Composite filler particles and process for the preparation thereof

Patent metadata

Field	Value
Publication number	US-10040969-B2
Application number	US-201514872557-A
Country	US
Kind code	B2
Filing date	Oct 1, 2015
Priority date	Dec 15, 2011
Publication date	Aug 7, 2018
Grant date	Aug 7, 2018

Abstract

A process for the preparation of composite filler particles, comprising: (a) coating a particulate filler having a median particle size (D50) of from 1 to 1200 nm; (b) agglomerating the coated particulate filler, for providing a granulation of the coated particulate filler wherein the granulation contains the coated particulate filler particles whereby the at least one coating layer may be crosslinked by crosslinking groups obtained by reacting the reactive groups and optionally a further crosslinking agent.

First claim

The invention claimed is:

1. A process for preparation of composite filler particles, comprising the steps of:
(a) coating a particulate glass filler having a median particle size (D50) of from 100 to 1200 nm with a coating composition containing a film-forming agent forming a coating layer on the surface of the particulate glass filler, said coating layer displaying reactive groups on the surface of the coating layer, said reactive groups being selected from addition polymerizable groups and step-growth polymerizable groups, thereby forming a coated particulate glass filler; subsequently or concurrently
(b) agglomerating the coated particulate glass filler, for providing a granulation of the coated particulate glass filler wherein the granulation contains the coated particulate glass filler particles separated from and connected to each other by at least one coating layer, whereby the at least one coating layer may be crosslinked by crosslinking groups obtained by reacting the reactive groups of the coated layer, whereby the agglomeration is carried out by spray agglomeration;
wherein the prepared composite filler particles have a median particle size (D50) of from 1 to 70 μm;
wherein reactive groups are transformed into crosslinking groups by addition polymerization or step-growth polymerisation; and
wherein the particulate glass filler is the main component by volume of the composite filler particles.

2. The process according to claim 1 , wherein said reactive groups are selected from step-growth polymerizable groups.

3. The process according to claim 1 , wherein the coating composition contains a film-forming agent forming a covalent bond with the particulate glass filler.

4. The process according to claim 3 , wherein the covalent bond is obtained by the reaction of a hydroxyl group on the surface of the particulate glass filler and a silane group.

5. The process according to claim 1 , wherein the maximum thickness of the coating layer on the particulate glass filler is less than the median particle diameter (D50) of the particulate glass filler.

6. The process according to claim 1 , wherein the coating composition comprises one or more polymerizable monomers, a polymerization initiator, and a solvent.

7. The process according to claim 1 , wherein the coating composition has a dynamic viscosity in the range of from 0.0001 to 15 Pas (23° C.).

8. The process according to claim 1 , wherein the process is carried out in a fluidized bed.

9. The process according to claim 1 , wherein the particulate glass filler particles has a median particle size (D50) in the range of from 2 μm to 20 μm.

10. The process according to claim 1 , which further includes a step of treating the composite filler particles with a silanating agent or a surface active agent.

11. The process according to claim 1 , wherein agglomerating the coated particulate glass filler occurs in the presence of a further crosslinking agent.

12. The process according to claim 1 , wherein agglomerating the coated particulate glass filler occurs in the presence of a further particulate glass filler not displaying reactive groups.

13. The process according to claim 11 , wherein the at least one coating layer is crosslinked by crosslinking groups obtained by reacting the reactive groups and the further crosslinking agent.

14. The process according to claim 1 , further comprising at least one of milling, classifying or sieving the granulation of the coated particulate glass filler.

15. The process according to claim 1 , further comprising crosslinking the granulation of the coated particulate glass filler.

16. The process according to claim 1 , wherein the crosslinking of the at least one coating layer can occur during agglomeration or after agglomeration.

Assignees

• Dentsply Int Inc
• Dentsply Sirona Inc

Inventors

• Stelzig Simon
• Kempter Jörg
• Noerpel Stephanie
• Klee Joachim E
• Facher Andreas
• Walz Uwe
• Weber Christoph

Classifications

• A61K6/822

  comprising rare earth metal oxides · CPC title

• A61K6/807

  comprising magnesium oxide · CPC title

• A61K6/818

  comprising zirconium oxide · CPC title

• A61K6/75

  Apatite · CPC title

• A61K6/72

  comprising nitrogen-containing compounds · CPC title