IP Library Granted Patent US 9,951,194
Granted Patent B2
US 9,951,194 · App. 14/044,297 · Granted Apr 24, 2018

Iron oxide containing effect pigments, their manufacture and their use

Inventors: Juergen Walker (Ossining, NY); Gabe Uzunian (Rye, NY); Raimund Schmid (Neustadt, DE); Aron Wosylus (Bad Durkheim, DE); Christoph Schwidetzky (Ludwigshafen, DE)
Assignee: BASF CORPORATION
C08K3/0033A61K8/0241A61K8/19A61K8/965A61Q1/02A61Q3/04C09C1/0015C09C1/24A61K2800/43A61K2800/621A61Q1/04A61Q1/06A61Q1/08A61Q1/10A61Q3/02C01P2006/80
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Quick Facts
Patent No.
US 9,951,194
App. No.
14/044,297
Granted
Apr 24, 2018
Kind
B2
Abstract

An iron oxide containing effect pigment, and methods for producing and using the same are discussed. The iron oxide containing effect pigment may include an iron oxide coating in direct contact with a particulate substrate, which may have high levels of hematite, magnetite, or maghemite; and low amounts of toxic metals. A method for producing the pigment may include chemical vapor deposition of iron pentacarbonyl onto a particulate substrate. The iron oxide containing effect pigments may be incorporated into compositions, such as cosmetics.

Claims (54)

1. An iron oxide containing effect pigment comprising:

a particulate substrate; and

an iron oxide coating which is in direct contact with the particulate substrate and at least partially encapsulates the particulate substrate;

wherein:

the iron oxide coating comprises >98% hematite, magnetite, or maghemite; and

the iron oxide containing effect pigment comprises ≤15.0 ppm Cr, based on the total iron oxide containing effect pigment as determined by total dissolution.

2. The iron oxide containing effect pigment of claim 1 , wherein the particulate substrate is one or more of natural mica, synthetic mica, TiO 2 -coated natural mica, TiO 2 -coated synthetic mica, tin oxide-coated natural mica, tin oxide-coated synthetic mica, silica, alumina, a glass flake, SiO 2 -coated mica, and TiO 2 -coated SnO x -coated mica wherein x is 1 or 2.

3. The iron oxide containing effect pigment of claim 1 , wherein the particulate substrate comprises synthetic mica.

4. The iron oxide containing effect pigment of claim 1 , wherein the iron oxide containing effect pigment has a diameter from about 10 μm to about 300 μm.

5. The iron oxide containing effect pigment of claim 3 , wherein the particulate substrate comprises fluorophlogopite.

6. A method of producing an iron oxide containing effect pigment, the method comprising:

depositing iron oxide from an iron pentacarbonyl using chemical vapor deposition directly onto a particulate substrate to form an iron oxide coating on the particulate substrate;

wherein:

the iron oxide coating is in direct contact with and at least partially encapsulates the substrate, and the iron oxide coating comprises:

>98% hematite, magnetite, or maghemite; and

the iron oxide containing effect pigment comprises:

≤15.0 ppm Cr, based on the total iron oxide containing effect pigment as determined by total dissolution.

7. The method of claim 6 , wherein the depositing step comprises:

providing the particulate substrate into a reaction chamber;

fluidizing the particulate substrate by pumping a first inert gas into the reaction chamber;

heating the reaction chamber to from about 80° C. to about 325° C.;

pumping a second gas into the reaction chamber, wherein the second gas comprises oxygen;

pumping a third inert gas into the reaction chamber, wherein the third inert gas comprises iron pentacarbonyl; and

forming an iron oxide coating on the particulate substrate to produce the iron oxide containing effect pigment.

8. The method of claim 7 , wherein the first inert gas is pumped in the reaction chamber at a rate of about 1600 l/h to about 2400 l/h.

9. The method of claim 7 , wherein the third inert gas is pumped in the reaction chamber at a rate of from about 160 l/h to about 240 l/h.

10. The method of claim 6 , wherein the iron oxide coating has a thickness of from about 1 nm to about 200 nm.

11. The method of claim 6 , wherein the substrate comprises fluorophlogopite.

12. A cosmetic product comprising the iron oxide containing effect pigment of claim 1 .

13. The cosmetic of claim 12 , wherein the cosmetic is a cream, emulsion, foam, gel, lotion, milk, mousse, ointment, paste, powder, spray, suspension, or a combination thereof.

