.2, 1.3, 1.34, 1.4, 1.5, 1.6, 1.7, 1.8, 1.9, 2, 3, 4, 5, 6, 7, 8, 9, or 10 percent by weight based on the total amount of the composition, or any ranges formed by selecting any two contents mentioned above as the two limits, for example, the content of the first active component may be 0.3 to 8, or 0.5 to 5 percent by weight based on the total amount of the composition.
  • the content of the first active component may be 0.8 to 3 percent by weight based on the total amount of the composition. More preferably, the content of the first active component may be 0.9 to 2 percent by weight based on the total amount of the composition. More preferably, the content of the first active component may be 1 to 1.5 percent by weight based on the total amount of the composition. For example, the content of the first active component may be 1.2 or 1.3 percent by weight based on the total amount of the composition.
  • the content of the second active component may be 1 to 60 percent by weight based on the total amount of the composition.
  • the content of the second active component may be 1, 2, 3, 4, 4.9, 5, 6, 7, 8, 9, 10, 10.2, 10.7, 10.9, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, 50, 51, 52, 53, 54, 55, 56, 57, 58, 59, or 60 percent by weight based on the total amount of the composition, or any ranges formed by selecting any two contents mentioned above as the two limits, for example, the content of the second active component may be 3 to 50, or 5 to 10 percent by weight based on the total amount of the composition.
  • the content of the second active component may be 2 to 30 percent by weight based on the total amount of the composition.
  • the content of the second active component may be 4 to 15 percent by weight based on the total amount of the composition.
  • the content of the second active component may be 4.9 to 11 percent by weight based on the total amount of the composition.
  • the content of the second active component may be 4.9, 10.2 or 10.9 percent by weight based on the total amount of the composition.
  • the content of the second active component may be 1 to 40 percent by weight based on the total amount of the composition.
  • the content of the second active component may be 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 10.2, 10.7, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, or 40 percent by weight based on the total amount of the composition, or any ranges formed by selecting any two contents mentioned above as the two limits, for example, the content of the second active component may be 2 to 30, or 5 to 20 percent by weight based on the total amount of the composition.
  • the content of the second active component may be 8 to 15 percent by weight based on the total amount of the composition. More preferably, the content of the second active component may be 9 to 12 percent by weight based on the total amount of the composition. For example, the content of the second active component may be 10.2 or 10.7 percent by weight based on the total amount of the composition.
  • the content of the third active component may be 3 to 90 percent by weight based on the total amount of the composition.
  • the content of the third active component may be 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 30.8, 31, 31.8, 32, 32.8, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, 50, 51, 52, 53, 54, 55, 56, 57, 58, 59, 60, 61, 62, 63, 64, 65, 66, 67, 68, 69, 70, 71, 72, 73, 74, 75, 76, 77, 78, 79, 80, 81, 82, 83, 84, 85, 86, 87, 88, 89, or 90 percent by weight based on the total amount of the composition, or any range
  • the content of the third active component may be 6 to 80 percent by weight based on the total amount of the composition. More preferably, the content of the third active component may be 12 to 40 percent by weight based on the total amount of the composition. More preferably, the content of the third active component may be 15 to 33 percent by weight based on the total amount of the composition. For example, the content of the third active component may be 30.8, 31.8 or 32.8 percent by weight based on the total amount of the composition.
  • the content of the third active component may be 3 to 80 percent by weight based on the total amount of the composition.
  • the content of the third active component may be 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 30.8, 31, 31.8, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, 50, 51, 52, 53, 54, 55, 56, 57, 58, 59, 60, 61, 62, 63, 64, 65, 66, 67, 68, 69, 70, 71, 72, 73, 74, 75, 76, 77, 78, 79, or 80 percent by weight based on the total amount of the composition, or any ranges formed by selecting any two contents mentioned above as the two limits, for example, the content of the third active component may be 6 to 70, or
  • the content of the third active component may be 20 to 40 percent by weight based on the total amount of the composition. More preferably, the content of the third active component may be 25 to 35 percent by weight based on the total amount of the composition. More preferably, the content of the third active component may be 29 to 35 percent by weight based on the total amount of the composition. For example, the content of the third active component may be 30.8, 31.8 or 32.8 percent by weight based on the total amount of the composition.
  • the weight ratio of the second active component to the third active component may be 1: (1 to 6) .
  • the weight ratio of the second active component to the third active component may be 1: (1.5 to 5) .
  • the weight ratio of the second active component to the third active component may be 1: (2 to 4) .
  • the weight ratio of the second active component to the third active component is 1: 3.
  • the composition also includes water.
  • Water is used as a carrier.
  • the content of the water in the composition may be 5 to 90 percent by weight based on the total amount of the composition.
  • the content of the third active component may be 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, 50, 51, 52, 53, 54, 55, 56, 57, 58, 59, 60, 61, 62, 63, 64, 65, 66, 67, 68, 69, 70, 71, 72, 73, 74, 75, 76, 77, 78, 79, 80, 81, 82, 83, 84, 85, 86, 87, 88, 89 or 90 percent by weight based on the total amount of the composition, or any ranges
  • the content of the water in the composition may be 10 to 75 percent by weight based on the total amount of the composition.
  • the content of the water in the composition may be 20 to 50 percent by weight based on the total amount of the composition.
  • the content of the water in the composition may be 25 to 45 percent by weight based on the total amount of the composition.
  • the content of the water in the composition may be 30 to 40 percent by weight based on the total amount of the composition.
  • the content of the water in the composition may be 35 percent by weight based on the total amount of the composition.
  • the composition may further comprise an organic solvent.
  • the organic solvent should be selected based at least on: (1) the specific second and third active components with the intention of preparing successfully for example an EC of the specific second and third active components; (2) that solubility of the organic solvent in water at room temperature should not be too high, for example that solubility of the organic solvent in water at room temperature should be less than 0.1 g/1000g.
  • the organic solvent may be selected from the group consisting of aromatic hydrocarbons (for example toluene, xylene, ethylbenzene, isopropylbenzene, tert-butylbenzene, naphthalenes, mono-or polyalkyl-substituted naphthalenes) , paraffins, petroleum, diesel, mineral oil, fatty acid amides, fatty acids, tall oil fatty acids, alkyl esters of fatty acids, modified vegetable oils, and any combination thereof.
  • the organic solvent may be selected from the group consisting of aromatic hydrocarbons, paraffins, petroleum, diesel, mineral oil, fatty acids, tall oil fatty acids, and any combination thereof.
  • the organic solvent may be aromatic hydrocarbons, especially in consideration of environmental protection, a low naphthalene aromatic hydrocarbons solvent, for example, aromatic solvent S-150ND or S-100A available from Jiangsu Hualun Chemical Industry Co., Ltd., Solvesso TM grades from ExxonMobil Chemical (for example Solvesso TM 100 (CAS No. 64742- 95-6) , Solvesso TM 150 (CAS No. 64742-94-5) , and Solvesso TM 200 (CAS No. 64742-94-5) ) , and Caromax TM 28 LN from Petrochem Carless.
  • aromatic solvent S-150ND or S-100A available from Jiangsu Hualun Chemical Industry Co., Ltd.
  • Solvesso TM grades from ExxonMobil Chemical (for example Solvesso TM 100 (CAS No. 64742- 95-6) , Solvesso TM 150 (CAS No. 64742-94-5) , and Solvesso TM 200 (CAS No
  • the organic solvent When the organic solvent is present, its content in the composition should be enough to (1) dissolve the second active material which is not fully disclosed in the third active material and (2) prepare successfully for example an EC of the specific second and third active components. In one embodiment, when the organic solvent is present, its content in the composition may be 1 to 40 percent by weight based on the total amount of the composition.
  • the content of the solvent may be 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 11.1, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, or 40 percent by weight based on the total amount of the composition, or any ranges formed by selecting any two contents mentioned above as the two limits, for example, the content of the solvent may be 2 to 30, or 5 to 20 percent by weight based on the total amount of the composition.
  • the content of the solvent may be 9 to 16 percent by weight based on the total amount of the composition. More preferably, the content of the solvent may be 10 to 12 percent by weight based on the total amount of the composition.
  • the content of the solvent may be 11 or 11.1 percent by weight based on the total amount of the composition.
  • the composition may optionally comprise one or more additives selected from the group consisting of thickener, dispersant, wetting agent, emulsifier, antifreeze, antifoam, and bactericide.
  • additives selected from the group consisting of thickener, dispersant, wetting agent, emulsifier, antifreeze, antifoam, and bactericide.
  • the content of all the additives in the composition may be 3 to 70 percent by weight based on the total amount of the composition.
  • the content of all the additives may be 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 21.1, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, 50, 51, 52, 53, 54, 55, 56, 57, 58, 59, 60, 61, 62, 63, 64, 65, 66, 67, 68, 69, or 70 percent by weight based on the total amount of the composition, or any ranges formed by selecting any two contents mentioned above as the two limits, for example, the content of all the additives may be 3 to 60, or 6 to 50 percent by weight based on the total amount of the composition.
  • the content of all the additives may be 10 to 42 percent by weight based on the total amount of the composition. More preferably, the content of all the additives may be 15 to 33 percent by weight based on the total amount of the composition. More preferably, the content of all the additives may be 18 to 28 percent by weight based on the total amount of the composition. More preferably, the content of all the additives may be 20 to 23 percent by weight based on the total amount of the composition. For example, the content of all the additives may be 21.1 percent by weight based on the total amount of the composition.
  • the thickener any thickeners that are generally used in the agrochemical field, especially herbicidal field to increase the viscosity of the composition may be used.
  • the thickener may be inorganic clays, organoclays, fumed and precipitated silica, organo modified bentonite, microcrystalline cellulose, xanthan gum, polyamides, hydrogenated caster oils, EO/PO block co-polymers, etc.
  • the thickener is xanthan gum.
  • Fumed and precipitated silica may be hydrophobic and hydrophilic silica and any combination thereof. Examples of fumed silica may include but are not limited to A200, R 202, R 972 and R 805 (all available from Evonik) .
  • Examples of precipitated silica may include but are not limited to 22S (available from Evonik) , D17 (available from Evonik) and 38 (available from Rhodia Operations, a member of the Solvay Group) .
  • An example of organo modified bentonite is SD-1 (available from Elementis Specialties) .
  • An example of inorganic clays is 40 (available from BASF) .
  • An example of xanthan gum is AG RH 23 (available from Ametech srl) .
  • the content of the thickener in the composition may be selected based on the nature of the thickener, the required viscosity of the composition and the cost.
  • the content of the thickener in the composition may be 0.005 to 0.5 percent by weight based on the total amount of the composition.
  • the content of the thickener in the composition may be 0.01 to 0.1 percent by weight based on the total amount of the composition.
  • the content of the thickener in the composition may be 0.02 to 0.06 percent by weight based on the total amount of the composition.
  • the content of the thickener in the composition may be 0.03 to 0.05 percent by weight based on the total amount of the composition.
  • the content of the thickener in the composition may be 0.04 percent by weight based on the total amount of the composition.
  • any dispersants that are generally used in the agrochemical field, especially herbicidal field to prevent the aggregation of solid particles in the solid-liquid dispersion system and keep them uniformly dispersed in the liquid phase for a long time may be used.
  • the dispersant may be alkylarylsulfonate salts, such as calcium dodecylbenzenesulfonate; alkylphenol-alkylene oxide addition products, such as nonylphenol-C 18 ethoxylate; soaps, such as sodium stearate; alkylnaphthalene-sulfonate salts and condensates, such as sodium dibutyl-naphthalenesulfonate; dialkyl esters of sulfosuccinate salts, such as sodium di (2-ethylhexyl) sulfosuccinate; quaternary amines, such as lauryl trimethylammonium chloride; alkyl amines, such as tallow amine or derivatives thereof; block copolymers of ethylene oxide and propylene oxide; acrylic copolymers grafted with polyethylene oxide side chains; amphoteric polymers; comb polymers such as polyvinylpyrrolidinones or polyacryl
  • the dispersant is a combination of two different dispersants, for example, a combination of block copolymers of ethylene oxide and propylene oxide with comb polymers such as polyvinylpyrrolidinones or polyacrylates or with a polymeric dispersant (such as Geropon MAI available from Solvay or Rhodia) . More preferably, the dispersant is a combination of block copolymers of ethylene oxide and propylene oxide (such as, ETHYLAN TM NS-500LQ available from AKZO NOBEL SURFACE CHEMISTRY LLC.
  • TERMUL 5500 available from HUNTSMAN INTERNATIONAL LLC
  • comb polymers such as polyvinylpyrrolidinones or polyacrylates, e.g., Atlox 4913-LQ- (MV) available from Croda Europe Limited, or Agrilan 755 available from AKZO NOBEL SURFACE CHEMISTRY LLC
  • block copolymers of ethylene oxide and propylene oxide such as, ETHYLAN TM NS-500LQ available from AzokNobel
  • a polymeric dispersant such as Geropon MAI available from Solvay
  • the dispersant is a combination of block copolymers of ethylene oxide and propylene oxide (such as, TERMUL 5500 available from HUNTSMAN INTERNATIONAL LLC) with a polyacrylate comb polymer (such as Agrilan 755 available from AKZO NOBEL SURFACE CHEMISTRY LLC) .
  • the dispersant is a combination of block copolymers of ethylene oxide and propylene oxide (such as, ETHYLAN TM NS-500LQ available from AzokNobel) with a polymeric dispersant (such as Geropon MAI available from Solvay) .
  • the content of all the dispersants in the composition may be selected based on the nature of the dispersant, the required properties of the composition and cost.
  • the content of all the dispersants in the composition may be 0.2 to 20 percent by weight based on the total amount of the composition.
  • the content of all the dispersants in the composition may be 0.1 to 12 percent by weight based on the total amount of the composition.
  • the content of all the dispersants in the composition may be 0.2 to 6 percent by weight based on the total amount of the composition.
  • the content of all the dispersants in the composition may be 0.5 to 5 percent by weight based on the total amount of the composition.
  • the content of all the dispersants in the composition may be 1 to 3 percent by weight based on the total amount of the composition.
  • the content of all the dispersants in the composition may be 2 percent by weight based on the total amount of the composition.
  • the content of each dispersant in the composition may be 0.1 to 10 percent by weight based on the total amount of the composition.
  • the content of each dispersant in the composition may be 0.2 to 4 percent by weight based on the total amount of the composition.
  • the content of each dispersant in the composition may be 0.5 to 2 percent by weight based on the total amount of the composition.
  • the content of each dispersant in the composition may be 0.8 to 1.2 percent by weight based on the total amount of the composition.
  • the content of each dispersant in the composition may independently be 0.5, 1, or 1.5 percent by weight based on the total amount of the composition.
  • the wetting agent any wetting agents that are generally used in the agrochemical field, especially herbicidal field to reduce the surface tension between the solid surface and water surface and make solid materials more easily wetted by water may be used.
  • the wetting agent may be anionic or nonionic surfactants.
  • Anionic surfactants include alkyl sulfates, sulfonates, fatty acid or fatty acid ester sulfates, carboxylic acid soaps, phosphate esters, and the like.
  • Nonionic surfactants include polyoxyethylene alkylphenol ethers, polyoxyethylene fatty alcohol ethers, polyoxyethylene polyoxypropylene block copolymers and the like.
  • the wetting agent is selected from nonionic surfactants, especially polyoxyethylene polyoxypropylene block copolymers.
  • the content of the wetting agent in the composition may be selected based on the nature of the wetting agent, the required properties of the composition and cost.
  • the content of the wetting agents in the composition may be 0.05 to 5 percent by weight based on the total amount of the composition.
  • the content of wetting agents in the composition may be 0.08 to 3 percent by weight based on the total amount of the composition.
  • the content of the wetting agents in the composition may be 0.1 to 2 percent by weight based on the total amount of the composition.
  • the content of the wetting agents in the composition may be 0.2 to 1 percent by weight based on the total amount of the composition.
  • the content of the wetting agents in the composition may be 0.3 to 0.8 percent by weight based on the total amount of the composition.
  • the content of the wetting agents in the composition may be 0.4 to 0.6 percent by weight based on the total amount of the composition.
  • the content of the wetting agents in the composition may be 0.5 percent by weight based on the total amount of the composition.
  • the emulsifier any emulsifiers that are generally used in the agrochemical field, especially herbicidal field to reduce surface tension and interfacial tension, reduce emulsification energy, and reduce surface free energy to form a stable emulsion may be used.
  • the emulsifier may be salt (e.g. an alkaline earth metal salt, e.g. a calcium salt) of a C 1 -C 22 alkyl-phenyl-sulfonate (e.g.
  • a salt of a C 8 -C 18 alkyl-phenylsulfonate) such as calcium dodecylbenzenesulfonate
  • a castor oil-alkylene oxide addition product condensation product
  • castor oil ethoxylate which can for example have varying amounts of ethoxylation, e.g. a castor oil ethoxylate (e.g., 20 to 50 EO) (i.e.
  • ethylene oxide for example Surfom R 200 available from OXITENO NORDESTE SA INDUSTRIA E COMERCIO
  • a polyalkylene glycol ether especially, a polyethylene glycol ether, for example, polyethylene glycol mono (tristyrylphenyl) ethers (Tristyrylphenol ethoxylates, e.g., Soprophor BSU available from SOLVAY SOLUTIONS ITALIA S. P. A.
