Process for preparing an aqueous dispersion of microparticles

Patent metadata

Field	Value
Publication number	US-12330128-B2
Application number	US-201615769158-A
Country	US
Kind code	B2
Filing date	Oct 20, 2016
Priority date	Oct 22, 2015
Publication date	Jun 17, 2025
Grant date	Jun 17, 2025

Abstract

Provided herein is a process for preparing an aqueous dispersion of microparticles containing a water-insoluble, solid, non-polymeric, organic active or functional material (M) and an aminoplast resin (A) which surrounds or embeds material (M). The process includes the following steps: i) providing an aqueous slurry of the material (M) in the form of coarse particles; ii) subjecting the aqueous slurry to shear forces such that the coarse particles of the material (M) are comminuted and an aqueous suspension of fine particles of the material (M) is obtained; and iii) performing a polycondensation of an aminoplast pre-condensate during step (ii) or in the aqueous suspension of the fine particles of the material (M) obtained in step (ii); wherein step (ii) is performed in the presence of at least one protective colloid and in the presence of at least a portion of the aminoplast pre-condensate subjected to the polycondensation of step (iii).

First claim

We claim:

1. A process for preparing an aqueous dispersion of microcapsules containing a water-insoluble solid organic material selected from agriculturally active compounds and an aminoplast resin that surrounds or embeds the water-insoluble solid organic material, the process comprising the following steps:
i. providing an aqueous slurry of a water-insoluble solid organic material in a form of coarse particles;
ii. subjecting the aqueous slurry to shear forces in order to comminute the coarse particles, wherein an aqueous suspension of fine particles of the water-insoluble solid organic material is obtained; and
iii. performing a polycondensation of an aminoplast pre-condensate in the aqueous suspension obtained in step ii;
wherein the subjecting the aqueous slurry to shear forces of step ii is performed in the presence of at least one protective colloid and at least a portion of the aminoplast pre-condensate subjected to the polycondensation of step iii;
wherein the protective colloid is selected from the group consisting of a homo-or copolymer of a (meth) acrylate monomer having a sulfonic acid group, a (meth) acrylamide monomer having a sulfonic acid group, arylsulfonic acid formaldehyde condensates, and mixtures thereof.

2. The process of claim 1 , wherein the aminoplast pre-condensate is selected from the group consisting of melamine formaldehyde pre-condensates, urea formaldehyde pre-condensates, and mixtures thereof.

3. The process of claim 2 , wherein the aminoplast pre-condensate comprises an etherified melamine formaldehyde pre-condensate.

4. The process of claim 1 , wherein at least 50% of the aminoplast pre-condensate subjected to the polycondensation of step iii is present in the aqueous suspension during step ii.

5. The process of claim 1 , wherein the aminoplast pre-condensate is present in the aqueous suspension of step ii in an amount from 1 to 30% by weight, based on water-insoluble solid organic material to be encapsulated.

6. The process of claim 1 , wherein the aqueous suspension of step ii additionally contains at least one anionic emulsifier different from the protective colloid.

7. The process of claim 1 , wherein the coarse particles of the water-insoluble solid organic material are milled to a volume average particle diameter in a range from 0.5 to 25 μm, as determined by dynamic light scattering.

8. The process of claim 1 , wherein the comminution in step ii is performed by grinding.

9. The process of claim 8 , wherein the comminution in step ii is performed in a stirred media mill.

10. The process of claim 1 , wherein a concentration of the water-insoluble solid organic material in the aqueous slurry of step i is from 5 to 40% by weight.

11. The process of claim 1 , wherein the water-insoluble solid organic material is selected from organic compounds having a melting point above 50° C.

12. The process of claim 1 , wherein at least 50% of the aminoplast pre-condensate subjected to the polycondensation of step iii and at least 50% of the protective colloid are contained in the aqueous suspension of the water-insoluble solid organic material prior to the comminution.

13. The process of claim 1 , wherein the aqueous suspension of the water-insoluble solid organic material has a pH of at least 6 during the comminution in step ii.

14. The process of claim 1 , wherein the polycondensation of the aminoplast pre-condensate in the aqueous suspension obtained in step ii is performed at a pH of at most 5.

15. The process of claim 1 , wherein the aqueous suspension of the water-insoluble solid organic material has a pH in a range of 6.5 to 9.0 during the comminution in step ii, and wherein the polycondensation of the aminoplast pre-condensate in the aqueous suspension obtained in step ii is performed at a pH in a range of 2 to 4.

Assignees

• Basf Se

Inventors

• Winkelmann Marion
• Muelheims Kerstin
• Tauber Ralph
• Fuchs Yannick
• Cetinkaya Murat
• Sachweh Bernd

Classifications

• A01N2300/00

  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 title

• A01N43/54

  1,3-Diazines; Hydrogenated 1,3-diazines · CPC title

• A61K9/5089

  Processes · CPC title

• A61K9/145

  with organic compounds · CPC title

• C09B67/0097

  Dye preparations of special physical nature; Tablets, films, extrusion, microcapsules, sheets, pads, bags with dyes · CPC title