Production of solid solutions of pesticides by short-term superheating and rapid drying

• US 9,480,250 B2
• Filed: 11/23/2007
• Issued: 11/01/2016
• Est. Priority Date: 12/01/2006
• Status: Active Grant

• Current Assignee: BASF SE
• Original Assignee: BASF SE
• Inventors: Kolter, Karl, Schnherr, Michael, Ascherl, Hermann, Dieleman, Cedric, Knieriem, Torsten, Koltzenburg, Sebastian, Trk, Holger
• Primary Examiner(s): Haghighatian, Mina
• Assistant Examiner(s): HIRT, ERIN E
• Application Number:
  US12/516,376
• Publication Number:
  US 20100062940A1
• Time in Patent Office: 3,266 Days
• Field of Search: 504/116
• US Class Current: 1/1
• CPC Class Codes: A01N 2300/00 Combinations or mixtures of active ingredients covered by classes A01N27/00 - A01N65/48 with other active or formulation relevant ingredients, e.g. specific carrier materials or surfactants, covered by classes A01N25/00 - A01N65/48
• CPC Class Codes: A01N 25/10 Macromolecular compounds
• CPC Class Codes: A01N 25/12 Powders or granules A01N25/26 takes precedence
• CPC Class Codes: A01N 43/653 1,2,4-Triazoles; Hydrogenated 1,2,4-triazoles
• CPC Class Codes: A01N 47/24 containing the groups , or; Thio analogues thereof

Abstract

The present invention relates to a method for the production of solid solutions of sparingly soluble pesticides, pulverulent products that are obtained by said method and their use for pesticide formulations.

Claims

1. A method for the production of pulverulent or granulated solid solution of a sparingly soluble pesticide, in which the sparingly soluble pesticide is molecularly dispersed in a matrix of inactive ingredients, comprising

preparing a hot, pressurized aqueous solution of the pesticide and of the inactive ingredients of the matrix by heating an aqueous suspension of the sparingly soluble pesticide in the presence of the inactive ingredients of the matrix to temperatures that are above the boiling point at normal pressure and the sparingly soluble pesticide is dissolved, the temperatures during heating being in the range from 90°

C. to 300°

C., and

converting the hot, pressurized aqueous solution of the sparingly soluble pesticide and of the inactive ingredients of the matrix to a solid form by spraying and drying, the temperature of the hot, pressurized aqueous solution before being fed into a spraying device being between 90°

C. to 300°

C., and the pressure of the aqueous solution before feed into the spraying device being from 1 to 15 MPa,

where the aqueous suspension of the sparingly soluble pesticide in the presence of the inactive ingredients of the matrix is heated continuously in a devices such that the residence time of the solution containing the active substance at temperatures above 90°

C. is less than 180 seconds and where the solution is led directly to a spraying device,

where the pesticide is selected from the group consisting of insecticides, fungicides, herbicides and safeners and where the solubility of the pesticide at 20°

C. is less than 1% by weight in water, 0.1 molar aqueous hydrochloric acid, aqueous phosphate buffer at pH 7.2, and 0.9 wt. % aqueous sodium chloride,

and where the sparingly soluble pesticide molecularly dispersed in the matrix of inactive ingredients has a crystalline fraction less than 3 wt. %.

2. The method of claim 1, wherein the concentration of the sparingly soluble pesticide in the matrix of inactive ingredients is between 1 and 50 wt. %.

3. The method of claim 1, wherein the solution contains an adsorbent.

4. The method of claim 1, wherein the aqueous suspension of the pesticide is heated by mixing with a hot stream of liquid or a hot stream of steam.

5. The method of claim 4, wherein the ratio of the suspension of the pesticide to the hot liquid stream is between 9:

1 and 1;

9.

6. The method of claim 1, wherein methods of spray drying or fluidized-bed spray granulation are used for drying.

7. The method of claim 6, wherein an adsorbent or dusting agent is injected into a spraying tower during spray drying.

8. The method of claim 1, where the pesticide is a fungicide selected from the group consisting of triazoles, strobilurins and boscalid.

9. The method of claim 1, where the pesticide is a fungicide selected from the group consisting of epoxiconazole, metconazole, pyraclostrobin, kresoxim-methyl, 5-chloro-7-(4-methylpiperidin-1-yl)-6-(2,4,6-trifluorophenyl)-[1,2,4]triazolo[1,5-a]pyrimidine and boscalid.

10. The method of claim 1, where the pesticide is an insecticide selected from the group consisting of metaflumizone, fipronil and alpha-cypermethrin.

11. The method of claim 1, where the matrix forming inactive ingredients comprise a water soluble polymer, selected from the group consisting of polyvinylpyrrolidone, vinylpyrrolidone-vinylacetate copolymers, polyvinylcaprolactams, polyvinylformamide, polyvinylacetamide, polyacrylates, polymethacrylates, polyacrylamides, polyethylene-imines, polyvinylamines, hydroxyalkylcelluloses, alkylhydroxyalkylcelluloses, carboxyalkylcelluloses, alkylhydroxyalkylcellulose-acetate-succinates, alkyl-hydroxyalkylcellulose-acetatephthalates, alkylhydroxyalkylcellulose-phthalates, celluloseacetate-phthalates, starches, hydroxy alkyl starches, carboxy alkyl starches, modified starch, octenylsuccinate-starches, dextrans, polyoxyethylene-polyoxypropylene block copolymers, polyethylene oxides, polypropylene oxides, and polyamino acids.

12. The method of claim 1, where the matrix forming inactive ingredients comprise a water soluble polymer, selected from the group consisting of polyvinylpyrrolidone and vinylpyrrolidone-vinylacetate copolymers.