  • a tristyrylphenol alkoxylate such as a tristyrylphenol ethoxylate and/or a tristyrylphenol ethoxylate-propoxylate, more particularly a tristyrylphenol ethoxylate containing 8 to 30 (preferably 10 to 25) moles of ethylene oxide (EO) per mole of tristyrylphenol, such as Soprophor TS/10 TM (10 moles EO) , Soprophor BSU TM (16 moles EO) , or Soprophor S/25 TM (25 moles EO) , for example available from Solvay Solutions Nederland B.V.; or a mixture of two or more of these emulsifiers.
  • EO ethylene oxide
  • a combination of two or more emulsifiers may be used in the composition.
  • a combination of a castor oil-alkylene oxide addition product and a polyethylene glycol ether may be used in the composition as the emulsifiers.
  • a combination of a castor oil ethoxylate and a polyethylene glycol mono (tristyrylphenyl) ether is used in the composition as the emulsifiers.
  • the content of the emulsifiers in the composition may be selected based on the nature of the emulsifiers, the required properties of the composition and cost.
  • the content of all the emulsifiers in the composition may be 0.5 to 30 percent by weight based on the total amount of the composition.
  • the content of all the emulsifiers in the composition may be 1 to 20 percent by weight based on the total amount of the composition.
  • the content of all the emulsifiers in the composition may be 2 to 15 percent by weight based on the total amount of the composition.
  • the content of all the emulsifiers in the composition may be 4 to 9 percent by weight based on the total amount of the composition.
  • the content of all the emulsifiers in the composition may be 5 to 8 percent by weight based on the total amount of the composition.
  • the content of all the emulsifiers in the composition may be 6 percent by weight based on the total amount of the composition.
  • the content of each emulsifier in the composition may be 0.1 to 10 percent by weight based on the total amount of the composition.
  • the content of each emulsifier in the composition may be 0.2 to 7 percent by weight based on the total amount of the composition.
  • the content of each emulsifier in the composition may be 0.3 to 6 percent by weight based on the total amount of the composition.
  • the content of each emulsifier in the composition may be 0.5 to 5 percent by weight based on the total amount of the composition.
  • the content of each emulsifier in the composition may independently be 2 or 4 percent by weight based on the total amount of the composition.
  • the antifreeze any antifreezes that are generally used in the agrochemical field, especially herbicidal field to increase flowability at low temperature may be used.
  • the antifreeze may be alcohol or phenols, for example ethylene glycol, 1, 2-propylene glycol, 1, 3-propylene glycol, 1, 2-butanediol, 1, 3-butanediol, 1, 4-butanediol, 1, 4-pentanediol, 3-methyl-1, 5-pentanediol, 2, 3-dimethyl-2, 3-butanediol, trimethylol propane, mannitol, sorbitol, glycerol, pentaerythritol, 1, 4-cyclohexanedimethanol, xylenol, bisphenols such as bisphenol A, urea or the like; ether alcohols such as diethylene glycol, triethylene glycol, tetraethylene glycol, polyoxyethylene or polyoxypropylene glycol
  • the antifreeze may be alcohol, for example ethylene glycol, 1, 2-propylene glycol, 1, 3-propylene glycol, 1, 2-butanediol, 1, 3-butanediol, 1, 4-butanediol, 1, 4-pentanediol, 3-methyl-1, 5-pentanediol, 2, 3-dimethyl-2, 3-butanediol, trimethylol propane, mannitol, sorbitol, glycerol, pentaerythritol, 1, 4-cyclohexanedimethanol, especially ethylene glycol.
  • alcohol for example ethylene glycol, 1, 2-propylene glycol, 1, 3-propylene glycol, 1, 2-butanediol, 1, 3-butanediol, 1, 4-butanediol, 1, 4-pentanediol, 3-methyl-1, 5-pentanediol, 2, 3-dimethyl-2, 3-butanediol, trimethylo
  • the content of the antifreeze in the composition may be selected based on the nature of the antifreeze, the required properties of the composition and cost.
  • the content of the antifreeze in the composition may be 0.1 to 30 percent by weight based on the total amount of the composition.
  • the content of the antifreeze in the composition may be 0.3 to 20 percent by weight based on the total amount of the composition.
  • the content of the antifreeze in the composition may be 0.6 to 10 percent by weight based on the total amount of the composition.
  • the content of the antifreeze in the composition may be 0.8 to 6 percent by weight based on the total amount of the composition.
  • the content of the antifreeze in the composition may be 1 to 4 percent by weight based on the total amount of the composition.
  • the content of the antifreeze in the composition may be 2 percent by weight based on the total amount of the composition.
  • the bactericide any bactericides that are generally used in the agrochemical field, especially herbicidal field to control molds and bacteria may be used.
  • the bactericide may be isothiazolinone compound, especially, benzisothiazolinone, such as, 2-methyl-4-isothiazolin-3-one, 5-chloro-2-methyl-4-isothiazolin-3-one, 1, 2-benzisothiazolin-3-one and the like, sulphur (wettable sulphur) , copper preparations, benzimidazole, bitertanol, dichlofluanid, fenamidone, fenarimol, fenhexamid, fludioxonil, fluopyram, fosetyl-aluminium, iprodione, myclobutanil, penconazole, triadimenol, vinclozolin, tolylfluanid (Euparen ) , eaptan
  • the bactericide may be isothiazolinone compound, especially, benzisothiazolinone, such as, 2-methyl-4-isothiazolin-3-one, 5-chloro-2-methyl-4-isothiazolin-3-one, 1, 2-benzisothiazolin-3-one and the like, especially 1, 2-benzisothiazolin-3-one.
  • the content of the bactericide in the composition may be selected based on the nature of the bactericide, the required properties of the composition and cost. When present, the content of the bactericide in the composition may be 0.005 to 1 percent by weight based on the total amount of the composition.
  • the content of the bactericide in the composition may be 0.002 to 0.5 percent by weight based on the total amount of the composition.
  • the content of the bactericide in the composition may be 0.01 to 0.1 percent by weight based on the total amount of the composition.
  • the content of the bactericide in the composition may be 0.03 to 0.05 percent by weight based on the total amount of the composition.
  • the content of the bactericide in the composition may be 0.04 percent by weight based on the total amount of the composition.
  • the antifoam any antifoams that are generally used in the agrochemical field, especially herbicidal field to reduce the formation of foams upon dilution may be used.
  • the antifoam may be silica, a poly organosiloxane, polydialkylsiloxanes, in particular polydimethylsiloxanes, fluoroaliphatic esters or perfluoroalkylphosphonic/perfluoroalkylphosphonic acids or the salts thereof; and the combination thereof.
  • the antifoam is a poly organosiloxane, for example Silcolapse 432 available from Elkem Silicones (UK) Ltd or Silcolapse C565 available from BLUESTAR SILICONES SHANGHAI CO LTD.
  • the content of the antifoam in the composition may be selected based on the nature of the antifoam, the required properties of the composition and cost.
  • the content of the antifoam in the composition may be 0.002 to 0.2 percent by weight based on the total amount of the composition.
  • the content of the antifoam in the composition may be 0.005 to 0.12 percent by weight based on the total amount of the composition.
  • the content of the antifoam in the composition may be 0.008 to 0.06 percent by weight based on the total amount of the composition.
  • the content of the antifoam in the composition may be 0.01 to 0.03 percent by weight based on the total amount of the composition.
  • the content of the antifoam in the composition may be 0.02 percent by weight based on the total amount of the composition.
  • the composition may comprise other components in addition to those mentioned before, e.g., any impurities brought in along with the active components.
  • the sum of all the components in the composition should be 100 percent by weight based on the total amount of the composition.
  • the stable agrochemical composition of this disclosure may be any stable agrochemical compositions, such as, a stable herbicidal composition, a stable insecticidal composition, a stable pesticidal composition, a stable fungicidal composition, a stable bactericidal composition, and the like.
  • the stable agrochemical composition of this disclosure is a stable herbicidal composition.
  • the stable agrochemical composition of this disclosure may be in any forms, such as a dispersion, a suspo-emulsion (SE) , and the like.
  • the stable composition of this disclosure may include particles, in some cases may include different types of particles.
  • the stable composition is a SE
  • at least two types of particle are present which are solid particles and liquid oil particles
  • at least three phases are present which include a suspension phase formed by the solid particles suspended, an emulsion phase formed by the liquid oil particles, and a continuous phase formed by water.
  • the solid particles in the suspension phase are the solid particles of the first solid active component suspended in water
  • the liquid oil particles in the emulsion phase are formed by the second active component dissolved in the third active component and the organic solvent.
  • the stable composition is a SE, and include solid particles formed by the first active component and liquid oil particles formed by the second active component dissolved in the third active component and the organic solvent, and the mean particle size d90 may be ⁇ 15 ⁇ m, preferably may be ⁇ 7 ⁇ m, based on all particles.
  • the solid particles may have a mean particle size d90 of ⁇ 15 ⁇ m, preferably a mean particle size d90 of ⁇ 7 ⁇ m
  • the liquid oil particles may have a mean particle size d90 of ⁇ 5 ⁇ m, preferably a mean particle size d90 of ⁇ 2 ⁇ m.
  • the mean particle size d90 may be measured by a laser diffractometer or microscope.
  • an oil phase and an aqueous phase in the composition e.g. SE.
  • the first active component, water and some additives like antifoams, thickener, and antifreeze are present in the aqueous phase, while the second and third active components, the organic solvent and other additives are present in the oil phase.
  • the composition e.g.
  • the content of the oil phase (the sum of the second and third active components, the organic solvent and any additives used therein) is at least 30 percent by weight based on the total amount of the composition, preferably at least 40 percent by weight based on the total amount of the composition, preferably at least 50 percent by weight based on the total amount of the composition, preferably at least 60 percent by weight based on the total amount of the composition.
  • compositions of the present disclosure have a superior stability and can satisfy the following stability requirements set forth for suspo-emulsion (SE) as recited in NY/T 2989-2016 (Guidelines on developing the specifications of pesticides for registration) : appearance, wet sieve test, dispersion stability, low temperature stability, and heat storage stability.
  • SE suspo-emulsion
  • the compositions of the present disclosure have a superior dispersion stability, which for example may be measured by CIPAC MT 180 “Dispersion Stability of Suspo-Emulsion. ”
  • the compositions of this disclosure can be stable at 54 °C for at least 2 weeks measured by CIPAC MT 180.
  • the compositions of the disclosure can be stable at room temperature for at least 2 years measured by CIPAC MT 180.
  • the present disclosure provides a process for preparing the stable agrochemical composition described in the first aspect which comprises the steps of:
  • a stable agrochemical composition comprising two solid active components and one liquid active component, especially a stable SE comprising two solid active components and one liquid active component can be successfully prepared from combining EC with SC by carefully selecting the active components in each of EC and SC.
  • the stable agrochemical composition especially the stable SE can be formulated successfully only if a suspension concentrate (SC) of the first active component is mixed with an emulsifiable concentrate (EC) of the second active component and the third active component when the content of the oil phase (the sum of the second and third active components, the organic solvent and other optional additives used therein) is at least 30 percent by weight based on the total amount of the composition, preferably at least 40 percent by weight based on the total amount of the composition, preferably at least 50 percent by weight based on the total amount of the composition, preferably at least 60 percent by weight based on the total amount of the composition.
  • SC suspension concentrate
  • EC emulsifiable concentrate
  • the inventors of the present disclosure surprisingly found that if the second active component is added to SC along with the first active component, no matter what the third active component is formulated into (for example into a EC or a EW) , a stable agrochemical composition, especially a stable SE can not be formulated successfully.
  • the inventors of the present disclosure also surprisingly found that if the second active component is formulated together with the third active component into a EW, even if the first active component is formulated into a SC, a stable agrochemical composition, especially a stable SE can not be formulated successfully especially when the content of the oil phase (the sum of the second and third active components, the organic solvent and any optional additives) is at least 30 percent by weight based on the total amount of the composition, preferably at least 40 percent by weight based on the total amount of the composition, preferably at least 50 percent by weight based on the total amount of the composition, preferably at least 60 percent by weight based on the total amount of the composition.
  • the step a) may comprise mixing the first active component, a first portion of water, and other optional additives to form a homogeneous suspension.
  • the other optional additives that may be used in the step a) may include but are not limited to antifreezes, antifoams, dispersants, other possible surfactants, and the combination thereof.
  • Homogeneous suspension can be determined by visual assessment of appearance, active component content analysis of different spot of a sample, and/or microscope test of different spot of a sample.
  • the mixing may be carried out by any means in the art, such as a mixer.
  • the mixing time is selected based on the nature and amount of the first active component, the nature and amount of other optional additives, and their relative amounts as compared to water.
  • the mixing time may be from 5 min to 60 min depending on e.g., the total amount of the materials.
  • the amount of the first portion of water may be determined by the minimum amount of water required for successfully dispersing the first active component and the total amount of the water used in the composition.
  • the step a) may further comprise milling the obtained suspension until a desirable mean particle size is obtained, for example until a mean particle size d90 ⁇ 15 ⁇ m, preferably ⁇ 7 ⁇ m, more preferably ⁇ 5 ⁇ m is obtained.
  • the milling may be conducted by any suitable machines in the art, for example NETZSCH MINIZETA.
  • the mean particle size may be measured by any conventional method in the art, for example laser particle size analyzer Malvern MS3000.
  • the milling time may be determined by the desirable mean particle size, the machine used for milling and the total amount of the materials. Generally, the milling time may be from 5 min to 60 min depending on e.g., the total amount of the materials and the desired particle size.
  • the step b) may comprise mixing the second and third active components, the organic solvent, and other optional additives to form a clear liquid.
  • the other optional additives may include but are not limited to wetting agents, emulsifiers, bactericides, other possible surfactants, and the combination thereof.
  • the mixing may be conducted by any means in the art, such as a mixer.
  • the mixing time may be selected based on the nature and amount of the second and third active components, the nature and amount of other optional additives, and their relative amounts as compared to the organic solvent, etc. Generally, the mixing time may be from 5 min to 30 min depending on e.g., the total amount of the materials.
  • the mixing in step b) may be conducted under heating for facilitating the dissolution. Heating is optional.
  • the heating may be conducted by any means in the art, for example a magnetic stirring heater.
  • the heating temperature is generally from 30 °C to the boiling point of the organic solvent, preferably 30 to 80 °C, more preferably 40 to 60 °C, e.g., 50°C.
  • the heating time may be the same as, longer or shorter than the mixing time. Generally, the heating time may be from 5 min to 60 min depending on e.g., the total amount of the materials.
  • step a) may be conducted before, after, or at the same time as step b) .
  • step c) the mixing of the SC with the EC and other optional ingredients may be conducted by any means in the art, such as a mixer.
  • the other optional ingredients may include but are not limited to the second portion of water, thickener, other possible surfactants, and the combination thereof.
  • the amount of the second portion of water is decided by the first portion of water and the total amount of water.
  • the mixing time may be from 5 min to 30 min depending on e.g., the total amount of the materials.
  • the mixing of the SC with EC and other optional ingredients may be conducted under a shear (e.g., at 500 to 100000 rpm, for example 1000 to 80000 rpm, especially 2000 to 40000 rpm, more specifically 12000 to 20000 rpm) to obtain a mean particle size d90 ⁇ 15 ⁇ m, preferably a mean particle size d90 ⁇ 7 ⁇ m, more preferably a mean particle size d90 ⁇ 5 ⁇ m based on all particles of all types.
  • the mean particle size may be measured by any conventional method in the art, for example laser particle size analyzer Malvern MS3000.
  • the shear may be accomplished by any means conventional in the art, such as a high shear machine.
  • the shear time may be the same or shorter than the mixing time. Generally, the shear time may be from 5 min to 30 min depending on e.g., the total amount of the materials and the desired particle size.
  • the thickener may be added in step a) , step c) and/or an optional step d) .
  • the step c) i.e., the mixing of the SC with EC and other optional ingredients, may comprise c1) mixing the SC with a part of or all of the thickener to form a homogeneous suspension, and c2) mixing the suspension obtained in c1) with the EC.
  • the remaining other optional ingredients e.g., the second portion of water, and other possible additives
  • the process may further comprise a step d) : mixing the dispersion obtained in step c) with a part of or all of the thickener.
  • the mixing may be conducted by any means in the art, such as a mixer.
  • the mixing time may be from 5 min to 60 min depending on e.g., the total amount of the materials.
  • the present disclosure provides a stable agrochemical composition prepared by a process comprise the steps of:
  • the first active component is solid at room temperature and insoluble in water at room temperature
  • the second active component is solid at room temperature
  • the third active component is liquid at room temperature
  • the first active component is insoluble in the third active component at room temperature, and the second active component has a solubility in the third active component of from 1 to 33 g/100g at room temperature.
  • a stable agrochemical composition comprising first and second solid active components and a liquid third active component, especially a stable SE comprising these two solid active components and the liquid active component can be successfully prepared from combining EC with SC by carefully selecting the active components in each of EC and SC especially when (1) the first active component is insoluble in both water and the third active component, and (2) the second solid active components has a solubility in the liquid active component of from 1 to 33 g/100g at room temperature.
