IP Library Granted Patent US 9,051,471
Granted Patent B2
US 9,051,471 · App. 14/007,383 · Granted Jun 9, 2015

Weather-resistant pearlescent pigments, process for the production and use thereof

Inventors: Michael Grüner (Auerbach, DE); Thomas Schneider (Lauf a. d. Pegnitz, DE); Günter Kaupp (Neuhaus, DE)
Assignee: ECKART GMBH
C09C1/28C01P2004/60C09C1/0021C09C1/0024C09C2200/1004C09C2200/102C09C2200/1087C09C2200/40C09C2200/408C09C2220/106C09D5/36C09D11/037C01P2004/61A61Q1/02A61K8/0258A61K8/19A61K2800/436C09C1/405C01P2004/20C01P2006/60
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Quick Facts
Patent No.
US 9,051,471
App. No.
14/007,383
Granted
Jun 9, 2015
Kind
B2
Abstract

The present invention relates to a weather-resistant pearlescent pigment which consists of a platelet-shaped substrate coated with one or more highly refractive metal oxides, the platelet-shaped substrate being selected from the group consisting of synthetic mica flakes, glass flakes, SiO 2 flakes, Al 2 O 3 flakes, synthetic boehmite flakes, BiOCl flakes and mixtures thereof, and a top layer, wherein the top layer consists of the following layers: a) a cerium-containing layer, selected from the group consisting of cerium oxide, cerium hydroxide, hydrated cerium oxide, and mixtures thereof, the cerium-containing layer being applied directly to the highly refractive metal oxide layer, and b) an organic-chemical compatibilizing layer, which comprises the reaction products of oligomeric silanes, wherein the oligomeric silanes have one or more amino groups, the organic-chemical compatibilizing layer being applied directly to the cerium-containing layer a).

Claims (30)

1. A weather-resistant pearlescent pigment which consists of a platelet-shaped substrate coated with one or more metal oxides, thereby forming a metal oxide layer, wherein the metal oxide layer has a refractive index greater than 1.8, the platelet-shaped substrate being selected from the group consisting of synthetic mica flakes, glass flakes, SiO 2 flakes, Al 2 O 3 flakes, synthetic boehmite flakes, BiOCl flakes and mixtures thereof, and a top layer, wherein the top layer consists of the following layers:

a) a cerium-containing layer being applied directly to the metal oxide layer, the cerium-containing layer being selected from the group consisting of cerium oxide, cerium hydroxide, hydrated cerium oxide and mixtures thereof, and

b) an organic-chemical compatibilizing layer being applied directly to the cerium-containing layer a), the organic-chemical compatibilizing layer comprising the reaction product(s) of one or more oligomeric silane(s), wherein the oligomeric silane(s) have one or more amino groups; and

wherein the organic-chemical compatibilizing layer is essentially free of a separate layer of SiO 2 .

2. The weather-resistant pearlescent pigment according to claim 1 , wherein the platelet-shaped synthetic substrate is selected from the group consisting of synthetic mica flakes, glass flakes, Al 2 O 3 flakes and mixtures thereof.

3. The weather-resistant pearlescent pigment according to claim 1 , wherein the layer a) is present in quantities in a range of from 0.05 to 0.9 weight percent, relative to the total weight of the pearlescent pigment and calculated as elemental cerium.

4. The weather-resistant pearlescent pigment according to claim 1 , wherein the oligomeric silane(s) have one or more alkyl groups of from 1 to 18 C atoms.

5. The weather-resistant pearlescent pigment according to claim 1 , wherein the proportion of the top layer on all of the pearlescent pigment is 0.3 to 2.5 weight percent, relative to the total weight of the pearlescent pigment.

6. The weather-resistant pearlescent pigment according to claim 1 , wherein the coating of the pearlescent pigment with the entire top layer has taken place in aqueous medium.

7. The weather-resistant pearlescent pigment according to claim 1 , wherein the substrate is coated with one highly refractive metal oxide layer selected from the group consisting of TiO 2 , Fe 2 O 3 , TiFe 2 O 5 , Fe 2 Ti 3 O 9 , FeTiO 3 and mixtures thereof.

