Method for producing microcapsules

Patent metadata

Field	Value
Publication number	US-10835885-B2
Application number	US-201716097007-A
Country	US
Kind code	B2
Filing date	Apr 22, 2017
Priority date	Apr 29, 2016
Publication date	Nov 17, 2020
Grant date	Nov 17, 2020

Abstract

The invention relates to a method for producing microcapsules, comprising the following steps: (a) providing a first aqueous preparation containing at least one prepolymer; (b) providing a second non-aqueous preparation containing the active substance to be encapsulated; (c) mixing the aqueous and the non-aqueous phases in the presence of at least one emulsifier and/or stabilizer in order to form an emulsion; (d) polymerizing the at least one prepolymer contained in the emulsion from step (c) in order to obtain a dispersion of microcapsules that enclose the active substance; (e) hardening and cross-linking the microcapsules obtained in step (d); and optionally (f) removing the microcapsules from the dispersion and drying the microcapsules, the method being characterized in that the emulsion is formed in the presence of at least one 1,2-diol in step (c).

First claim

The invention claimed is:

1. A process for producing microcapsules and controlling their particle size, comprising the following steps:
(a) providing a first, aqueous formulation comprising at least one prepolymer;
(b) providing a second, nonaqueous formulation comprising an active to be encapsulated;
(c) mixing the aqueous phase and the nonaqueous phase in the presence of at least one emulsifier and/or stabilizer to form an emulsion;
(d) polymerizing the at least one prepolymer present in the emulsion from step (c) to obtain a dispersion of microcapsules enclosing the active;
(e) hardening and crosslinking the microcapsules obtained in step (d), and optionally
(f) removing and drying the microcapsules from the dispersion,
wherein
(i) the emulsion is formed in step (c) in the presence of at least one 1,2-diol and
(ii) the particles from the process have a single average particle size distribution of from 10 to 35 microns.

2. The process as claimed in claim 1 , wherein the prepolymer is selected from the group consisting of optionally alkylated mono- and polymethylolurea or mono- and polymethylolmelamine precondensates, partially methylated mono- and polymethylol-1,3,5-triamino-2,4,6-triazine precondensates, mono- and polyalkylolbenzoguanamine and mono- and polyalkylolglycoluril precondensates, poly[N-(2,2-dimethoxy-1-hydroxy)]polyamines, dialdehydes and resorcinol and mixtures thereof.

3. The process as claimed in claim 1 , wherein the active to be encapsulated is at least one aroma, at least one fragrance or at least one biogenic principle.

4. The process as claimed in claim 1 , wherein the emulsifier is a 1,2-diol selected from the group consisting of pentane-1,2-diol, hexane-1,2-diol, octane-1,2-diol, decane-1,2-diol, dodecane-1,2-diol and mixtures thereof.

5. The process as claimed in claim 4 , wherein the 1,2-diol is a mixture of hexane-1,2-diol and octane-1,2-diol.

6. The process as claimed in claim 1 , wherein the diol is used in amounts of about 0.1% to about 10% by weight based on the emulsion.

7. The process as claimed in claim 1 , wherein the stabilizer is selected from the group consisting of sulfonated acrylic copolymers, copolymers of acrylamides and acrylic acid, copolymers of alkyl acrylates and N-vinylpyrrolidone, sodium polycarboxylates, sodium polystyrenesulfonates, vinyl ether- and methyl vinyl ether-maleic anhydride copolymers, and ethylene-, isobutylene- or styrene-maleic anhydride copolymers and mixtures thereof.

8. The process as claimed in claim 1 , wherein the emulsifier and stabilizer are each used in a total amount of about 1% to about 10% by weight based on the emulsion.

9. The process as claimed in claim 2 wherein polycondensation of an amine-formaldehyde precondensate is triggered by adjusting the pH of the emulsion to about 1.0 to about 5.8.

10. The process as claimed in claim 1 , wherein the microcapsules are hardened or crosslinked by adjusting the temperature of the dispersion to about 50 to about 90° C.

11. The process as claimed in claim 1 , wherein the microcapsules are hardened by adding melamine to the dispersion.

12. The process as claimed in claim 1 , wherein the entire reaction is conducted with vigorous stirring.

13. The process as claimed in claim 1 , wherein a formaldehyde scavenger is added to the dispersion after the capsules have been hardened.

Assignees

• Symrise Ag

Inventors

• Rost Benjamin
• Bertram Ralf
• Gregor Daniela
• Ebbecke Jan Peter
• Lange Sabine

Classifications

• B01J13/18

  In situ polymerisation with all reactants being present in the same phase · CPC title

• C11D3/505

  encapsulated or adsorbed on a carrier, e.g. zeolite or clay · CPC title

• B01J13/14 Primary

  Polymerisation; cross-linking · CPC title

• B01J13/206

  Hardening; drying · CPC title