  • a stable agrochemical composition especially a stable SE can be formulated successfully only if a suspension concentrate (SC) of the first active component is mixed with an emulsifiable concentrate (EC) of the second active component and the third active component, especially when the content of the oil phase (the sum of the second and third active components, the organic solvent and any optional additives used therein) is at least 30 percent by weight based on the total amount of the composition, preferably at least 40 percent by weight based on the total amount of the composition, preferably at least 50 percent by weight based on the total amount of the composition, preferably at least 60 percent by weight based on the total amount of the composition.
  • SC suspension concentrate
  • EC emulsifiable concentrate
  • the inventors of the present disclosure surprisingly found that if the second active component is added to SC along with the first active component, no matter what dosage form the third active component is formulated into (for example into a EC or a EW) , a stable agrochemical composition, especially a stable SE can not be formulated successfully.
  • the inventors of the present disclosure also surprisingly found that if the second active component is formulated together with the third active component into a EW, even if the first active component is formulated into SC, a stable agrochemical composition, especially a stable SE can not be formulated successfully especially when the content of the oil phase (the sum of the second and third active components, the organic solvent and any optional additives used therein) is at least 30 percent by weight based on the total amount of the composition, preferably at least 40 percent by weight based on the total amount of the composition, preferably at least 50 percent by weight based on the total amount of the composition, preferably at least 60 percent by weight based on the total amount of the composition.
  • Appearance is measured by visual evaluation.
  • Dispersion stability is measured according to CIPAC MT 180 “Dispersion Stability of Suspo-Emulsion” at a specified temperature.
  • Low temperature stability is measured according to CIPAC MT 39.3 “Stability of Liquid Formulations at 0 °C” for a defined period of time.
  • Heat storage stability is measured according to CIPAC MT 46.3 “Accelerated Storage Procedure” at a specified temperature for a defined period of time.
  • Mean Particle size d90 is measured by laser particle size analyzer Malvern MS3000 according to CIPAC MT 187.
  • the suspension was milled in a bead mill until a mean particle size d90 ⁇ 5 ⁇ m was obtained as measured by laser particle size analyzer Malvern MS3000.
  • a SE1 was formulated as follows:
  • the SE1 was tested for Heat storage stability at 54 °C according to the method mentioned before. A phenomenon of delamination and precipitation was clearly observed at 14 days in the test.
  • ii) The mixture obtained in i) was mixed uniformly at room temperature, and was added into water in the amount as shown in Table 4 in another reactor, and sheared at 12000 to 15000rpm at the same temperature in a high shear machine resulting in an oily mixture rather than an uniform white emulsion.
  • a SC2 was formulated by repeating the procedure in CE1 for formulating SC1 with the exception that the amount of water was reduced to 14.8 g.
  • ASE2 was formulated as follows:
  • EW1 obtained in I was added to SC2 obtained in II, the resulting mixture was mixed evenly. Then, the resulting material was sheared in a high shear machine IKA RW 20 digital at a 15000 to 20000rpm until a mean particle size d90 ⁇ 2 ⁇ m based on all particles of all types was obtained as measured by laser particle size analyzer Malvern MS3000 to obtain a white-like sample with oily droplets on the edge.
  • the SE2 was tested for Heat storage stability at 54 °Caccording to the method mentioned before. A phenomenon of delamination and precipitation was clearly observed at 14 days in the test.
  • the mixture in the reactor was mixed uniformly at room temperature, and was added into water in the amount as shown in Table 5 in another reactor, and sheared at 12000 to 15000rpm at the same temperature resulting in an oily mixture rather than an uniform white emulsion.
  • a SC3 was formulated by repeating the procedure in CE1 for formulating SC1 with the exception that (1) the amount of water was reduced to 14.8 g and (2) Fenclorim tech was not added.
  • a SE3 was formulated as follows:
  • EW2 obtained in I was added to SC3 obtained in II, the resulting mixture was mixed evenly. Then, the resulting material was sheared in a high shear machine IKA RW 20 digital at a 15000 to 20000rpm until a mean particle size d90 based on all particles of all types ⁇ 2 ⁇ m was obtained as measured by laser particle size analyzer Malvern MS3000 to obtain a white-like sample with oily droplets on the edge.
  • the SE3 was tested for Heat storage stability at 54 °C according to the method mentioned before. A phenomenon of delamination and precipitation was clearly observed at 14 days in the test.
  • a SE 4 was formulated as follows:
  • the SE4 was tested for Heat storage stability at 54 °C according to the method mentioned before. A phenomenon of delamination and precipitation was clearly observed at 14 days in the test.
  • SE1 to SE4 all failed in Heat storage stability test at 54 °C.
  • SE1 to SE4 demonstrated that if Fenclorim as the second active component is added to SC along with Penoxsulam as the first active component, no matter what dosage form Pretilachlor as the third active component is formulated into (a EC or a EW) , a stable SE can not be formulated successfully.
  • SE1 to SE4 also demonstrated if Fenclorim as the second active component is formulated together with Pretilachlor as the third active component into a EW, even if Penoxsulam as the first active component is formulated into a SC, a stable SE can not be formulated successfully.
  • the suspension was milled in a bead mill until a mean particle size d90 ⁇ 5 ⁇ m was obtained as measured by laser particle size analyzer Malvern MS3000.
  • SE5 was tested for appearance, wet sieve test, dispersion stability, low temperature stability, and heat storage stability at 54 °C according to the methods mentioned before. SE5 passed all the tests. Specifically, SE5 maintained its dispersion stability after storing both at 0 °C for 7 days and at 54 °C for 14 days.
  • the content of oil phase in CE1 to CE4 and E1 was the same, 58percent by weight.
  • FIG. 1 A microscope photograph was taken on the SE1 obtained in Example 1 using Microscope model BX53, OLYMPUS, which is shown in Fig. 1.
  • Fig. 1 two types of particles were shown, the solid particles formed by Penoxsulam (bright particles) , liquid oil particles formed by Fenclorim dissolved in Pretilachlor and the organic solvent (dark particles) .
  • some of the particles were indicated in the blocks.
  • Fig. 1 also showed the continuous phase formed by water, a part of which was also specifically indicated in the block.
  • the suspension phase formed by the solid particles suspended and the emulsion phase formed by the liquid oil particles were also clear from Fig. 1.
  • the suspension was milled in a bead mill until mean particle size d90 ⁇ 5 ⁇ m was obtained as measured by laser particle size analyzer Malvern MS3000.
  • SE6-9 were formulated by combining SC6-9 with each batch of EC2, respectively, according to the same procedure as mentioned in III of E1.
  • SE6-9 were tested for appearance, wet sieve test, dispersion stability, low temperature stability, and heat storage stability at 54 °C according to the methods mentioned before. Only SE6 and SE9 passed all the tests.
  • the solubility Fenclorim in Pretilachlor at room temperature and 54 °C was tested according to the method as mentioned in Test Methods as 12.1g/100g and 13.1g/100g, respectively. It can be calculated that the solubility of Fenclorim in Pretilachlor has a difference between the room temperature and 54°C of 1 g/100g.
  • the suspension was milled in a bead mill until mean particle size d90 ⁇ 5 ⁇ m was obtained as measured by laser particle size analyzer Malvern MS3000.
  • SE10 to SE12 were formulated by combining SC10 to SC12 with EC3 to E5, respectively (i.e., SC10+EC3, SC11+EC4, SC12+EC5) , according to the same procedure as mentioned in III of E1 with a shear rate at a 12000 to 15000rpm.
  • SE10 to SE12 were tested for appearance, wet sieve test, dispersion stability, low temperature stability, and heat storage stability at 54 °C according to the methods mentioned before. All SE10 to SE12 passed all the tests.

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Abstract

The present disclosure relates to a stable agrochemical composition, a process for preparing the stable agrochemical composition, and a stable agrochemical composition prepared by the process disclosed in the present disclosure. The stable agrochemical composition comprises a first active component which is solid at room temperature and insoluble in water at room temperature; a second active component which is solid at room temperature; a third active component which is liquid at room temperature; and water; the first active component is insoluble in the third active component at room temperature, and the second solid active component has a solubility in the third liquid active component of from 1 to 33 g/100g at room temperature.

Description

STABLE AGROCHEMICAL COMPOSITION COMPRISING TWO SOLID ACTIVE COMPONENTS AND ONE LIQUID ACTIVE COMPONENT AND ITS PREPARATION PROCESS
TECHNICAL FIELD OF THE DISCLOSURE
The present disclosure relates to a stable agrochemical composition comprising two solid active components and one liquid active component and its preparation process. More specifically, the present disclosure relates to a stable agrochemical composition e.g., a suspo-emulsion (SE) comprising Penoxsulam, Pretilachlor, and a further solid active component, especially a solid safener, e.g., Fenclorim, and its preparation process. Alternatively, the present disclosure relates to a stable agrochemical composition e.g., a suspo-emulsion (SE) comprising Pretilachlor, Fenclorim, and a further solid active component selected from the group consisted of Penoxsulam, Pyrazosulfuron-ethyl, Bensulfuron methyl, Quinclorac, Oxyfluorfen, Oxadiazon, cyhalofop-butyl, Pyriminobac-methyl, Clomazone (Dimethazon) , Pyribenzoxim, Oxadiargyl, and Simetryn, and its preparation process.
FIELD AND BACKGROUND OF THE DISCLOSURE
Two or more agrochemical active components with different mechanisms of action are generally combined to provide an expanded range of applications, such as weed spectrum, or to provide a synergy. In the herbicidal field, in some cases, a safener is also be added to the agrochemical composition as an active component to protect the crops. For example, Fenclorim is generally used along with Pretilachlor in a ratio of 1: 2 to 1: 5 (e.g., 1: 3 or 1: 4) . Therefore, if Pretilachlor is intended to combine with another herbicide, e.g., Penoxsulam to provide e.g., an expanded weed spectrum, and Fenclorim is also used at the same time, a agrochemical composition (specifically in this case a herbicidal composition) comprising three active components has to be formulated in which two active components are solid and one active component is liquid. To formulate an agrochemical composition comprising two solid active components and one liquid active component, a suspo-emulsion (SE) is the usual choice, especially when at least one of the two solid active components is insoluble in water or the liquid active component.
In general, in order to formulate a SE of two solid active components and one liquid active component, it is a general practice to mill the two solid active  components into powders in micrometer and then disperse these powders into the liquid active component. However, this route is not always successful because a SE may not be formulated at all or a stable SE may not be obtained. It has now been found that, especially when any one of the two solid active components has a solubility in the liquid active component of from 1 to 33 g/100g (especially, 8 to 15 g/100g) at room temperature, a SE may not be formulated at all or a stable SE may not be obtained through the conventional route mentioned before. It has now also been found that, especially when any one of the two solid active components has a solubility in the liquid active component of from 1 to 33 g/100g at room temperature, routes adopting a combination of EC and SC or a combination of EW and SC may also not guarantee that a stable SE may be successfully formulated.
To address the existing problems in the art, the inventors completed the present disclosure.
SUMMARY OF THE DISCLOSURE
Surprisingly, it has now been found that, when any one of the two solid active components has a solubility in the liquid active component of from 1 to 33 g/100g at room temperature, an agrochemical composition comprising two solid active components and one liquid active component, e.g., a stable SE comprising two solid active components and on e liquid active component can be successfully prepared, e.g., from combining EC with SC by carefully selecting the active components in each of EC or SC, especially when the content of the oil phase is very high, e.g., at least 30 percent by weight based on the total amount of the composition, preferably at least 40 percent by weight based on the total amount of the composition, preferably at least 50 percent by weight based on the total amount of the composition, preferably at least 60 percent by weight based on the total amount of the composition.
The present disclosure provides a stable agrochemical composition comprising two solid active components and one liquid active component and its preparation process. More specifically, the present disclosure provides a stable agrochemical composition e.g., a suspo-emulsion comprising Penoxsulam, Pretilachlor, and a further solid active component, especially a solid safener, e.g., Fenclorim, and its preparation process. Alternatively, the present disclosure relates to a stable agrochemical composition e.g., a suspo-emulsion (SE) comprising Pretilachlor, Fenclorim, and a further solid active component selected from the group consisted of  Penoxsulam, Pyrazosulfuron-ethyl, Bensulfuron methyl, Quinclorac, Oxyfluorfen, Oxadiazon, cyhalofop-butyl, Pyriminobac-methyl, Clomazone (Dimethazon) , Pyribenzoxim, Oxadiargyl, and Simetryn, and its preparation process.
Specifically, the present disclosure provides:
1. A stable agrochemical composition, comprising:
a first active component which is solid at room temperature and insoluble in water at room temperature;
a second active component which is solid at room temperature;
a third active component which is liquid at room temperature; and
water;
the first active component is insoluble in the third active component at room temperature, and the second solid active component has a solubility in the third liquid active component of from 1 to 33 g/100g at room temperature.
2. The stable agrochemical composition of embodiment 1 wherein the first active component, the second active component and the third active component are herbicidal active components.
3. The stable agrochemical composition of embodiment 2 wherein the first active component is neither Pretilachlor nor a safener, the third liquid active component is Pretilachlor, and the second active component is Fenclorim.
4. The stable agrochemical composition of embodiment 3, wherein the first active component is any one selected from the group consisted of Penoxsulam, Pyrazosulfuron-ethyl, Bensulfuron methyl, Quinclorac, Oxyfluorfen, Oxadiazon, cyhalofop-butyl, Pyriminobac-methyl, Clomazone (Dimethazon) , Pyribenzoxim, Oxadiargyl, and Simetryn.
5. The stable agrochemical composition of embodiment 2 wherein the first active component is a triazolopyrimidine sulfonamide herbicide compound, the third liquid active component is an acetanilide herbicide compound, and the second active component is a safener compound
6. The stable agrochemical composition of embodiment 1, wherein the first active component is Penoxsulam, the third liquid active component is Pretilachlor, and the second active component is Fenclorim.
7. The stable agrochemical composition of any one of embodiments 1 to 6, wherein the content of the first active component is 0.02 to 40 percent by weight based on the total amount of the composition, the content of the second active component is 1 to 60 percent by weight based on the total amount of the composition, and the content of the third active component is 3 to 90 percent by weight based on the total amount of the composition.
8. The stable agrochemical composition of embodiment 7, wherein the content of the first active component is 0.04 to 20 percent by weight based on the total amount of the composition, the content of the second active component is 2 to 30 percent by weight based on the total amount of the composition, and the content of the third active component is 6 to 80 percent by weight based on the total amount of the composition.
9. The stable agrochemical composition of embodiment 7, wherein the content of the first active component is 0.08 to 10 percent by weight based on the total amount of the composition, the content of the second active component is 4 to 15 percent by weight based on the total amount of the composition, and the content of the third active component is 12 to 40 percent by weight based on the total amount of the composition.
10. The stable agrochemical composition of embodiment 7, wherein the content of the first active component is 0.1 to 8 percent by weight based on the total amount of the composition, the content of the second active component is 4.9 to 11 percent by weight based on the total amount of the composition, and the content of the third active component is 15 to 33 percent by weight based on the total amount of the composition.
11. The stable agrochemical composition of any one of embodiments 1 to 10, wherein the weight ratio of the second active component to the third active component is 1: 2 to 4.
12. The stable agrochemical composition of any one of embodiments 1 to 11, wherein the composition further comprises an organic solvent with a content of 1 to 40 percent by weight based on the total amount of the composition.
13. The stable agrochemical composition of any one of embodiments 1 to 12, wherein the composition further comprises one or more additives selected from the group consisting of thickener, dispersant, wetting agent, emulsifier, antifreeze, antifoam, and bactericide.
14. The stable agrochemical composition of embodiment 13, wherein the total amount the additives is 3 to 70 percent by weight based on the total amount of the composition.
15. The stable agrochemical composition of any one of embodiments 1 to 14, wherein the content of the oil phase in the composition is at least 50 percent by weight based on the total amount of the composition.
16. The stable agrochemical composition of any one of embodiments 1 to 15, wherein the composition is SE.
17. The stable agrochemical composition of any one of embodiments 1 to 16, wherein the stable composition has particles with a mean particle size d90 of ≤7 μm based on all particles of all types.
18. The stable agrochemical composition of any one of embodiments 1 to 17, wherein the stable composition satisfies the stability requirements set forth for SE as recited in NY/T 2989-2016.
19. The stable agrochemical composition of any one of embodiments 1 to 18, wherein the stable composition is a herbicidal composition.
20. A process for preparing the stable agrochemical composition of embodiments 1 to 19, comprising the steps of:
a) forming a SC of the first active component,
b) forming an EC of the second active component and the third active component; and
c) mixing the SC with the EC and other optional ingredients.
21. The process of embodiment 20, wherein the step a) comprises mixing the first active component, a first portion of water, and other optional additives to form a homogeneous suspension.
22. The process of embodiment 21, wherein the step a) further comprises milling the suspension until the mean particle size d90 is ≤7 μm.
23. The process of any of embodiments 19-22, wherein the step b) comprises mixing the second and third active components, an optional organic solvent and other optional additives to form a clear liquid.