14. The cosmetic of claim 12 , wherein the cosmetic is selected from the group consisting of: a concealing stick, foundation, stage make-up, mascara, eye shadow, hair color, lipstick, lip gloss, kohl pencil, eye liner, blusher, eyebrow pencil, cream powder, nail enamel, skin glosser stick, hair spray, face powder, leg-makeup, insect repellent lotion, nail enamel remover, perfume lotion, and shampoo.

15. The iron oxide containing effect pigment of claim 1 wherein the iron oxide containing effect pigment does not contain pseudobrookite.

16. The iron oxide containing effect pigment of claim 1 formed by a chemical vapor deposition method, comprising:

fluidizing a particulate substrate in a reaction chamber with a first inert gas;

heating the reaction chamber;

pumping a second gas into the reaction chamber, the second gas including i) oxygen, water vapor, and a second inert gas, or ii) air, water vapor, and a second inert gas; and

pumping a third inert gas including iron pentacarbonyl into the reaction chamber to form a distilled iron pentacarbonyl that reacts with the particulate substrate to form an iron oxide coating on the particulate substrate.

17. An iron oxide containing effect pigment consisting of:

a particulate substrate selected from the group consisting of one or more of natural mica, synthetic mica, TiO 2 -coated natural mica, TiO 2 -coated synthetic mica, tin oxide-coated natural mica, tin oxide-coated synthetic mica, silica, alumina, SiO 2 -coated mica, and TiO 2 -coated SnO x -coated mica wherein x is 1 or 2; and

an iron oxide coating which is in direct contact with the particulate substrate and at least partially encapsulates the particulate substrate;

wherein:

the iron oxide coating is deposited on the particulate substrate using chemical vapor deposition and the iron oxide coating comprises >98% hematite, magnetite, or maghemite; and

the iron oxide containing effect pigment comprises:

≤30.0 ppm Ba,

≤15.0 ppm Cr,

≤10.0 ppm Pb, and

≤10.0 ppm Ni,

based on the total iron oxide containing effect pigment as determined by total dissolution.

18. An iron oxide containing effect pigment of claim 17 , wherein: the particulate substrate consists of synthetic mica.

19. The iron oxide containing effect pigment of claim 1 , wherein the iron oxide containing effect pigment further comprises ≤30.0 ppm Ba; ≤10.0 ppm Pb; and ≤10.0 ppm Ni, based on the total iron oxide containing effect pigment as determined by total dissolution.

20. The iron oxide containing effect pigment of claim 1 , wherein the iron oxide containing effect pigment further comprises ≤12.0 ppm Ba; ≤1.0 ppm Pb; and ≤8.0 ppm Ni, based on the total iron oxide containing effect pigment as determined by total dissolution.

21. The method of claim 6 , wherein the iron oxide containing effect pigment further comprises ≤30.0 ppm Ba; ≤10.0 ppm Pb; and ≤10.0 ppm Ni, based on the total iron oxide containing effect pigment as determined by total dissolution.

22. The method of claim 6 , wherein the iron oxide containing effect pigment further comprises ≤12.0 ppm Ba; ≤1.0 ppm Pb; and ≤8.0 ppm Ni, based on the total iron oxide containing effect pigment as determined by total dissolution.

23. The method of claim 6 , wherein the substrate comprises synthetic mica.

Assignments (5)
NUNC PRO TUNC ASSIGNMENT Recorded Mar 18, 2023
From: BASF CORPORATION
To: BASF COLORS & EFFECTS USA LLC
Reel/Frame 063026/0239 →
NUNC PRO TUNC ASSIGNMENT Recorded Mar 18, 2023
From: COLORS & EFFECTS USA LLC F/K/A BASF COLORS & EFFECTS USA LLC
To: SUN CHEMICAL CORPORATION
Reel/Frame 063026/0296 →
CHANGE OF NAME Recorded Mar 18, 2023
From: BASF COLORS & EFFECTS USA LLC
To: COLORS & EFFECTS USA LLC
Reel/Frame 063117/0399 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Dec 22, 2017
From: BASF SE
To: BASF CORPORATION
Reel/Frame 044473/0245 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Mar 5, 2014
From: WALKER, JUERGEN; UZUNIAN, GABE; SCHMID, RAIMUND; WOSYLUS, ARON; SCHWIDETZKY, CHRISTOPH
To: BASF SE
Reel/Frame 032353/0889 →
Continuity (2)
Provisional Application 61710191 · Oct 5, 2012
Related Publication 20140099346A1 · Apr 10, 2014