8. The weather-resistant pearlescent pigment according to claim 1 , wherein the weather-resistant pearlescent pigment has the values D 10 , D 50 , D 90 from the cumulative frequency distribution of the volume-averaged size distribution function with a span ΔD of from 0.7-1.4, wherein the span ΔD is calculated according to Formula (I):

Δ D =( D 90 −D 10 )/ D 50   (I).

9. The weather-resistant pearlescent pigment according to claim 8 , wherein the pearlescent pigment has a span ΔD of from 0.75-1.3.

10. A process for producing the weather-resistant pearlescent pigment according to claim 1 , comprising:

a) optionally classifying the platelet-shaped substrate, obtaining substrates which have the values D 10 , D 50 , D 90 from the cumulative frequency distribution of the volume-averaged size distribution function with a span ΔD of from 0.7-1.4,

b) suspending a platelet-shaped substrate, optionally from step a), in aqueous solution, and coating the platelet-shaped substrate with one or more highly refractive metal oxides, obtaining pearlescent pigments,

c) coating the pearlescent pigments from step b) in aqueous solution with a cerium salt or a hydrolyzable cerium metalorganic compound, obtaining a layer which is selected from the group consisting of cerium hydroxide, hydrated cerium oxide and mixtures thereof,

d) coating the pearlescent pigments from step c) in aqueous solution with oligomeric silanes, and

e) separating the coated pearlescent pigments, optional washing with demineralized water, and drying at a temperature of from 80° to 160° C.

11. A coating, printing ink, varnish, plastic or cosmetic comprising the weather-resistant pearlescent pigments according to claim 1 .

12. The weather-resistant pearlescent pigment according to claim 1 , wherein the organic-chemical compatibilizing layer consists of the reaction product(s) of one or more oligomeric silane(s), wherein the oligomeric silane(s) have one or more amino groups.

13. The weather-resistant pearlescent pigment according to claim 1 , wherein the organic-chemical compatibilizing layer consists of the reaction product(s) of one or more oligomeric silane(s), wherein the oligomeric silane(s) have one or more amino groups, with one or more other silanes.

14. The weather-resistant pearlescent pigment according to claim 1 , wherein the organic-chemical compatibilizing layer is free of metal oxides.

15. The weather-resistant pearlescent pigment according to claim 1 , wherein the oligomeric silane is selected from the group consisting of amino/alkyl functional siloxane co-oligomer, diamino/alkyl functional siloxane co-oligomer, amino/vinyl functional siloxane co-oligomer, amino/methacrylate functional siloxane co-oligomer, oligomeric diaminosilane and mixtures thereof.

16. The weather-resistant pearlescent pigment according to claim 1 , wherein the pigment is produced by a process comprising:

a) optionally classifying the platelet-shaped substrate, obtaining substrates which have the values D 10 , D 50 , D 90 from the cumulative frequency distribution of the volume-averaged size distribution function with a span ΔD of from 0.7-1.4,

b) suspending a platelet-shaped substrate, optionally from step a), in aqueous solution, and coating the platelet-shaped substrate with one or more highly refractive metal oxides, obtaining pearlescent pigments,

c) coating the pearlescent pigments from step b) in aqueous solution with a cerium salt or a hydrolyzable cerium metalorganic compound, obtaining a layer which is selected from the group consisting of cerium hydroxide, hydrated cerium oxide and mixtures thereof,

d) coating the pearlescent pigments from step c) in aqueous solution with one or more oligomeric silane(s), and

e) separating the coated pearlescent pigments, optional washing with demineralized water, and drying at a temperature of from 80° to 160° C.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 25, 2013
From: GRUNER, MICHAEL; SCHNEIDER, THOMAS; KAUPP, GUNTER
To: ECKART GMBH
Reel/Frame 031275/0520 →
Priority Claims (1)
DE 10 2011 015 338 · Mar 28, 2011 · national
Continuity (1)
Related Publication 20140018439A1 · Jan 16, 2014