24. The process of embodiment 23, wherein the mixing is conducted under heating.
25. The process of any of embodiments 19-24, wherein in the step c) , the mixing of the SC with EC is conducted under a shear and the mean particle size d90 of the composition is ≤7 μm based on all particles of all types.
26. The process of any of embodiments 19-25, wherein the composition comprises a thickener, and the step c) comprises c1) mixing the SC with a part of or all of the thickener to form a homogeneous suspension, and c2) mixing the suspension obtained in c1) with the EC.
27. The process of any of embodiments 19-25, wherein the composition comprises a thickener, and the process further comprises a step d) : mixing the dispersion obtained in step c) with a part of or all of the thickener.
28. Astable agrochemical composition prepared by a process comprise the steps of
a)forming a SC of a first active component;
b)forming an EC of a second active component and a third active component; and
c)mixing the SC with EC and other optional ingredients;
wherein the first active component is solid at room temperature and insoluble in water at room temperature, the second active component is solid at room temperature, and the third active component is liquid at room temperature; and
the first active component is insoluble in the third active component at room temperature, and the second active component has a solubility in the third active component of from 1 to 33 g/100g at the room temperature.
29. The stable agrochemical composition of embodiment 28, wherein the step a) comprises mixing the first active component, a first portion of water, and other optional additives to form a homogeneous suspension.
30. The stable agrochemical composition of embodiment 29, wherein the step a) further comprises milling the suspension until the mean particle size d90 is ≤7 μm.
31. The stable agrochemical composition of any one of embodiments 28 to 30, wherein the step b) comprises mixing the second and third active components, an optional organic solvent and other optional additives to form a clear liquid.
32. The stable agrochemical composition of embodiments 31, wherein the mixing is conducted under heating.
33. The stable agrochemical composition of any one of embodiments 28 to 32, wherein the composition comprises a thickener, and the step c) comprises c1) mixing the SC with the thickener to form a homogeneous suspension, and c2) mixing the suspension obtained in c1) with the EC.
34. The stable agrochemical composition of any one of embodiments 28 to 32, wherein the composition comprises a thickener, and the thickener is not added in the step c) , the process further comprises a step d) : mixing the obtained dispersion in step c) with the thickener.
35. The stable agrochemical composition of any one of embodiments 28 to 34, wherein in the step c) , the mixing of the SC with EC is conducted under a shear until the mean particle size d90 of the composition is ≤7 μm based on all particles of all types.
36. The stable agrochemical composition of any one of embodiments 28 to 35, wherein the first active component, the second active component and the third active component are herbicidal active components.
37. The stable agrochemical composition of embodiment 36, wherein the first active component is neither Pretilachlor nor a safener, the third liquid active component is Pretilachlor, and the second active component is Fenclorim.
38. The stable agrochemical composition of embodiment 37, wherein the first active component is any one selected from the group consisted of Penoxsulam, Pyrazosulfuron-ethyl, Bensulfuron methyl, Quinclorac, Oxyfluorfen, Oxadiazon, cyhalofop-butyl, Pyriminobac-methyl, Clomazone (Dimethazon) , Pyribenzoxim, Oxadiargyl, and Simetryn.
39. The stable agrochemical composition of any one of embodiments 28 to 36, wherein the first active component is a triazolopyrimidine sulfonamide herbicide compound, the third liquid active component is an acetanilide herbicide compound, and the second active component is a safener compound.
40. The stable agrochemical composition of any one of embodiments 28 to 39, wherein the first active component is Penoxsulam, the third liquid active component is Pretilachlor, and the second active component is Fenclorim.
41. The stable agrochemical composition of any one of embodiments 28 to 40, wherein the content of the first active component is 0.02 to 40 percent by weight based on the total amount of the composition, the content of the second active component is 1 to 60 percent by weight based on the total amount of the composition, and the content of the third active component is 3 to 90 percent by weight based on the total amount of the composition.
42. The stable agrochemical composition of embodiment 41, wherein the content of the first active component is 0.04 to 20 percent by weight based on the total amount of the composition, the content of the second active component is 2 to 30 percent by weight based on the total amount of the composition, and the content of the third active component is 6 to 80 percent by weight based on the total amount of the composition.
43. The stable agrochemical composition of embodiment 41, wherein the content of the first active component is 0.08 to 10 percent by weight based on the total amount of the composition, the content of the second active component is 4 to 15 percent by weight based on the total amount of the composition, and the content of the third active component is 12 to 40 percent by weight based on the total amount of the composition.
44. The stable agrochemical composition of embodiment 41, wherein the content of the first active component is 0.1 to 8 percent by weight based on the total amount of the composition, the content of the second active component is 4.9 to 11 percent by weight based on the total amount of the composition, and the content of the third active component is 15 to 33 percent by weight based on the total amount of the composition.
45. The stable agrochemical composition of any one of embodiments 28 to 44, wherein the weight ratio of the second active component to the third active component is 1: 2 to 4.
46. The stable agrochemical composition of any one of embodiments 28 to 45, wherein the composition further comprises an organic solvent with a content of 1 to 40 percent by weight based on the total amount of the composition.
47. The stable agrochemical composition of any one of embodiments 28 to 46, wherein the composition further comprises one or more additives selected from the group consisting of thickener, dispersant, wetting agent, emulsifier, antifreeze, antifoam, and bactericide.
48. The stable agrochemical composition of embodiment 47, wherein the total amount the additives is 3 to 70 percent by weight based on the total amount of the composition.
49. The stable agrochemical composition of any one of embodiments 28 to 48, wherein the content of the oil phase in the composition is at least 50 percent by weight based on the total amount of the composition.
50. The stable agrochemical composition of any one of embodiments 28 to 49, wherein the composition is SE.
51. The stable agrochemical composition of any one of embodiments 28 to 50, wherein the stable composition has particles with a mean particle size d90 of ≤7 μm based on all particles of all types.
52. The stable agrochemical composition of any one of embodiments 28 to 51, wherein the stable composition satisfies the stability requirements set forth for SE as recited in NY/T 2989-2016.
53. The stable agrochemical composition of any one of embodiments 28 to 52, wherein the stable composition is a herbicidal composition.
BRIEF DESCRIPTION OF THE DRAWINGS
Fig. 1 shows a microscope photograph which was taken on the SE1 obtained in Example 1.
DESCRIPTION OF SPECIFIC EMBODIMENTS OF THE DISCLOSURE
Definitions
Prior to setting forth the present subject matter in detail, it may be helpful to provide definitions of certain terms to be used herein. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as is commonly understood by one of skill in the art to which this disclosure pertains.
Penoxsulam is the common name for 2- (2, 2-difluoroethoxy) -N- (5, 8-dimethoxy- [l, 2, 4] triazolo [l, 5-c] pyrimidin-2-yl) -6- (trifluoromethyl) benzenesulfonamide with a structure of
Figure PCTCN2022118727-appb-000001
Its herbicidal activity is described in The Pesticide Manual, Fifteenth Edition, 2009. Penoxsulam is a solid at room temperature with a melting point of 212 ℃ and has a solubility in water of 5.7 mg/L (pH=5) at room temperature.
Pretilachlor is the common name for 2-chloro-N- (2, 6-diethylphenyl) -N- (2-propoxyethyl) acetamide with a structure of
Figure PCTCN2022118727-appb-000002
Its herbicidal activity is described in The Pesticide Manual, Fifteenth Edition, 2009. Pretilachlor is a liquid at room temperature with a melting point less of -20 ℃.
Fenclorim is the common name for 4, 6-dichloro-2-phenylpyrimidine with a structure of
Figure PCTCN2022118727-appb-000003
Fenclorim is a solid at room temperature with a melting point of 96.9 ℃ and has a solubility in water of 2.5 mg/L at room temperature.
As used herein, the term "composition" refers, but is not limited to, a combination in any physical form, e.g., blend, solution, alloy, or the like.
As used herein, the term "active component" refers, but is not limited to, any compounds which have an agricultural activity, for example, insecticidal activity, fungicidal activity, bactericidal activity, herbicidal activity, safening activity,  protecting activity, etc. Therefore, the term "active component" comprises, but is not limited to, insecticide compound, fungicide compound, bactericide compound, herbicide compound, safener compound, acaricide compound, nematicide compound, bird repellent compound, and plant nutrient compound, etc.
As used herein, the term "herbicidal active component" refers, but is not limited to, any compounds which have herbicidal activity, safening activity, or protecting activity, etc. Therefore, the term "herbicidal active component" comprises herbicide compound, safener compound, etc.
As used herein, the term "suspo-emulsion (SE) " means a mixture of water-insoluble active ingredients dispersed in an aqueous solution, where one (or more) of the active ingredients is in suspension form and one (or more) of the active ingredients is in emulsion form. The formulation is intended for dilution into water prior to spray application. Mixtures of active ingredients are often used to provide a broader spectrum of control. Formulating the active ingredients together eliminates the need for tank mixing (which can lead to incompatibilities) . Like other aqueous liquid formulations, suspo-emulsions are easy to handle and measure, dust free, non-flammable and offer good miscibility with water (see, “Manual on development and use of FAO and WHO specifications for pesticides” ) .
As used herein, the term “stable” when used in connection with a composition means that the composition should satisfy the following stability requirements set forth for suspo-emulsion (SE) as recited in NY/T 2989-2016 (Guidelines on developing the specifications of pesticides for registration) : appearance, wet sieve test, dispersion stability, low temperature stability (only for appearance, wet sieve test, and dispersion stability) , and heat storage stability (only for appearance, wet sieve test, and dispersion stability) .
As used herein, the term "insoluble" means the solubility of a material (e.g., an active component) in a specified material (for example, water, the third active component, etc., ) is less than 0.1g/1000g at a specified temperature.
As used herein, an "ultra-low naphthalene solvent" is a solvent with a naphthalene concentration of less than 0.1 wt %.
As used herein, a "low naphthalene solvent" is a solvent with a naphthalene concentration of less than 1 wt %.
As used herein, the term "additive" is defined as any substance that is not an active component but is added to the composition such as sticking agents, surfactants, synergists, buffers, acidifiers, defoaming agents, thickeners, etc.
As used herein, the term "safener" refers to an agent that increases the tolerance of plants to herbicides without significantly affecting the effectiveness of the herbicide.
As used herein, the term "thickener" refers to an agent that increases the viscosity of a liquid composition without substantially changing other properties of the composition.
As used herein the term "agriculturally acceptable carrier" means carriers of which are known and accepted in the art for the formation of formulations for agricultural or horticultural use.
The term "surfactant, " as used herein, refers to an agriculturally acceptable material which imparts emulsifiability, stability, spreading, wetting, dispersibility or other surface-modifying properties.
As used herein the term "mean Particle size d90" means particle size distribution D90, which represents the particle diameter corresponding to 90%cumulative (from 0 to 100%) undersize particle size distribution.
As used herein the term "room temperature" means 23±2℃.
The term “a” or “an” as used herein includes the singular and the plural, unless specifically stated otherwise. Therefore, the term “a, ” “an, ” or “at least one” can be used interchangeably in this application.
It is understood that where a parameter range is provided, all integers within that range, and tenths thereof, are also provided by the disclosure as if the integers and tenths thereof are expressly described herein. For example, “0.1%to 70%” includes 0.1%, 0.2%, 0.3%, 0.4%, 0.5%etc. up to 70%.
Throughout the application, descriptions of various embodiments use the term "comprising" ; however, it will be understood by one of skill in the art, that in some specific instances, an embodiment can alternatively be described using the language "consisting essentially of" or "consisting of" .
For purposes of better understanding the present teachings and in no way limiting the scope of the teachings, unless otherwise indicated, all numbers expressing quantities, percentages, or proportions, and other numerical values used in the  specification and claims, are to be understood as being modified in all instances by the term "about. " Accordingly, unless indicated to the contrary, the numerical parameters set forth in the following specification and attached claims are approximations that may vary depending upon the desired properties sought to be obtained. At the very least, each numerical parameter should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques. In this regard, use of the term "about" herein specifically includes ±10%from the indicated values in the range. In addition, the endpoints of all ranges directed to the same component or property herein are inclusive of the endpoints, are independently combinable, and include all intermediate points and ranges.
First Aspect
In the first aspect, the present disclosure provides a stable agrochemical composition, comprising:
a first active component which is solid at room temperature and insoluble in water at room temperature;
a second active component which is solid at room temperature;
a third active component which is liquid at room temperature; and
water;
the first active component is insoluble in the third active component at room temperature, and the second active component has a solubility in the third active component of from 1 to 33 g/100g at room temperature.
The first active component is solid at room temperature and insoluble in water at room temperature. In general, the solubility of the first active component in water at room temperature is less than 0.1g/L, preferably less than 0.08g/L. The first active component is slightly soluble to insoluble in the third active component at room temperature. In general, the solubility of the first active component in the third active component at room temperature is less than 1g/100g, preferably less than 0.2g/100g.
The second active component is solid at room temperature and the second active component has a solubility in the third active component of from 1 to 33 g/100g at room temperature. Within the range of 1 to 33 g/100g, the solubility of the second active component in the third active component at room temperature may be 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 12.1, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, or 33 g/100g, or any ranges formed by selecting any two  solubilities mentioned above as the two limits, for example, the solubility of the second active component in the third active component at room temperature may be 2 to 30 g/100g, or 5 to 25 g/100g. Preferably, the second active component has a solubility in the third active component of from 2 to 28 g/100g, 5 to 20 g/100g, 7 to 18 g/100g, 8 to 15 g/100g, 9 to 14 g, or 11 to 13 /100g at room temperature. For example, the second active component has a solubility in the third active component of 12.1 g/100g at room temperature.
Surprisingly, without bound by the theory, it has now been found that, the solubility of the second solid active component in the third liquid active component at room temperature is important to understand why in some cases a stable agrochemical composition comprising the three active components, especially a stable SE comprising the three active components can not be formulated. When the second active component has a solubility in the third active component of from 1 to 33 g/100g at room temperature, a stable agrochemical composition comprising the three active components, especially a stable SE comprising the three active components, may not be formulated at all or may not be obtained through the conventional route mentioned before, in some cases also depending on the amounts of the second active component and the third active component. It has now also been found that, especially when the second solid active component has a solubility in the third liquid active component of from 1 to 33 g/100g at room temperature, routes adopting a combination of EC and SC or a combination of EW and SC may also not guarantee that a stable SE may be successfully formulated. The same is true especially when the second active component has a solubility in the third active component of from 1 to 33 g/100g at room temperature, and the solubility of the second active component in the third active component has a difference between the room temperature and 54℃ of higher than or equal to 1 g/100g, in some cases also depending on the amounts of the second active component and the third active component.
If the solubility of the second solid active component in the third liquid active component is high enough, and the amounts of the second active component and the third active component are such that the second active component is dissolved totally in the third active component no matter at room temperature or 54℃, a stable SE will be easily formulated through the conventional route mentioned before. To the contrary, if the solubility of the second solid active component in the third liquid active component is small enough, and also considering the amounts of the second  active component and the third active component, those skilled in the art will not even think of formulating a SE through the conventional route mentioned before.
The third active component is liquid at room temperature.
The first active component, the second active component and the third active component may be independently selected from the group consisting of insecticide compounds, fungicide compounds, bactericide compounds, herbicide compounds, safener compounds, acaricide compounds, nematicide compounds, bird repellent compounds, and plant nutrient compounds. Preferably, all the first active component, the second active component and the third active component are selected from the herbicidal active components. For example, both the first and third active components are herbicide compounds, and the second active component is a safener. Preferably, the first active component is a triazolopyrimidine sulfonamide herbicide compound, the third liquid active component is an acetanilide herbicide compound, and the second active component is a safener compound e.g., a phenylpyrimidine safener compound. Alternatively, for example, the first active component is a herbicidal compound which is neither Pretilachlor nor a safener compound, the third liquid active component is Pretilachlor, and the second active component is Fenclorim. Preferably, the first active component is any one selected from the group consisted of Penoxsulam, Pyrazosulfuron-ethyl, Bensulfuron methyl, Quinclorac, Oxyfluorfen, Oxadiazon, cyhalofop-butyl, Pyriminobac-methyl, Clomazone (Dimethazon) , Pyribenzoxim, Oxadiargyl, and Simetryn, the third liquid active component is Pretilachlor, and the second active component is Fenclorim. Most preferably, the first active component is Penoxsulam, the third liquid active component is Pretilachlor, and the second active component is Fenclorim.
In the composition, the content of the first active component may be 0.02 to 40 percent by weight based on the total amount of the composition. Within the range of 0.02 to 40 percent by weight based on the total amount of the composition, the content of the first active component may be 0.02, 0.03, 0.04, 0.05, 0.06, 0.07, 0.08, 0.09, 0.1, 0.11, 0.12, 0.13, 0.14, 0.15, 0.16, 0.17, 0.18, 0.19, 0.2, 0.25, 0.3, 0.35, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, 1.1, 1.2, 1.3, 1.34, 1.4, 1.5, 1.6, 1.7, 1.8, 1.9, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40 percent by weight based on the total amount of the composition, or any ranges formed by selecting any two contents mentioned above as the two limits, for example, the content of the first active component may be 0.03 to  10, or 1.2 to 8 percent by weight based on the total amount of the composition. Preferably, the content of the first active component may be 0.04 to 20 percent by weight based on the total amount of the composition. More preferably, the content of the first active component may be 0.08 to 10 percent by weight based on the total amount of the composition. More preferably, the content of the first active component may be 0.1 to 8 percent by weight based on the total amount of the composition. For example, the content of the first active component may be 0.1, 1.2 or 8 percent by weight based on the total amount of the composition.
