Method for producing aqueous active substance compositions of active substances that are hardly soluble in water
First Claim
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1. A process for preparing an aqueous active compound composition for the protection of crops or materials, which process comprises the following steps:
- a) providing an aqueous suspension of (1) solid active compound particles of at least one active compound having a solubility in water of not more than 5 g/l at 25°
C./1013 mbar, and at least one surfactant, wherein the active compound particles in the suspension have a mean particle size, determined by dynamic light scattering, of 20 to 1200 nm, where the preparation of the suspension of the solid active compound particles comprises comminution of the solid active compound in the presence of the at least surfactant, or precipitating the active compound from a solution of the active compound in the presence of the at least one surfactant,b) adding a first monomer composition M1 to the suspension of solid active compound particles and initiating an emulsion polymerization of said first monomer composition M1 in the aqueous suspension of the active compound, wherein the monomer composition M1 comprises at least 95% by weight, based on its total weight, of at least one neutral, monoethylenically unsaturated monomer M1.1 having a solubility in water of not more than 30 g/l at 25°
C./1 013 mbar, giving an aqueous dispersion of polymer/active compound particles, andc) conducting emulsion polymerization of a second monomer composition M2 in an aqueous dispersion of the polymer/active compound particles obtained in step b), wherein the monomer composition M2 comprises at least 60% by weight, based on its total weight, of at least one neutral, monoethylenically unsaturated monomer M2.1 having a solubility in water of not more than 30 g/l at 25°
C./1013 mbar,wherein the monomer M1.1 is selected from the group consisting of vinylaromatic monomers and the esters of α
,β
-ethylenically unsaturated mono- and dicarboxylic acids having 3 to 8 carbon atoms with C1-C10-alkanols or C3-C10-cycloalkanols,wherein the monomer M2.1 is selected from the group consisting of vinylaromatic monomers and the esters of α
,β
-ethylenically unsaturated C3-C10-monocarboxylic and C3-C10-dicarboxylic acids with C1-C10-alkanols or C3-C10-cycloalkanols, andwherein the active compound is a solid at a temperature of 50°
C. and selected from the group consisting of herbicides, fungicides, insecticides, acaricides, nematicides, bactericides, algicides, molluscicides, plant growth regulators and biocides.
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Abstract
The present invention relates to a process for preparing aqueous active compound compositions of active compounds which are poorly soluble in water, in particular of active compounds for the protection of crops and materials. Moreover, the invention relates to the active compound compositions obtainable by the process and to their use for controlling harmful organisms in plants and in the protection of materials.
The process comprises the following steps:
- a) provision of an aqueous suspension of solid active compound particles of at least one active compound having a solubility in water of not more than 5 g/l at 25° C./1013 mbar, comprising, for stabilizing the active compound particles, at least one surfactant, where the active compound particles in the suspension have a mean particle size, determined by dynamic light scattering, of not more than 1200 nm,
- b) emulsion polymerization of a first monomer composition M1 in the aqueous suspension of the active compound, where the monomer composition M1 comprises at least 95% by weight, based on its total weight, of at least one neutral, monoethylenically unsaturated monomer M1.1 having a solubility in water of not more than 30 g/l at 25° C./1013 mbar, giving an aqueous dispersion of polymer/active compound particles, and
- c) emulsion polymerization of a second monomer composition M2 in an aqueous dispersion of the polymer/active compound particles obtained in step b), where the monomer composition M2 comprises at least 60% by weight, based on its total weight, of at least one neutral, monoethylenically unsaturated monomer M2.1 having a solubility in water of not more than 30 g/l at 25° C./1013 mbar.
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Citations
20 Claims
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1. A process for preparing an aqueous active compound composition for the protection of crops or materials, which process comprises the following steps:
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a) providing an aqueous suspension of (1) solid active compound particles of at least one active compound having a solubility in water of not more than 5 g/l at 25°
C./1013 mbar, and at least one surfactant, wherein the active compound particles in the suspension have a mean particle size, determined by dynamic light scattering, of 20 to 1200 nm, where the preparation of the suspension of the solid active compound particles comprises comminution of the solid active compound in the presence of the at least surfactant, or precipitating the active compound from a solution of the active compound in the presence of the at least one surfactant,b) adding a first monomer composition M1 to the suspension of solid active compound particles and initiating an emulsion polymerization of said first monomer composition M1 in the aqueous suspension of the active compound, wherein the monomer composition M1 comprises at least 95% by weight, based on its total weight, of at least one neutral, monoethylenically unsaturated monomer M1.1 having a solubility in water of not more than 30 g/l at 25°
C./1 013 mbar, giving an aqueous dispersion of polymer/active compound particles, andc) conducting emulsion polymerization of a second monomer composition M2 in an aqueous dispersion of the polymer/active compound particles obtained in step b), wherein the monomer composition M2 comprises at least 60% by weight, based on its total weight, of at least one neutral, monoethylenically unsaturated monomer M2.1 having a solubility in water of not more than 30 g/l at 25°
C./1013 mbar,wherein the monomer M1.1 is selected from the group consisting of vinylaromatic monomers and the esters of α
,β
-ethylenically unsaturated mono- and dicarboxylic acids having 3 to 8 carbon atoms with C1-C10-alkanols or C3-C10-cycloalkanols,wherein the monomer M2.1 is selected from the group consisting of vinylaromatic monomers and the esters of α
,β
-ethylenically unsaturated C3-C10-monocarboxylic and C3-C10-dicarboxylic acids with C1-C10-alkanols or C3-C10-cycloalkanols, andwherein the active compound is a solid at a temperature of 50°
C. and selected from the group consisting of herbicides, fungicides, insecticides, acaricides, nematicides, bactericides, algicides, molluscicides, plant growth regulators and biocides. - View Dependent Claims (2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20)
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Specification