Brilliant black pigments

Patent metadata

Field	Value
Publication number	US-9657185-B2
Application number	US-201113991638-A
Country	US
Kind code	B2
Filing date	Nov 14, 2011
Priority date	Dec 9, 2010
Publication date	May 23, 2017
Grant date	May 23, 2017

Abstract

The present invention is related to brilliant black pigments comprising a flaky aluminum oxide substrate having a coating comprising a layered structure composed of a hematite and a magnetite layer, to a process for the production of said pigments, as well as to their use.

First claim

The invention claimed is:

1. Brilliant black pigments, each pigment comprising
flaky aluminum oxide substrate particles exhibiting an aspect ratio of at least 85, and
a coating comprising a layered structure consisting of
a first layer composed of hematite and/or goethite and
a second layer composed of magnetite, in this sequence, on the substrate,

wherein the thickness of the layer composed of magnetite is 50 to 250 nm, and
wherein the substrate particles have a mean particle diameter of lower than 20 μm and a D 50 value of 10 to 15 μm, measured by the laser diffraction method,
wherein the pigments are brilliant black pigments.

2. The brilliant black pigments according to claim 1 , wherein the substrate particles are of Al 2 O 3 or of Al 2 O 3 containing up to 5% by weight TiO 2 .

3. The brilliant black pigments according to claim 1 , wherein the substrate particles have a mean thickness between 50 and 200 nm.

4. The brilliant black pigments according to claim 1 , wherein the substrate particles have a mean particle diameter of 5 and 15 μm μm.

5. The brilliant black pigments according to claim 1 , wherein the mean particle diameter is lower than 16 μm.

6. The brilliant black pigments according to claim 1 , wherein the thickness of the layer composed of magnetite is higher than the thickness of the layer composed of hematite and/or goethite.

7. The brilliant black pigments according to claim 1 , wherein the layer composed of hematite and/or goethite is located directly on the substrate.

8. The brilliant black pigments according to claim 1 , wherein there is at least one dielectric coating located between the substrate and the layer composed of hematite and/or goethite.

9. The brilliant black pigments according to claim 1 , comprising furthermore a colourless dielectric layer on top of the magnetite layer.

10. The brilliant black pigments according to claim 9 , wherein the colourless dielectric layer is a silicon oxide hydrate layer which is located directly on top of the magnetite layer.

11. The brilliant black pigments according to claim 1 , wherein the magnetite layer is doped with an aluminum compound.

12. The brilliant black pigments according to claim 11 , wherein the aluminum compound is an oxide and/or an oxide hydrate.

13. The brilliant black pigments according to claim 11 , wherein the content of the aluminum compound is between 0.1 and less than 5% by weight, based on the weight of the magnetite layer.

14. The brilliant black pigments according to claim 9 , exhibiting a deep black body colour and, optionally, a blue interference colour.

15. A product selected from the group consisting of pigmenting inks, paints, varnishes, coating compositions, plastics, foils, paper, ceramics, glasses, cosmetic formulations, pharmaceutic formulations, laser marking and pigment preparations of diverse solvent contents, comprising pigments according to claim 1 .

16. The product according to claim 15 , wherein the ink is a printing ink.

17. The product according to claim 15 , wherein the paint or coating composition is an automotive paint or automotive coating composition.

18. The product according to claim 15 , wherein the cosmetic formulation is a mascara formulation, an eyeliner formulation or a kohl eye pencil formulation.

19. A product, comprising a pigment according to claim 1 .

20. A process for preparing the pigments according to claim 1 , comprising the following steps:
(a) dispersing flaky aluminum oxide substrate particles exhibiting an aspect ratio of at least 85, optionally being coated with at least one dielectric coating, in water,
(b) adding a water soluble iron (III) compound at a pH of between 2 and 4 and keeping the pH value constant, thereby precipitating a layer composed of hematite and/or goethite onto the surface of the substrate particles,
(c) raising the pH to a value between 5.5 and 7.5 and adding a water soluble iron (II) compound and a water soluble iron (III) compound, and optionally also adding an aqueous solution of an aluminum compound, while keeping the pH value constant, thereby directly precipitating a magnetite layer, which is optionally doped with an aluminum compound, onto the surface of the substrate particles precoated in step (b),
(d) optionally washing and filtering the resulting product and
(e) drying at a temperature in the range of from >100° C. to <180° C.

21. The process according to claim 20 which is executed in an inert gas atmosphere.

22. The process according to claim 20 , wherein after performing step (c) and prior to performing step (e), in an additional step at least one colourless dielectric layer is coated onto the magnetite layer.

23. The process according to claim 22 , wherein the dielectric layer coated onto the magnetite layer is a silicon oxide hydrate layer.

24. The process according to claim 20 , wherein the layer composed of magnetite is applied onto the substrate particles at a higher thickness than the layer composed of hematite and/or goethite.

Assignees

• Shimizu Kaiman
• Sasaki Fumiko
• Watanabe Yukitaka
• Merck Patent Gmbh

Inventors

• Shimizu Kaiman
• Sasaki Fumiko
• Watanabe Yukitaka

Classifications

• C01P2004/54

  Particles characterised by their aspect ratio, i.e. the ratio of sizes in the longest to the shortest dimension · CPC title

• C09D7/1291 Primary

  Chemistry & Metallurgy · mapped topic

• C09D11/037

  characterised by the pigment · CPC title

• C09C2200/30

  Interference pigments characterised by the thickness of the core or layers thereon or by the total thickness of the final pigment particle · CPC title

• C09C1/0015

  Pigments exhibiting interference colours, e.g. transparent platelets of appropriate thinness or flaky substrates, e.g. mica, bearing appropriate thin transparent coatings · CPC title