In the composition, the content of the first active component may be 0.1 to 10 percent by weight based on the total amount of the composition. Within the range of 0.1 to 10 percent by weight based on the total amount of the composition, the content of the first active component may be 0.2, 0.3, 0.4, 0.5, 0.6, 0.7, 0.8, 0.9, 1.0, 1.1, 1.2, 1.3, 1.34, 1.4, 1.5, 1.6, 1.7, 1.8, 1.9, 2, 3, 4, 5, 6, 7, 8, 9, or 10 percent by weight based on the total amount of the composition, or any ranges formed by selecting any two contents mentioned above as the two limits, for example, the content of the first active component may be 0.3 to 8, or 0.5 to 5 percent by weight based on the total amount of the composition. Preferably, the content of the first active component may be 0.8 to 3 percent by weight based on the total amount of the composition. More preferably, the content of the first active component may be 0.9 to 2 percent by weight based on the total amount of the composition. More preferably, the content of the first active component may be 1 to 1.5 percent by weight based on the total amount of the composition. For example, the content of the first active component may be 1.2 or 1.3 percent by weight based on the total amount of the composition.
In the composition, the content of the second active component may be 1 to 60 percent by weight based on the total amount of the composition. Within the range of 1 to 60 percent by weight based on the total amount of the composition, the content of the second active component may be 1, 2, 3, 4, 4.9, 5, 6, 7, 8, 9, 10, 10.2, 10.7, 10.9, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, 50, 51, 52, 53, 54, 55, 56, 57, 58, 59, or 60 percent by weight based on the total amount of the composition, or any ranges formed by selecting any two contents mentioned above as the two limits, for example, the content of the second active component may be 3 to 50, or 5 to 10 percent by weight based on the total amount of the composition. Preferably, the content of the second active component may be 2 to 30 percent by weight based on  the total amount of the composition. Preferably, the content of the second active component may be 4 to 15 percent by weight based on the total amount of the composition. More preferably, the content of the second active component may be 4.9 to 11 percent by weight based on the total amount of the composition. For example, the content of the second active component may be 4.9, 10.2 or 10.9 percent by weight based on the total amount of the composition.
In the composition, the content of the second active component may be 1 to 40 percent by weight based on the total amount of the composition. Within the range of 1 to 40 percent by weight based on the total amount of the composition, the content of the second active component may be 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 10.2, 10.7, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, or 40 percent by weight based on the total amount of the composition, or any ranges formed by selecting any two contents mentioned above as the two limits, for example, the content of the second active component may be 2 to 30, or 5 to 20 percent by weight based on the total amount of the composition. Preferably, the content of the second active component may be 8 to 15 percent by weight based on the total amount of the composition. More preferably, the content of the second active component may be 9 to 12 percent by weight based on the total amount of the composition. For example, the content of the second active component may be 10.2 or 10.7 percent by weight based on the total amount of the composition.
In the composition, the content of the third active component may be 3 to 90 percent by weight based on the total amount of the composition. Within the range of 3 to 90 percent by weight based on the total amount of the composition, the content of the third active component may be 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 30.8, 31, 31.8, 32, 32.8, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, 50, 51, 52, 53, 54, 55, 56, 57, 58, 59, 60, 61, 62, 63, 64, 65, 66, 67, 68, 69, 70, 71, 72, 73, 74, 75, 76, 77, 78, 79, 80, 81, 82, 83, 84, 85, 86, 87, 88, 89, or 90 percent by weight based on the total amount of the composition, or any ranges formed by selecting any two contents mentioned above as the two limits, for example, the content of the third active component may be 10 to 70, or 15 to 60 percent by weight based on the total amount of the composition. Preferably, the content of the third active component may be 6 to 80 percent by weight based on the total amount of the composition. More preferably, the content of the third active component may be 12 to 40 percent by weight based on the total  amount of the composition. More preferably, the content of the third active component may be 15 to 33 percent by weight based on the total amount of the composition. For example, the content of the third active component may be 30.8, 31.8 or 32.8 percent by weight based on the total amount of the composition.
In the composition, the content of the third active component may be 3 to 80 percent by weight based on the total amount of the composition. Within the range of 3 to 80 percent by weight based on the total amount of the composition, the content of the third active component may be 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 30.8, 31, 31.8, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, 50, 51, 52, 53, 54, 55, 56, 57, 58, 59, 60, 61, 62, 63, 64, 65, 66, 67, 68, 69, 70, 71, 72, 73, 74, 75, 76, 77, 78, 79, or 80 percent by weight based on the total amount of the composition, or any ranges formed by selecting any two contents mentioned above as the two limits, for example, the content of the third active component may be 6 to 70, or 15 to 50 percent by weight based on the total amount of the composition. Preferably, the content of the third active component may be 20 to 40 percent by weight based on the total amount of the composition. More preferably, the content of the third active component may be 25 to 35 percent by weight based on the total amount of the composition. More preferably, the content of the third active component may be 29 to 35 percent by weight based on the total amount of the composition. For example, the content of the third active component may be 30.8, 31.8 or 32.8 percent by weight based on the total amount of the composition.
Depending on the specific second and third active components, in the composition, the weight ratio of the second active component to the third active component may be 1: (1 to 6) . Preferably, the weight ratio of the second active component to the third active component may be 1: (1.5 to 5) . More preferably, the weight ratio of the second active component to the third active component may be 1: (2 to 4) . For example, the weight ratio of the second active component to the third active component is 1: 3.
The composition also includes water. Water is used as a carrier. The content of the water in the composition may be 5 to 90 percent by weight based on the total amount of the composition. Within the range of 5 to 90 percent by weight based on the total amount of the composition, the content of the third active component may be 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29,  30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, 50, 51, 52, 53, 54, 55, 56, 57, 58, 59, 60, 61, 62, 63, 64, 65, 66, 67, 68, 69, 70, 71, 72, 73, 74, 75, 76, 77, 78, 79, 80, 81, 82, 83, 84, 85, 86, 87, 88, 89 or 90 percent by weight based on the total amount of the composition, or any ranges formed by selecting any two contents mentioned above as the two limits, for example, the content of the water in the composition may be 6 to 70, or 15 to 50 percent by weight based on the total amount of the composition. Preferably, the content of the water in the composition may be 10 to 75 percent by weight based on the total amount of the composition. Preferably, the content of the water in the composition may be 20 to 50 percent by weight based on the total amount of the composition. Preferably, the content of the water in the composition may be 25 to 45 percent by weight based on the total amount of the composition. Preferably, the content of the water in the composition may be 30 to 40 percent by weight based on the total amount of the composition. For example, the content of the water in the composition may be 35 percent by weight based on the total amount of the composition.
The composition may further comprise an organic solvent. The organic solvent should be selected based at least on: (1) the specific second and third active components with the intention of preparing successfully for example an EC of the specific second and third active components; (2) that solubility of the organic solvent in water at room temperature should not be too high, for example that solubility of the organic solvent in water at room temperature should be less than 0.1 g/1000g. In generally, the organic solvent may be selected from the group consisting of aromatic hydrocarbons (for example toluene, xylene, ethylbenzene, isopropylbenzene, tert-butylbenzene, naphthalenes, mono-or polyalkyl-substituted naphthalenes) , paraffins, petroleum, diesel, mineral oil, fatty acid amides, fatty acids, tall oil fatty acids, alkyl esters of fatty acids, modified vegetable oils, and any combination thereof. Preferably, the organic solvent may be selected from the group consisting of aromatic hydrocarbons, paraffins, petroleum, diesel, mineral oil, fatty acids, tall oil fatty acids, and any combination thereof. More preferably, the organic solvent may be aromatic hydrocarbons, especially in consideration of environmental protection, a low naphthalene aromatic hydrocarbons solvent, for example, aromatic solvent S-150ND or S-100A available from Jiangsu Hualun Chemical Industry Co., Ltd., Solvesso TM grades from ExxonMobil Chemical (for example Solvesso TM 100 (CAS No. 64742- 95-6) , Solvesso TM 150 (CAS No. 64742-94-5) , and Solvesso TM 200 (CAS No. 64742-94-5) ) , and Caromax TM 28 LN from Petrochem Carless.
When the organic solvent is present, its content in the composition should be enough to (1) dissolve the second active material which is not fully disclosed in the third active material and (2) prepare successfully for example an EC of the specific second and third active components. In one embodiment, when the organic solvent is present, its content in the composition may be 1 to 40 percent by weight based on the total amount of the composition. Within the range of 1 to 40 percent by weight based on the total amount of the composition, the content of the solvent may be 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 11.1, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, or 40 percent by weight based on the total amount of the composition, or any ranges formed by selecting any two contents mentioned above as the two limits, for example, the content of the solvent may be 2 to 30, or 5 to 20 percent by weight based on the total amount of the composition. Preferably, the content of the solvent may be 9 to 16 percent by weight based on the total amount of the composition. More preferably, the content of the solvent may be 10 to 12 percent by weight based on the total amount of the composition. For example, the content of the solvent may be 11 or 11.1 percent by weight based on the total amount of the composition.
The composition may optionally comprise one or more additives selected from the group consisting of thickener, dispersant, wetting agent, emulsifier, antifreeze, antifoam, and bactericide. When the additives are present, the content of all the additives in the composition may be 3 to 70 percent by weight based on the total amount of the composition. Within the range of 3 to 70 percent by weight based on the total amount of the composition, the content of all the additives may be 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 21.1, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, 50, 51, 52, 53, 54, 55, 56, 57, 58, 59, 60, 61, 62, 63, 64, 65, 66, 67, 68, 69, or 70 percent by weight based on the total amount of the composition, or any ranges formed by selecting any two contents mentioned above as the two limits, for example, the content of all the additives may be 3 to 60, or 6 to 50 percent by weight based on the total amount of the composition. Preferably, the content of all the additives may be 10 to 42 percent by weight based on the total amount of the composition. More preferably, the content of all the additives may be 15 to 33 percent by weight based on  the total amount of the composition. More preferably, the content of all the additives may be 18 to 28 percent by weight based on the total amount of the composition. More preferably, the content of all the additives may be 20 to 23 percent by weight based on the total amount of the composition. For example, the content of all the additives may be 21.1 percent by weight based on the total amount of the composition.
As the thickener, any thickeners that are generally used in the agrochemical field, especially herbicidal field to increase the viscosity of the composition may be used. In one embodiment, the thickener may be inorganic clays, organoclays, fumed and precipitated silica, organo modified bentonite, microcrystalline cellulose, xanthan gum, polyamides, hydrogenated caster oils, EO/PO block co-polymers, etc. Preferably, the thickener is xanthan gum. Fumed and precipitated silica may be hydrophobic and hydrophilic silica and any combination thereof. Examples of fumed silica may include but are not limited to
Figure PCTCN2022118727-appb-000004
A200, 
Figure PCTCN2022118727-appb-000005
R 202, 
Figure PCTCN2022118727-appb-000006
R 972 and
Figure PCTCN2022118727-appb-000007
R 805 (all available from Evonik) . Examples of precipitated silica may include but are not limited to
Figure PCTCN2022118727-appb-000008
22S (available from Evonik) , 
Figure PCTCN2022118727-appb-000009
D17 (available from Evonik) and
Figure PCTCN2022118727-appb-000010
38 (available from Rhodia Operations, a member of the Solvay Group) . An example of organo modified bentonite is 
Figure PCTCN2022118727-appb-000011
SD-1 (available from Elementis Specialties) . An example of inorganic clays is
Figure PCTCN2022118727-appb-000012
40 (available from BASF) . An example of xanthan gum is AG RH 23 (available from Ametech srl) . When present, the content of the thickener in the composition may be selected based on the nature of the thickener, the required viscosity of the composition and the cost. When present, the content of the thickener in the composition may be 0.005 to 0.5 percent by weight based on the total amount of the composition. Preferably, when present, the content of the thickener in the composition may be 0.01 to 0.1 percent by weight based on the total amount of the composition. Preferably, when present, the content of the thickener in the composition may be 0.02 to 0.06 percent by weight based on the total amount of the composition. Preferably, when present, the content of the thickener in the composition may be 0.03 to 0.05 percent by weight based on the total amount of the composition. For example, when present, the content of the thickener in the composition may be 0.04 percent by weight based on the total amount of the composition.
As the dispersant, any dispersants that are generally used in the agrochemical field, especially herbicidal field to prevent the aggregation of solid particles in the  solid-liquid dispersion system and keep them uniformly dispersed in the liquid phase for a long time may be used. In one embodiment, the dispersant may be alkylarylsulfonate salts, such as calcium dodecylbenzenesulfonate; alkylphenol-alkylene oxide addition products, such as nonylphenol-C 18ethoxylate; soaps, such as sodium stearate; alkylnaphthalene-sulfonate salts and condensates, such as sodium dibutyl-naphthalenesulfonate; dialkyl esters of sulfosuccinate salts, such as sodium di (2-ethylhexyl) sulfosuccinate; quaternary amines, such as lauryl trimethylammonium chloride; alkyl amines, such as tallow amine or derivatives thereof; block copolymers of ethylene oxide and propylene oxide; acrylic copolymers grafted with polyethylene oxide side chains; amphoteric polymers; comb polymers such as polyvinylpyrrolidinones or polyacrylates; a polymeric dispersant (such as Geropon MAI from Solvay) ; and salts of mono and dialkyl phosphate esters; polyethylene glycol alkyl/aryl ethers, and a combination of thereof. Preferably, the dispersant is a combination of two different dispersants, for example, a combination of block copolymers of ethylene oxide and propylene oxide with comb polymers such as polyvinylpyrrolidinones or polyacrylates or with a polymeric dispersant (such as Geropon MAI available from Solvay or Rhodia) . More preferably, the dispersant is a combination of block copolymers of ethylene oxide and propylene oxide (such as, ETHYLAN TM NS-500LQ available from AKZO NOBEL SURFACE CHEMISTRY LLC. or TERMUL 5500 available from HUNTSMAN INTERNATIONAL LLC) with comb polymers (such as polyvinylpyrrolidinones or polyacrylates, e.g., Atlox 4913-LQ- (MV) available from Croda Europe Limited, or Agrilan 755 available from AKZO NOBEL SURFACE CHEMISTRY LLC) , or a combination of block copolymers of ethylene oxide and propylene oxide (such as, ETHYLAN TM NS-500LQ available from AzokNobel) with a polymeric dispersant (such as Geropon MAI available from Solvay) . In one embodiment, the dispersant is a combination of block copolymers of ethylene oxide and propylene oxide (such as, TERMUL 5500 available from HUNTSMAN INTERNATIONAL LLC) with a polyacrylate comb polymer (such as Agrilan 755 available from AKZO NOBEL SURFACE CHEMISTRY LLC) . In one embodiment, the dispersant is a combination of block copolymers of ethylene oxide and propylene oxide (such as, ETHYLAN TM NS-500LQ available from AzokNobel) with a polymeric dispersant (such as Geropon MAI available from Solvay) . If present, the content of all the dispersants in the composition may be selected based on the nature of the dispersant, the required  properties of the composition and cost. When present, the content of all the dispersants in the composition may be 0.2 to 20 percent by weight based on the total amount of the composition. Preferably, when present, the content of all the dispersants in the composition may be 0.1 to 12 percent by weight based on the total amount of the composition. Preferably, when present, the content of all the dispersants in the composition may be 0.2 to 6 percent by weight based on the total amount of the composition. Preferably, when present, the content of all the dispersants in the composition may be 0.5 to 5 percent by weight based on the total amount of the composition. Preferably, when present, the content of all the dispersants in the composition may be 1 to 3 percent by weight based on the total amount of the composition. For example, when present, the content of all the dispersants in the composition may be 2 percent by weight based on the total amount of the composition. When present, the content of each dispersant in the composition may be 0.1 to 10 percent by weight based on the total amount of the composition. Preferably, when present, the content of each dispersant in the composition may be 0.2 to 4 percent by weight based on the total amount of the composition. Preferably, when present, the content of each dispersant in the composition may be 0.5 to 2 percent by weight based on the total amount of the composition. Preferably, when present, the content of each dispersant in the composition may be 0.8 to 1.2 percent by weight based on the total amount of the composition. For example, when present, the content of each dispersant in the composition may independently be 0.5, 1, or 1.5 percent by weight based on the total amount of the composition.
As the wetting agent, any wetting agents that are generally used in the agrochemical field, especially herbicidal field to reduce the surface tension between the solid surface and water surface and make solid materials more easily wetted by water may be used. In one embodiment, the wetting agent may be anionic or nonionic surfactants. Anionic surfactants include alkyl sulfates, sulfonates, fatty acid or fatty acid ester sulfates, carboxylic acid soaps, phosphate esters, and the like. Nonionic surfactants include polyoxyethylene alkylphenol ethers, polyoxyethylene fatty alcohol ethers, polyoxyethylene polyoxypropylene block copolymers and the like. Preferably, the wetting agent is selected from nonionic surfactants, especially polyoxyethylene polyoxypropylene block copolymers. If present, the content of the wetting agent in the composition may be selected based on the nature of the wetting agent, the required properties of the composition and cost. When present, the content of the wetting  agents in the composition may be 0.05 to 5 percent by weight based on the total amount of the composition. Preferably, when present, the content of wetting agents in the composition may be 0.08 to 3 percent by weight based on the total amount of the composition. Preferably, when present, the content of the wetting agents in the composition may be 0.1 to 2 percent by weight based on the total amount of the composition. Preferably, when present, the content of the wetting agents in the composition may be 0.2 to 1 percent by weight based on the total amount of the composition. Preferably, when present, the content of the wetting agents in the composition may be 0.3 to 0.8 percent by weight based on the total amount of the composition. Preferably, when present, the content of the wetting agents in the composition may be 0.4 to 0.6 percent by weight based on the total amount of the composition. For example, when present, the content of the wetting agents in the composition may be 0.5 percent by weight based on the total amount of the composition.
As the emulsifier, any emulsifiers that are generally used in the agrochemical field, especially herbicidal field to reduce surface tension and interfacial tension, reduce emulsification energy, and reduce surface free energy to form a stable emulsion may be used. In one embodiment, the emulsifier may be salt (e.g. an alkaline earth metal salt, e.g. a calcium salt) of a C 1-C 22 alkyl-phenyl-sulfonate (e.g. a salt of a C 8-C 18alkyl-phenylsulfonate) , such as calcium dodecylbenzenesulfonate; a castor oil-alkylene oxide addition product (condensation product) , in particular castor oil ethoxylate which can for example have varying amounts of ethoxylation, e.g. a castor oil ethoxylate (e.g., 20 to 50 EO) (i.e. containing and/or produced using 20 to 50 moles of ethylene oxide (EO) per mole of castor oil) , for example Surfom R 200 available from OXITENO NORDESTE SA INDUSTRIA E COMERCIO; a polyalkylene glycol ether, especially, a polyethylene glycol ether, for example, polyethylene glycol mono (tristyrylphenyl) ethers (Tristyrylphenol ethoxylates, e.g., Soprophor BSU available from SOLVAY SOLUTIONS ITALIA S. P. A. or Surfom CE 1299 available from OXITENO NORDESTE SA INDUSTRIA E COMERCIO) ; an alcohol-alkylene oxide addition product (condensation product) , such as tridecyl alcohol ethoxylate; an alkylphenol-alkylene oxide addition product (condensation product) , such as nonylphenol ethoxylate; a di C 1-C 22 alkyl ester of a sulfosuccinate salt, such as sodium di (2-ethylhexyl) sulfosuccinate; a sorbitol ester, such as sorbitol oleate; a polyethylene glycol ester of a C 8-C 22 fatty acid, such as polyethylene glycol  stearate; a block copolymer of ethylene oxide (EO) and propylene oxide (PO) ; an ethylene oxide (EO) /propylene oxide (PO) copolymer, such as Atlas G-5000 TM EO/PO copolymer (e.g. available from Croda) ; or a salt of a mono-and/or di-alkyl phosphate ester; a tristyrylphenol alkoxylate such as a tristyrylphenol ethoxylate and/or a tristyrylphenol ethoxylate-propoxylate, more particularly a tristyrylphenol ethoxylate containing 8 to 30 (preferably 10 to 25) moles of ethylene oxide (EO) per mole of tristyrylphenol, such as Soprophor TS/10 TM (10 moles EO) , Soprophor BSU TM (16 moles EO) , or Soprophor S/25 TM (25 moles EO) , for example available from Solvay Solutions Nederland B.V.; or a mixture of two or more of these emulsifiers. In one embodiment, a combination of two or more emulsifiers may be used in the composition. For example, a combination of a castor oil-alkylene oxide addition product and a polyethylene glycol ether may be used in the composition as the emulsifiers. In one embodiment, a combination of a castor oil ethoxylate and a polyethylene glycol mono (tristyrylphenyl) ether is used in the composition as the emulsifiers. If present, the content of the emulsifiers in the composition may be selected based on the nature of the emulsifiers, the required properties of the composition and cost. When present, the content of all the emulsifiers in the composition may be 0.5 to 30 percent by weight based on the total amount of the composition. Preferably, when present, the content of all the emulsifiers in the composition may be 1 to 20 percent by weight based on the total amount of the composition. Preferably, when present, the content of all the emulsifiers in the composition may be 2 to 15 percent by weight based on the total amount of the composition. Preferably, when present, the content of all the emulsifiers in the composition may be 4 to 9 percent by weight based on the total amount of the composition. Preferably, when present, the content of all the emulsifiers in the composition may be 5 to 8 percent by weight based on the total amount of the composition. For example, when present, the content of all the emulsifiers in the composition may be 6 percent by weight based on the total amount of the composition. When present, the content of each emulsifier in the composition may be 0.1 to 10 percent by weight based on the total amount of the composition. Preferably, when present, the content of each emulsifier in the composition may be 0.2 to 7 percent by weight based on the total amount of the composition. Preferably, when present, the content of each emulsifier in the composition may be 0.3 to 6 percent by weight based on the total amount of the composition. Preferably, when present, the content of each  emulsifier in the composition may be 0.5 to 5 percent by weight based on the total amount of the composition. For example, when present, the content of each emulsifier in the composition may independently be 2 or 4 percent by weight based on the total amount of the composition.
As the antifreeze, any antifreezes that are generally used in the agrochemical field, especially herbicidal field to increase flowability at low temperature may be used. In one embodiment, the antifreeze may be alcohol or phenols, for example ethylene glycol, 1, 2-propylene glycol, 1, 3-propylene glycol, 1, 2-butanediol, 1, 3-butanediol, 1, 4-butanediol, 1, 4-pentanediol, 3-methyl-1, 5-pentanediol, 2, 3-dimethyl-2, 3-butanediol, trimethylol propane, mannitol, sorbitol, glycerol, pentaerythritol, 1, 4-cyclohexanedimethanol, xylenol, bisphenols such as bisphenol A, urea or the like; ether alcohols such as diethylene glycol, triethylene glycol, tetraethylene glycol, polyoxyethylene or polyoxypropylene glycols of molecular weight up to about 4000, diethylene glycol monomethylether, diethylene glycol monoethylether, triethylene glycol monomethylether, butoxyethanol, butylene glycol monobutylether, dipentaerythritol, tripentaerythritol, tetrapentaerythritol, diglycerol, triglycerol, tetraglycerol, pentaglycerol, hexaglycerol, heptaglycerol, octaglycerol and the like, and the combination thereof. Preferably, the antifreeze may be alcohol, for example ethylene glycol, 1, 2-propylene glycol, 1, 3-propylene glycol, 1, 2-butanediol, 1, 3-butanediol, 1, 4-butanediol, 1, 4-pentanediol, 3-methyl-1, 5-pentanediol, 2, 3-dimethyl-2, 3-butanediol, trimethylol propane, mannitol, sorbitol, glycerol, pentaerythritol, 1, 4-cyclohexanedimethanol, especially ethylene glycol. If present, the content of the antifreeze in the composition may be selected based on the nature of the antifreeze, the required properties of the composition and cost. When present, the content of the antifreeze in the composition may be 0.1 to 30 percent by weight based on the total amount of the composition. Preferably, when present, the content of the antifreeze in the composition may be 0.3 to 20 percent by weight based on the total amount of the composition. Preferably, when present, the content of the antifreeze in the composition may be 0.6 to 10 percent by weight based on the total amount of the composition. Preferably, when present, the content of the antifreeze in the composition may be 0.8 to 6 percent by weight based on the total amount of the composition. Preferably, when present, the content of the antifreeze in the composition may be 1 to 4 percent by weight based on the total amount of the  composition. For example, when present, the content of the antifreeze in the composition may be 2 percent by weight based on the total amount of the composition.
As the bactericide, any bactericides that are generally used in the agrochemical field, especially herbicidal field to control molds and bacteria may be used. In one embodiment, the bactericide may be isothiazolinone compound, especially, benzisothiazolinone, such as, 2-methyl-4-isothiazolin-3-one, 5-chloro-2-methyl-4-isothiazolin-3-one, 1, 2-benzisothiazolin-3-one and the like, sulphur (wettable sulphur) , copper preparations, benzimidazole, bitertanol, dichlofluanid, fenamidone, fenarimol, fenhexamid, fludioxonil, fluopyram, fosetyl-aluminium, iprodione, myclobutanil, penconazole, triadimenol, vinclozolin, tolylfluanid (Euparen
Figure PCTCN2022118727-appb-000013
) , eaptan, propineb, tebuconazol trifloxystrobin, kresoxim-methyl, dithianon, cyprodinil, pyrimethanil, mancozeb (Dithane
Figure PCTCN2022118727-appb-000014
) and metiram; and the combination thereof. Preferably, the bactericide may be isothiazolinone compound, especially, benzisothiazolinone, such as, 2-methyl-4-isothiazolin-3-one, 5-chloro-2-methyl-4-isothiazolin-3-one, 1, 2-benzisothiazolin-3-one and the like, especially 1, 2-benzisothiazolin-3-one. If present, the content of the bactericide in the composition may be selected based on the nature of the bactericide, the required properties of the composition and cost. When present, the content of the bactericide in the composition may be 0.005 to 1 percent by weight based on the total amount of the composition. Preferably, when present, the content of the bactericide in the composition may be 0.002 to 0.5 percent by weight based on the total amount of the composition. Preferably, when present, the content of the bactericide in the composition may be 0.01 to 0.1 percent by weight based on the total amount of the composition. Preferably, when present, the content of the bactericide in the composition may be 0.03 to 0.05 percent by weight based on the total amount of the composition. For example, when present, the content of the bactericide in the composition may be 0.04 percent by weight based on the total amount of the composition.
As the antifoam, any antifoams that are generally used in the agrochemical field, especially herbicidal field to reduce the formation of foams upon dilution may be used. In one embodiment, the antifoam may be silica, a poly organosiloxane, polydialkylsiloxanes, in particular polydimethylsiloxanes, fluoroaliphatic esters or perfluoroalkylphosphonic/perfluoroalkylphosphonic acids or the salts thereof; and the combination thereof. Preferably, the antifoam is a poly organosiloxane, for example Silcolapse 432 available from Elkem Silicones (UK) Ltd or Silcolapse C565 available  from BLUESTAR SILICONES SHANGHAI CO LTD. If present, the content of the antifoam in the composition may be selected based on the nature of the antifoam, the required properties of the composition and cost. When present, the content of the antifoam in the composition may be 0.002 to 0.2 percent by weight based on the total amount of the composition. Preferably, when present, the content of the antifoam in the composition may be 0.005 to 0.12 percent by weight based on the total amount of the composition. Preferably, when present, the content of the antifoam in the composition may be 0.008 to 0.06 percent by weight based on the total amount of the composition. Preferably, when present, the content of the antifoam in the composition may be 0.01 to 0.03 percent by weight based on the total amount of the composition. For example, when present, the content of the antifoam in the composition may be 0.02 percent by weight based on the total amount of the composition.
As easily understood by the skills, the composition may comprise other components in addition to those mentioned before, e.g., any impurities brought in along with the active components. As easily understood by the skills, the sum of all the components in the composition should be 100 percent by weight based on the total amount of the composition.
The stable agrochemical composition of this disclosure may be any stable agrochemical compositions, such as, a stable herbicidal composition, a stable insecticidal composition, a stable pesticidal composition, a stable fungicidal composition, a stable bactericidal composition, and the like. In one embodiment, the stable agrochemical composition of this disclosure is a stable herbicidal composition. The stable agrochemical composition of this disclosure may be in any forms, such as a dispersion, a suspo-emulsion (SE) , and the like.
Generally, the stable composition of this disclosure may include particles, in some cases may include different types of particles. For example, when the stable composition is a SE, at least two types of particle are present which are solid particles and liquid oil particles, and at least three phases are present which include a suspension phase formed by the solid particles suspended, an emulsion phase formed by the liquid oil particles, and a continuous phase formed by water. In this case, the solid particles in the suspension phase are the solid particles of the first solid active component suspended in water, and the liquid oil particles in the emulsion phase are formed by the second active component dissolved in the third active component and the organic solvent. In one embodiment, the stable composition is a SE, and include  solid particles formed by the first active component and liquid oil particles formed by the second active component dissolved in the third active component and the organic solvent, and the mean particle size d90 may be <15 μm, preferably may be <7 μm, based on all particles. In the embodiment, the solid particles may have a mean particle size d90 of <15 μm, preferably a mean particle size d90 of <7 μm, and the liquid oil particles may have a mean particle size d90 of <5μm, preferably a mean particle size d90 of <2 μm. The mean particle size d90 may be measured by a laser diffractometer or microscope. Sometimes, as easily understood by the skills, there are two phases, an oil phase and an aqueous phase in the composition e.g. SE. The first active component, water and some additives like antifoams, thickener, and antifreeze are present in the aqueous phase, while the second and third active components, the organic solvent and other additives are present in the oil phase. In one embodiment, in the composition e.g. SE, the content of the oil phase (the sum of the second and third active components, the organic solvent and any additives used therein) is at least 30 percent by weight based on the total amount of the composition, preferably at least 40 percent by weight based on the total amount of the composition, preferably at least 50 percent by weight based on the total amount of the composition, preferably at least 60 percent by weight based on the total amount of the composition.
The compositions of the present disclosure have a superior stability and can satisfy the following stability requirements set forth for suspo-emulsion (SE) as recited in NY/T 2989-2016 (Guidelines on developing the specifications of pesticides for registration) : appearance, wet sieve test, dispersion stability, low temperature stability, and heat storage stability. The specification for all these stability requirements are given in the Example part. For example, among others, the compositions of the present disclosure have a superior dispersion stability, which for example may be measured by CIPAC MT 180 “Dispersion Stability of Suspo-Emulsion. ” In one embodiment, the compositions of this disclosure can be stable at 54 ℃ for at least 2 weeks measured by CIPAC MT 180. In one embodiment, the compositions of the disclosure can be stable at room temperature for at least 2 years measured by CIPAC MT 180.
Second Aspect
In the second aspect, the present disclosure provides a process for preparing the stable agrochemical composition described in the first aspect which comprises the steps of:
a) forming a suspension concentrate (SC) of the first active component,
b) forming an emulsifiable concentrate (EC) of the second active component and the third active component; and
c) mixing the SC with the EC and other optional ingredients.
It has now also been found that, especially when (1) the first active component is insoluble in either water or the third active component at room temperature, and (2) the second solid active components has a solubility in the liquid third active component of from 1 to 33 g/100g at room temperature, a stable agrochemical composition comprising two solid active components and one liquid active component, especially a stable SE comprising two solid active components and one liquid active component can be successfully prepared from combining EC with SC by carefully selecting the active components in each of EC and SC. Specifically, the inventors of the present disclosure surprisingly found that, the stable agrochemical composition, especially the stable SE can be formulated successfully only if a suspension concentrate (SC) of the first active component is mixed with an emulsifiable concentrate (EC) of the second active component and the third active component when the content of the oil phase (the sum of the second and third active components, the organic solvent and other optional additives used therein) is at least 30 percent by weight based on the total amount of the composition, preferably at least 40 percent by weight based on the total amount of the composition, preferably at least 50 percent by weight based on the total amount of the composition, preferably at least 60 percent by weight based on the total amount of the composition. More specifically, the inventors of the present disclosure surprisingly found that if the second active component is added to SC along with the first active component, no matter what the third active component is formulated into (for example into a EC or a EW) , a stable agrochemical composition, especially a stable SE can not be formulated successfully. The inventors of the present disclosure also surprisingly found that if the second active component is formulated together with the third active component into a EW, even if the first active component is formulated into a SC, a stable agrochemical composition, especially a stable SE can not be formulated successfully especially when the content of the oil phase (the sum of the second and third active components,  the organic solvent and any optional additives) is at least 30 percent by weight based on the total amount of the composition, preferably at least 40 percent by weight based on the total amount of the composition, preferably at least 50 percent by weight based on the total amount of the composition, preferably at least 60 percent by weight based on the total amount of the composition.
The step a) may comprise mixing the first active component, a first portion of water, and other optional additives to form a homogeneous suspension. The other optional additives that may be used in the step a) may include but are not limited to antifreezes, antifoams, dispersants, other possible surfactants, and the combination thereof. Homogeneous suspension can be determined by visual assessment of appearance, active component content analysis of different spot of a sample, and/or microscope test of different spot of a sample. The mixing may be carried out by any means in the art, such as a mixer. The mixing time is selected based on the nature and amount of the first active component, the nature and amount of other optional additives, and their relative amounts as compared to water. Generally, the mixing time may be from 5 min to 60 min depending on e.g., the total amount of the materials. The amount of the first portion of water may be determined by the minimum amount of water required for successfully dispersing the first active component and the total amount of the water used in the composition.
The step a) may further comprise milling the obtained suspension until a desirable mean particle size is obtained, for example until a mean particle size d90 ≤ 15 μm, preferably ≤7 μm, more preferably ≤5 μm is obtained. The milling may be conducted by any suitable machines in the art, for example NETZSCH MINIZETA. As mentioned in the first aspect, the mean particle size may be measured by any conventional method in the art, for example laser particle size analyzer Malvern MS3000. The milling time may be determined by the desirable mean particle size, the machine used for milling and the total amount of the materials. Generally, the milling time may be from 5 min to 60 min depending on e.g., the total amount of the materials and the desired particle size.
The step b) may comprise mixing the second and third active components, the organic solvent, and other optional additives to form a clear liquid. The other optional additives may include but are not limited to wetting agents, emulsifiers, bactericides, other possible surfactants, and the combination thereof. The mixing may be  conducted by any means in the art, such as a mixer. The mixing time may be selected based on the nature and amount of the second and third active components, the nature and amount of other optional additives, and their relative amounts as compared to the organic solvent, etc. Generally, the mixing time may be from 5 min to 30 min depending on e.g., the total amount of the materials.
The mixing in step b) may be conducted under heating for facilitating the dissolution. Heating is optional. The heating may be conducted by any means in the art, for example a magnetic stirring heater. The heating temperature is generally from 30 ℃ to the boiling point of the organic solvent, preferably 30 to 80 ℃, more preferably 40 to 60 ℃, e.g., 50℃. The heating time may be the same as, longer or shorter than the mixing time. Generally, the heating time may be from 5 min to 60 min depending on e.g., the total amount of the materials.
As easily understood by the skills, the order of step a) and step b) is not important. Therefore, step a) may be conducted before, after, or at the same time as step b) .
In step c) , the mixing of the SC with the EC and other optional ingredients may be conducted by any means in the art, such as a mixer. The other optional ingredients may include but are not limited to the second portion of water, thickener, other possible surfactants, and the combination thereof. The amount of the second portion of water is decided by the first portion of water and the total amount of water. Generally, the mixing time may be from 5 min to 30 min depending on e.g., the total amount of the materials.
In step c) , the mixing of the SC with EC and other optional ingredients may be conducted under a shear (e.g., at 500 to 100000 rpm, for example 1000 to 80000 rpm, especially 2000 to 40000 rpm, more specifically 12000 to 20000 rpm) to obtain a mean particle size d90 ≤15 μm, preferably a mean particle size d90 ≤7 μm, more preferably a mean particle size d90 ≤5 μm based on all particles of all types. As mentioned in the first aspect, the mean particle size may be measured by any conventional method in the art, for example laser particle size analyzer Malvern MS3000. The shear may be accomplished by any means conventional in the art, such as a high shear machine. Generally, the shear time may be the same or shorter than the mixing time. Generally, the shear time may be from 5 min to 30 min depending on e.g., the total amount of the materials and the desired particle size.
When the composition comprises a thickener, depending on the amount of the thickener and actual requirements, the thickener may be added in step a) , step c) and/or an optional step d) . In one embodiment, when the composition comprises a thickener, the step c) , i.e., the mixing of the SC with EC and other optional ingredients, may comprise c1) mixing the SC with a part of or all of the thickener to form a homogeneous suspension, and c2) mixing the suspension obtained in c1) with the EC. In this case, except for the thickener, the remaining other optional ingredients (e.g., the second portion of water, and other possible additives) may be all added in c1) or c2) . It is also possible that some of the remaining other optional ingredients are added in c1) , and the others are added in c2) . In another embodiment, when the composition comprises a thickener, the process may further comprise a step d) : mixing the dispersion obtained in step c) with a part of or all of the thickener. The mixing may be conducted by any means in the art, such as a mixer. Generally, the mixing time may be from 5 min to 60 min depending on e.g., the total amount of the materials.
In the present disclosure, unless otherwise indicated, all the specific descriptions made in the first aspect apply to the second aspect as all relevant descriptions have been copied here. For example, unless otherwise indicated, all the specific descriptions on the stable agrochemical compositions, the first, second and third active components, their contents in the composition and relative amount compared to each other, organic solvent and its content, the possible additives (thickener, dispersant, wetting agent, emulsifier, antifreeze, antifoam, and bactericide) and their contents in the first aspect apply to the second aspect as all relevant specific descriptions have been copied here.
Third Aspect
In the third aspect, the present disclosure provides a stable agrochemical composition prepared by a process comprise the steps of:
a) forming a SC of a first active component;
b) forming an EC of a second active component and a third active component; and
c) mixing the SC with the EC and other optional ingredients;
wherein the first active component is solid at room temperature and insoluble in water at room temperature, the second active component is solid at room temperature, and the third active component is liquid at room temperature; and
the first active component is insoluble in the third active component at room temperature, and the second active component has a solubility in the third active component of from 1 to 33 g/100g at room temperature.
As mentioned in the second aspect, it has now been found that, a stable agrochemical composition comprising first and second solid active components and a liquid third active component, especially a stable SE comprising these two solid active components and the liquid active component can be successfully prepared from combining EC with SC by carefully selecting the active components in each of EC and SC especially when (1) the first active component is insoluble in both water and the third active component, and (2) the second solid active components has a solubility in the liquid active component of from 1 to 33 g/100g at room temperature. Specifically, the inventors of the present disclosure surprisingly found that, a stable agrochemical composition, especially a stable SE can be formulated successfully only if a suspension concentrate (SC) of the first active component is mixed with an emulsifiable concentrate (EC) of the second active component and the third active component, especially when the content of the oil phase (the sum of the second and third active components, the organic solvent and any optional additives used therein) is at least 30 percent by weight based on the total amount of the composition, preferably at least 40 percent by weight based on the total amount of the composition, preferably at least 50 percent by weight based on the total amount of the composition, preferably at least 60 percent by weight based on the total amount of the composition. More specifically, the inventors of the present disclosure surprisingly found that if the second active component is added to SC along with the first active component, no matter what dosage form the third active component is formulated into (for example into a EC or a EW) , a stable agrochemical composition, especially a stable SE can not be formulated successfully. The inventors of the present disclosure also surprisingly found that if the second active component is formulated together with the third active component into a EW, even if the first active component is formulated into SC, a stable agrochemical composition, especially a stable SE can not be formulated successfully especially when the content of the oil phase (the sum of the second and third active components, the organic solvent and any optional additives used therein)  is at least 30 percent by weight based on the total amount of the composition, preferably at least 40 percent by weight based on the total amount of the composition, preferably at least 50 percent by weight based on the total amount of the composition, preferably at least 60 percent by weight based on the total amount of the composition.
In the present disclosure, unless otherwise indicated, all the specific descriptions made in the first and second aspects apply to the third aspect as all relevant descriptions have been copied here. For example, unless otherwise indicated, all the specific descriptions on the stable agrochemical compositions, the first, second and third active components, their contents in the composition and relative amount compared to each other, organic solvent and its content, the possible additives (thickener, dispersant, wetting agent, emulsifier, antifreeze, antifoam, and bactericide) and their contents in the first aspect apply to the third aspect as all relevant descriptions have been copied here, and unless otherwise indicated, all the specific descriptions on the steps a) , b) , c) , c1) , c2) and d) in the second aspect apply to the third aspect as all relevant descriptions have been copied here.
Each embodiment disclosed herein is contemplated as being applicable to each of the other disclosed embodiments. Thus, all combinations of the various elements described herein are within the scope of the disclosure. In addition, the elements recited in process embodiments can be used in combination with compound embodiments described herein and vice versa.
This disclosure will be better understood by reference to the Examples which follow, but those skilled in the art will readily appreciate that the specific experiments detailed are only illustrative of the disclosure as described more fully in the claims which follow thereafter.
The disclosure is illustrated by the following examples without limiting it thereby.
EXAMPLES
Test Methods
1. Appearance is measured by visual evaluation.
2. Wet sieve test is measured according to CIPAC MT 185 “Wet Sieve Test. ”
3. Dispersion stability is measured according to CIPAC MT 180 “Dispersion Stability of Suspo-Emulsion” at a specified temperature.
4. Low temperature stability is measured according to CIPAC MT 39.3 “Stability of Liquid Formulations at 0 ℃” for a defined period of time.
5. Heat storage stability is measured according to CIPAC MT 46.3 “Accelerated Storage Procedure” at a specified temperature for a defined period of time.
6. Mean Particle size d90 is measured by laser particle size analyzer Malvern MS3000 according to CIPAC MT 187.
The specifications for the relevant tests in the Examples are listed in Table 1.
Table 1. The specifications
Figure PCTCN2022118727-appb-000015
1Heat storage stability
2Low temperature stability
7. The solubility a material in Pretilachlor at a specified temperature is measured as follows:
10g of the material is added into a beaker, then 10g of pretilachlor is added. The resulting mixture is stirred in a magnetic stirrer for 1 hour while keeping the temperature at the specified temperature, the supernatant is taken, and the content of the material in the supernatant is measured as the saturated solubility at the specified temperature, given in a unit of g/100g.
Comparative Example (CE) 1
I. An EC1 was formulated in this CE1 as follows:
i) . The solvent S-150 ND, Pretilachlor tech, and emulsifiers as shown in Table 2 were added gradually in the amount as shown in Table 2 to a reactor under mixing; and
ii) . The mixture in the reactor was heated to about 50 ℃ and mixed at the same temperature until the liquid was clear.
Table 2: Formulating an EC of Pretilachlor
Figure PCTCN2022118727-appb-000016
II. A SC1 was formulated in this CE 1 as follows:
i) . The water and Propylene glycol were added at the amount indicated in Table 3 to a reactor and mixing was started;
ii) . Silcolapse C565, Penoxsulam tech, Fenclorim tech, dispersants, and other materials as shown in Table 3 were added in the amount as shown in Table 3 to the reactor, and mixing was continued until the suspension was homogeneous;
iii) . The suspension was milled in a bead mill until a mean particle size d90 <5 μm was obtained as measured by laser particle size analyzer Malvern MS3000.
Table 3: Formulating a SC of Penoxsulam and Fenclorim
Figure PCTCN2022118727-appb-000017
3: AG RH 23 was added in a 2%by weight aqueous solution, and the water used for AG RH 23 was accounted for the total amount 34.8g. The same applied to other CEs and Examples.
III. A SE1 was formulated as follows:
EC1 obtained in I was added to SC1 obtained in II, the resulting mixture was mixed evenly. Then, the resulting material was sheared in a high shear machine IKA RW 20 digital at a 15000 to 20000rpm until a mean particle size d90 based on all  particles of all types <2 μm was obtained as measured by laser particle size analyzer Malvern MS3000 to obtain a white-like uniform sample.
IV. Test
The SE1 was tested for Heat storage stability at 54 ℃ according to the method mentioned before. A phenomenon of delamination and precipitation was clearly observed at 14 days in the test.
CE2
I. An EW1 was formulated in this CE2 as follows:
i) . The solvent S-150 ND, Pretilachlor tech, and emulsifiers as shown in Table 4 were added gradually in the amount as shown in Table 4 to a reactor; and
ii) . The mixture obtained in i) was mixed uniformly at room temperature, and was added into water in the amount as shown in Table 4 in another reactor, and sheared at 12000 to 15000rpm at the same temperature in a high shear machine resulting in an oily mixture rather than an uniform white emulsion.
Table 4: Formulating an EW of Pretilachlor
Figure PCTCN2022118727-appb-000018
In order to figure out the possibility of formulating an uniform white emulsion, a second batch of EW1 was formulated in the same way as I, and the obtained oily mixture was added with another 14.8g water (which was intended for formulating SC as mentioned below) and sheared at 12000 to 15000rpm at room temperature. However, the resulting mixture was still oily.
II. A SC2 was formulated by repeating the procedure in CE1 for formulating SC1 with the exception that the amount of water was reduced to 14.8 g.
III. ASE2 was formulated as follows:
EW1 obtained in I was added to SC2 obtained in II, the resulting mixture was mixed evenly. Then, the resulting material was sheared in a high shear machine IKA RW 20 digital at a 15000 to 20000rpm until a mean particle size d90 <2 μm based on all particles of all types was obtained as measured by laser particle size analyzer Malvern MS3000 to obtain a white-like sample with oily droplets on the edge.
IV. Test
The SE2 was tested for Heat storage stability at 54 ℃according to the method mentioned before. A phenomenon of delamination and precipitation was clearly observed at 14 days in the test.
CE 3
I.An EW2 was formulated in this CE3 as follows:
i) . The solvent S-150 ND, Pretilachlor tech, Fenclorim tech, and emulsifiers as shown in Table 5 were added gradually in the amount as shown in Table 5 to a reactor under mixing; and
ii) . The mixture in the reactor was mixed uniformly at room temperature, and was added into water in the amount as shown in Table 5 in another reactor, and sheared at 12000 to 15000rpm at the same temperature resulting in an oily mixture rather than an uniform white emulsion.
Table 5: Formulating an EW of Pretilachlor and Fenclorim
Figure PCTCN2022118727-appb-000019
In order to figure out the possibility of formulating an uniform white emulsion, a second batch of EW2 was formulated in the same way as I, and the obtained oily mixture was added with another 14.8g water (which was intended for formulating SC as mentioned after) and sheared at 12000 to 15000rpm at room temperature. However the resulting mixture was still oily.
II. A SC3 was formulated by repeating the procedure in CE1 for formulating SC1 with the exception that (1) the amount of water was reduced to 14.8 g and (2) Fenclorim tech was not added.
III. A SE3 was formulated as follows:
EW2 obtained in I was added to SC3 obtained in II, the resulting mixture was mixed evenly. Then, the resulting material was sheared in a high shear machine IKA RW 20 digital at a 15000 to 20000rpm until a mean particle size d90 based on all particles of all types <2 μm was obtained as measured by laser particle size analyzer Malvern MS3000 to obtain a white-like sample with oily droplets on the edge.
IV. Test
The SE3 was tested for Heat storage stability at 54 ℃ according to the method mentioned before. A phenomenon of delamination and precipitation was clearly observed at 14 days in the test.
CE 4
I. A SE 4 was formulated as follows:
i) All materials as shown in Table 6 were added gradually in the amount as shown in Table 6 to a reactor and mixed uniformly; and
ii) The mixture obtained in i) was milled in a bead mill until a mean particle size d90<5 μm based on all particles was obtained as measured by laser particle size analyzer Malvern MS3000 to obtain a white-like sample.
Table 6: Formulating a SE directly
Figure PCTCN2022118727-appb-000020
II. Test
The SE4 was tested for Heat storage stability at 54 ℃ according to the method mentioned before. A phenomenon of delamination and precipitation was clearly observed at 14 days in the test.
SE1 to SE4 all failed in Heat storage stability test at 54 ℃. SE1 to SE4 demonstrated that if Fenclorim as the second active component is added to SC along with Penoxsulam as the first active component, no matter what dosage form Pretilachlor as the third active component is formulated into (a EC or a EW) , a stable SE can not be formulated successfully. SE1 to SE4 also demonstrated if Fenclorim as the second active component is formulated together with Pretilachlor as the third active component into a EW, even if Penoxsulam as the first active component is formulated into a SC, a stable SE can not be formulated successfully.
Example 1 (E1)
I. An EC2 was formulated in this E1 as follows:
i) . The solvent S-150 ND, Pretilachlor tech, Fenclorim tech, and emulsifiers as shown in Table 7 were added gradually in the amount as shown in Table 2 to a reactor under mixing; and
ii) . The mixture in the reactor was heated to about 50 ℃ and mixed at the same temperature until the liquid was clear.
Table 7: Formulating an EC of Pretilachlor and Fenclorim
Figure PCTCN2022118727-appb-000021
II. A SC5 was formulated in this E1 as follows:
i) . The water and Propylene glycol were added at the amount indicated in Table 8 to a reactor and mixing was started;
ii) . Silcolapse C565, Penoxsulam tech, dispersants, and other materials as shown in Table 8 were added in the amount as shown in Table 8 to the reactor, and mixing was continued until the suspension was homogeneous;
iii) . The suspension was milled in a bead mill until a mean particle size d90<5 μm was obtained as measured by laser particle size analyzer Malvern MS3000.
Table 8: Formulating a SC of Penoxsulam
Figure PCTCN2022118727-appb-000022
Figure PCTCN2022118727-appb-000023
III. A SE5 was formulated as follows:
EC2 obtained in I was added to SC5 obtained in II, the resulting mixture was mixed evenly. Then, the resulting material was sheared in a high shear machine IKA RW 20 digital at a 15000 to 20000rpm until a mean particle size d90 <2 μm based on all particles of all types was obtained as measured by laser particle size analyzer Malvern MS3000 to obtain a white-like uniform sample.
IV. Tests
The SE5 was tested for appearance, wet sieve test, dispersion stability, low temperature stability, and heat storage stability at 54 ℃ according to the methods mentioned before. SE5 passed all the tests. Specifically, SE5 maintained its dispersion stability after storing both at 0 ℃ for 7 days and at 54 ℃ for 14 days.
In consideration CE1 to CE4 and E1, it was demonstrated that a stable SE can be formulated successfully only if a SC of Penoxsulam as the first active component is mixed with an EC of Fenclorim as the second active component and Pretilachlor as the third active component.
The content of oil phase in CE1 to CE4 and E1 was the same, 58percent by weight.
V. Microscope Photograph
A microscope photograph was taken on the SE1 obtained in Example 1 using Microscope model BX53, OLYMPUS, which is shown in Fig. 1. In Fig. 1, two types of particles were shown, the solid particles formed by Penoxsulam (bright particles) , liquid oil particles formed by Fenclorim dissolved in Pretilachlor and the organic solvent (dark particles) . For illustration purpose, some of the particles were indicated in the blocks. Fig. 1 also showed the continuous phase formed by water, a part of which was also specifically indicated in the block. Although not specifically  indicated, the suspension phase formed by the solid particles suspended and the emulsion phase formed by the liquid oil particles were also clear from Fig. 1.
E2
I. Different SCs were formulated in this E2 as follows:
i) . The water and Propylene glycol were added at the amount indicated in Table 9 to a reactor and mixing was started;
ii) . Silcolapse 432, Penoxsulam tech, and corresponding dispersants as shown in Table 9 were added in the amount as shown in Table 9 to the reactor, and mixing was continued until the suspension was homogeneous;
iii) . The suspension was milled in a bead mill until mean particle size d90<5 μm was obtained as measured by laser particle size analyzer Malvern MS3000.
Figure PCTCN2022118727-appb-000024
In E2, SC6-9 were successfully formulated.
II. Six batches of EC2 was formulated in the same way as in I of E1.
III. SE6-9 were formulated by combining SC6-9 with each batch of EC2, respectively, according to the same procedure as mentioned in III of E1.
IV. Tests
The SE6-9 were tested for appearance, wet sieve test, dispersion stability, low temperature stability, and heat storage stability at 54 ℃ according to the methods mentioned before. Only SE6 and SE9 passed all the tests.
E3
Tests for solubility
1. The solubility Fenclorim in Pretilachlor at room temperature and 54 ℃ was tested according to the method as mentioned in Test Methods as 12.1g/100g and 13.1g/100g, respectively. It can be calculated that the solubility of Fenclorim in Pretilachlor has a difference between the room temperature and 54℃ of 1 g/100g.
2. The solubility Penoxsulam in Pretilachlor at room temperature and 54 ℃ was tested according to the method as mentioned in Test Methods as 0.12g/100g and 0.3g/100g, respectively.
E4
I. Different SCs were formulated in this E4 as follows:
i) . The water and Propylene glycol were added at the amount indicated in Table 10 to a reactor and mixing was started;
ii) . Silcolapse C565, Penoxsulam tech, dispersants, and other materials as shown in Table 10 were added in the amount as shown in Table 10 to the reactor, and mixing was continued until the suspension was homogeneous;
iii) . The suspension was milled in a bead mill until mean particle size d90<5μm was obtained as measured by laser particle size analyzer Malvern MS3000.
Figure PCTCN2022118727-appb-000025
In E4, SC10-12 were successfully formulated.
II. EC3 to EC5 were formulated in this E4 as follows:
i) . The solvent S-150 ND, Pretilachlor tech, Fenclorim tech, and emulsifiers as shown in Table 11 were added gradually in the amount as shown in Table 11 to a reactor under mixing; and
ii) . The mixture in the reactor was heated to about 50 ℃ and mixed at the same temperature until the liquid was clear.
Figure PCTCN2022118727-appb-000026
III. SE10 to SE12 were formulated by combining SC10 to SC12 with EC3 to E5, respectively (i.e., SC10+EC3, SC11+EC4, SC12+EC5) , according to the same procedure as mentioned in III of E1 with a shear rate at a 12000 to 15000rpm.
IV. Tests
The SE10 to SE12 were tested for appearance, wet sieve test, dispersion stability, low temperature stability, and heat storage stability at 54 ℃ according to the methods mentioned before. All SE10 to SE12 passed all the tests.
All publications, patents and patent applications mentioned in this specification are herein incorporated in their entirety by reference into the specification, to the same extent as if each individual publication, patent, or patent application was specifically and individually indicated to be incorporated herein by reference.
The examples illustrate the practice of the present subject matter in some of its embodiments but should not be construed as limiting the scope of the present subject matter. Other embodiments apparent to persons of ordinary skill in the art from consideration of the specification and examples herein that fall within the spirit and scope of the appended claims are part of this disclosure. The specification, including the examples, is intended to be exemplary only, without limiting the scope and spirit of the disclosure.

Claims (53)

  1. A stable agrochemical composition, comprising:
    a first active component which is solid at room temperature and insoluble in water at room temperature;
    a second active component which is solid at room temperature;
    a third active component which is liquid at room temperature; and
    water;
    the first active component is insoluble in the third active component at room temperature, and the second solid active component has a solubility in the third liquid active component of from 1 to 33 g/100g at room temperature.
  2. The stable agrochemical composition of claim 1 wherein the first active component, the second active component and the third active component are herbicidal active components.
  3. The stable agrochemical composition of claim 2 wherein the first active component is neither Pretilachlor nor a safener, the third liquid active component is Pretilachlor, and the second active component is Fenclorim.
  4. The stable agrochemical composition of claim 3, wherein the first active component is any one selected from the group consisted of Penoxsulam, Pyrazosulfuron-ethyl, Bensulfuron methyl, Quinclorac, Oxyfluorfen, Oxadiazon, cyhalofop-butyl, Pyriminobac-methyl, Clomazone (Dimethazon) , Pyribenzoxim, Oxadiargyl, and Simetryn.
  5. The stable agrochemical composition of claim 2 wherein the first active component is a triazolopyrimidine sulfonamide herbicide compound, the third liquid active component is an acetanilide herbicide compound, and the second active component is a safener compound
  6. The stable agrochemical composition of claim 1, wherein the first active component is Penoxsulam, the third liquid active component is Pretilachlor, and the second active component is Fenclorim.
  7. The stable agrochemical composition of any one of claims 1 to 6, wherein the content of the first active component is 0.02 to 40 percent by weight based on the total amount of the composition, the content of the second active component is 1 to 60 percent by weight based on the total amount of the composition, and the content of the third active component is 3 to 90 percent by weight based on the total amount of the composition.
  8. The stable agrochemical composition of claim 7, wherein the content of the first active component is 0.04 to 20 percent by weight based on the total amount of the composition, the content of the second active component is 2 to 30 percent by weight based on the total amount of the composition, and the content of the third active component is 6 to 80 percent by weight based on the total amount of the composition.
  9. The stable agrochemical composition of claim 7, wherein the content of the first active component is 0.08 to 10 percent by weight based on the total amount of the composition, the content of the second active component is 4 to 15 percent by weight based on the total amount of the composition, and the content of the third active component is 12 to 40 percent by weight based on the total amount of the composition.
  10. The stable agrochemical composition of claim 7, wherein the content of the first active component is 0.1 to 8 percent by weight based on the total amount of the composition, the content of the second active component is 4.9 to 11 percent by weight based on the total amount of the composition, and the content of the third active component is 15 to 33 percent by weight based on the total amount of the composition.
  11. The stable agrochemical composition of any one of claims 1 to 10, wherein the weight ratio of the second active component to the third active component is 1: 2 to 4.
  12. The stable agrochemical composition of any one of claims 1 to 11, wherein the composition further comprises an organic solvent with a content of 1 to 40 percent by weight based on the total amount of the composition.
  13. The stable agrochemical composition of any one of claims 1 to 12, wherein the composition further comprises one or more additives selected from the group consisting of thickener, dispersant, wetting agent, emulsifier, antifreeze, antifoam, and bactericide.
  14. The stable agrochemical composition of claim 13, wherein the total amount the additives is 3 to 70 percent by weight based on the total amount of the composition.
  15. The stable agrochemical composition of any one of claims 1 to 14, wherein the content of the oil phase in the composition is at least 50 percent by weight based on the total amount of the composition.
  16. The stable agrochemical composition of any one of claims 1 to 15, wherein the composition is SE.
  17. The stable agrochemical composition of any one of claims 1 to 16, wherein the stable composition has particles with a mean particle size d90 of ≤7 μm based on all particles of all types.
  18. The stable agrochemical composition of any one of claims 1 to 17, wherein the stable composition satisfies the stability requirements set forth for SE as recited in NY/T 2989-2016.
  19. The stable agrochemical composition of any one of claims 1 to 18, wherein the stable composition is a herbicidal composition.
  20. A process for preparing the stable agrochemical composition of claims 1 to 19, comprising the steps of:
    a) forming a SC of the first active component,
    b) forming an EC of the second active component and the third active component; and
    c) mixing the SC with the EC and other optional ingredients.
  21. The process of claim 20, wherein the step a) comprises mixing the first active component, a first portion of water, and other optional additives to form a homogeneous suspension.
  22. The process of claim 21, wherein the step a) further comprises milling the suspension until the mean particle size d90 is ≤7 μm.
  23. The process of any of claims 19-22, wherein the step b) comprises mixing the second and third active components, an optional organic solvent and other optional additives to form a clear liquid.
  24. The process of claim 23, wherein the mixing is conducted under heating.
  25. The process of any of claims 19-24, wherein in the step c) , the mixing of the SC with EC is conducted under a shear and the mean particle size d90 of the composition is ≤7 μm based on all particles of all types.
  26. The process of any of claims 19-25, wherein the composition comprises a thickener, and the step c) comprises c1) mixing the SC with a part of or all of the thickener to form a homogeneous suspension, and c2) mixing the suspension obtained in c1) with the EC.
  27. The process of any of claims 19-25, wherein the composition comprises a thickener, and the process further comprises a step d) : mixing the dispersion obtained in step c) with a part of or all of the thickener.
  28. A stable agrochemical composition prepared by a process comprise the steps of
    a) forming a SC of a first active component;
    b) forming an EC of a second active component and a third active component; and
    c) mixing the SC with EC and other optional ingredients;
    wherein the first active component is solid at room temperature and insoluble in water at room temperature, the second active component is solid at room temperature, and the third active component is liquid at room temperature; and
    the first active component is insoluble in the third active component at room temperature, and the second active component has a solubility in the third active component of from 1 to 33 g/100g at the room temperature.
  29. The stable agrochemical composition of claim 28, wherein the step a) comprises mixing the first active component, a first portion of water, and other optional additives to form a homogeneous suspension.
  30. The stable agrochemical composition of claim 29, wherein the step a) further comprises milling the suspension until the mean particle size d90 is ≤7 μm.
  31. The stable agrochemical composition of any one of claims 28 to 30, wherein the step b) comprises mixing the second and third active components, an optional organic solvent and other optional additives to form a clear liquid.
  32. The stable agrochemical composition of claims 31, wherein the mixing is conducted under heating.
  33. The stable agrochemical composition of any one of claims 28 to 32, wherein the composition comprises a thickener, and the step c) comprises c1) mixing the SC with the thickener to form a homogeneous suspension, and c2) mixing the suspension obtained in c1) with the EC.
  34. The stable agrochemical composition of any one of claims 28 to 32, wherein the composition comprises a thickener, and the thickener is not added in the step c) , the process further comprises a step d) : mixing the obtained dispersion in step c) with the thickener.
  35. The stable agrochemical composition of any one of claims 28 to 34, wherein in the step c) , the mixing of the SC with EC is conducted under a shear until the mean particle size d90 of the composition is ≤7 μm based on all particles of all types.
  36. The stable agrochemical composition of any one of claims 28 to 35, wherein the first active component, the second active component and the third active component are herbicidal active components.
  37. The stable agrochemical composition of claim 36, wherein the first active component is neither Pretilachlor nor a safener, the third liquid active component is Pretilachlor, and the second active component is Fenclorim.
  38. The stable agrochemical composition of claim 37, wherein the first active component is any one selected from the group consisted of Penoxsulam, Pyrazosulfuron-ethyl, Bensulfuron methyl, Quinclorac, Oxyfluorfen, Oxadiazon, cyhalofop-butyl, Pyriminobac-methyl, Clomazone (Dimethazon) , Pyribenzoxim, Oxadiargyl, and Simetryn.
  39. The stable agrochemical composition of any one of claims 28 to 36, wherein the first active component is a triazolopyrimidine sulfonamide herbicide compound, the  third liquid active component is an acetanilide herbicide compound, and the second active component is a safener compound.
  40. The stable agrochemical composition of any one of claims 28 to 39, wherein the first active component is Penoxsulam, the third liquid active component is Pretilachlor, and the second active component is Fenclorim.
  41. The stable agrochemical composition of any one of claims 28 to 40, wherein the content of the first active component is 0.02 to 40 percent by weight based on the total amount of the composition, the content of the second active component is 1 to 60 percent by weight based on the total amount of the composition, and the content of the third active component is 3 to 90 percent by weight based on the total amount of the composition.
  42. The stable agrochemical composition of claim 41, wherein the content of the first active component is 0.04 to 20 percent by weight based on the total amount of the composition, the content of the second active component is 2 to 30 percent by weight based on the total amount of the composition, and the content of the third active component is 6 to 80 percent by weight based on the total amount of the composition.
  43. The stable agrochemical composition of claim 41, wherein the content of the first active component is 0.08 to 10 percent by weight based on the total amount of the composition, the content of the second active component is 4 to 15 percent by weight based on the total amount of the composition, and the content of the third active component is 12 to 40 percent by weight based on the total amount of the composition.
  44. The stable agrochemical composition of claim 41, wherein the content of the first active component is 0.1 to 8 percent by weight based on the total amount of the composition, the content of the second active component is 4.9 to 11 percent by weight based on the total amount of the composition, and the content of the third  active component is 15 to 33 percent by weight based on the total amount of the composition.
  45. The stable agrochemical composition of any one of claims 28 to 44, wherein the weight ratio of the second active component to the third active component is 1: 2 to 4.
  46. The stable agrochemical composition of any one of claims 28 to 45, wherein the composition further comprises an organic solvent with a content of 1 to 40 percent by weight based on the total amount of the composition.
  47. The stable agrochemical composition of any one of claims 28 to 46, wherein the composition further comprises one or more additives selected from the group consisting of thickener, dispersant, wetting agent, emulsifier, antifreeze, antifoam, and bactericide.
  48. The stable agrochemical composition of claim 47, wherein the total amount the additives is 3 to 70 percent by weight based on the total amount of the composition.
  49. The stable agrochemical composition of any one of claims 28 to 48, wherein the content of the oil phase in the composition is at least 50 percent by weight based on the total amount of the composition.
  50. The stable agrochemical composition of any one of claims 28 to 49, wherein the composition is SE.
  51. The stable agrochemical composition of any one of claims 28 to 50, wherein the stable composition has particles with a mean particle size d90 of ≤7 μm based on all particles of all types.
  52. The stable agrochemical composition of any one of claims 28 to 51, wherein the stable composition satisfies the stability requirements set forth for SE as recited in NY/T 2989-2016.
  53. The stable agrochemical composition of any one of claims 28 to 52, wherein the stable composition is a herbicidal composition.
PCT/CN2022/118727 2021-09-16 2022-09-14 Stable agrochemical composition comprising two solid active components and one liquid active component and its preparation process WO2023040894A1 (en)

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JP2024516960A JP2024531780A (en) 2021-09-16 2022-09-14 Stable agrochemical composition containing two solid active ingredients and one liquid active ingredient, and process for preparing same
CN202280061845.4A CN117940016A (en) 2021-09-16 2022-09-14 Stable agrochemical composition comprising two solid active components and one liquid active component and method for preparing the same
IL311456A IL311456A (en) 2021-09-16 2022-09-14 Stable agrochemical composition comprising two solid active components and one liquid active component and its preparation process
CONC2024/0004249A CO2024004249A2 (en) 2021-09-16 2024-04-05 Stable agrochemical composition comprising two solid active components and one liquid active component and its preparation process

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1287782A (en) * 1999-09-14 2001-03-21 杭州振化化工有限公司 Composite herbicide contg. propisochlor/bensulfuron
CN1725952A (en) * 2002-11-21 2006-01-25 辛根塔参与股份公司 Herbicidal composition
CN1787743A (en) * 2003-03-13 2006-06-14 巴斯福股份公司 Synergistically acting herbicidal mixtures
CN103875686A (en) * 2009-08-28 2014-06-25 陶氏益农公司 Penoxsulam-containing herbicide composition
CN103906432A (en) * 2011-09-14 2014-07-02 陶氏益农公司 Synergistic herbicidal composition containing penoxsulam and pretilachlor
CN105142402A (en) * 2013-02-25 2015-12-09 美国陶氏益农公司 Synergistic weed control with penoxsulam and acetochlor

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1287782A (en) * 1999-09-14 2001-03-21 杭州振化化工有限公司 Composite herbicide contg. propisochlor/bensulfuron
CN1725952A (en) * 2002-11-21 2006-01-25 辛根塔参与股份公司 Herbicidal composition
CN1787743A (en) * 2003-03-13 2006-06-14 巴斯福股份公司 Synergistically acting herbicidal mixtures
CN103875686A (en) * 2009-08-28 2014-06-25 陶氏益农公司 Penoxsulam-containing herbicide composition
CN103906432A (en) * 2011-09-14 2014-07-02 陶氏益农公司 Synergistic herbicidal composition containing penoxsulam and pretilachlor
CN105142402A (en) * 2013-02-25 2015-12-09 美国陶氏益农公司 Synergistic weed control with penoxsulam and acetochlor

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