Effect pigments based on artificially produced substrates with a narrow size distribution

Abstract

The invention relates to effect pigments comprising artificial platelet-shaped substrates which have at least one optically active coating, where the effect pigments have a volume-averaged cumulative undersize distribution curve with the characteristic numbers D.sub.10, D.sub.50 and D.sub.90, said cumulative undersize distribution curve having a span ΔD of 0.7-1.4, and the span ΔD being calculated in accordance with formula (I):
ΔD=(D.sub.90−D.sub.10)/D.sub.50  (I),
and the average thickness of the artificial platelet-shaped substrates being 500 nm to 2000 nm.

Claims

1. Effect pigments consisting essentially of artificial platelet-shaped substrates which have only one optically active coating comprising TiO.sub.2 in the rutile or anatase crystal polymorph, wherein in case of the rutile polymorph, the coating is obtained by a process comprising applying SnO.sub.2 to the substrates, applying TiO.sub.2 to the applied SnO.sub.2, and then calcining the substrates, wherein the effect pigments have a volume-averaged cumulative undersize distribution curve with the characteristic numbers D.sub.10, D.sub.50 and D.sub.90, said cumulative undersize distribution curve having a span ΔD of 0.7-1.4, and the span ΔD being calculated in accordance with formula (I):
ΔD=(D.sub.90−D.sub.10)/D.sub.50  (I), and the average thickness of the artificial platelet-shaped substrates being 500 nm to 2000 nm, wherein the standard deviation of the thickness of the artificial platelet-shaped substrates is 15% to 100%, and wherein the artificial platelet-shaped substrates are substantially transparent and are selected from the group consisting of glass platelets, platelets of synthetic mica, SiO.sub.2 platelets, platelet-shaped bismuth oxychloride, platelet-shaped aluminum oxides, and mixtures thereof.

2. The effect pigments of claim 1, wherein the average thickness of the artificial platelet-shaped substrates is 750 nm to 1500 nm.

3. The effect pigments of claim 1, wherein the one optically active coating of the artificial substrates has a refractive index of n≥1.9.

4. Effect pigments consisting essentially of glass platelet-shaped substrates which have only one optically active coating comprising TiO.sub.2 in the rutile or anatase crystal polymorph, wherein in case of the rutile polymorph, the coating is obtained by a process comprising applying SnO.sub.2 to the substrates, applying TiO.sub.2 to the applied SnO.sub.2, and then calcining the substrates, wherein the effect pigments have a volume-averaged cumulative undersize distribution curve with the characteristic numbers D.sub.10, D.sub.50 and D.sub.90, said cumulative undersize distribution curve having a span ΔD of 0.7-1.4, and the span ΔD being calculated in accordance with formula (I):
ΔD=(D.sub.90−D.sub.10)/D.sub.50  (I), and the average thickness of the platelet-shaped substrates being 500 nm to 2000 nm.

5. The effect pigments of claim 4, wherein the average thickness of the artificial platelet-shaped substrates is 750 nm to 1500 nm.

6. The effect pigments of claim 4, wherein the standard deviation of the thickness of the artificial substrates is 15% to 100%.

7. The effect pigments of claim 4, wherein the one optically active coating of the artificial substrates has a refractive index of n≥1.9.

8. The effect pigments of claim 4, wherein the average thickness of the artificial platelet-shaped substrates is 750 nm to 1500 nm and the standard deviation of the thickness of the artificial substrates is 20% to 70%.

9. The effect pigments of claim 4, wherein the average thickness of the artificial platelet-shaped substrates is 750 nm to 1500 nm the span ΔD is within a range of 0.8 to 1.2.

10. The effect pigments of claim 1, wherein the standard deviation of the thickness of the artificial platelet-shaped substrates is in a range of 15% to 70%.

11. The effect pigments of claim 1, wherein the standard deviation of the thickness of the artificial platelet-shaped substrates is in a range of 20% to 70%.

12. The effect pigments of claim 1, wherein the standard deviation of the thickness of the artificial platelet-shaped substrates is in a range of 15% to 70%, and wherein the average thickness of the substrate is 750 nm to 1500 nm.

13. The effect pigments of claim 1, wherein the standard deviation of the thickness of the artificial platelet-shaped substrates is in a range of 20% to 70%, and wherein the average thickness of the substrate is 750 nm to 1500 nm.

14. The effect pigments of claim 4, wherein the average thickness of the artificial platelet-shaped substrates is 750 nm to 1500 nm, and wherein the standard deviation of the thickness of the artificial substrates is 15% to 70%.

Description

BRIEF DESCRIPTION OF THE FIGURES

(1) FIG. 1 shows a manually marked area fraction in a digital image of an effect pigment of the invention in a dried applicator drawdown.

(2) FIG. 2 shows the distribution of the color loci, calculated from the digital images of the manually marked effect pigments, in an a*b* color space.

(3) FIG. 3 shows the 90% quantile ΔC*.sub.90 of the color difference distribution.

EXAMPLES

(4) The examples below are intended to elucidate the invention in more detail, but without restricting it thereto.

Example 1

(5) A suspension of 200 g of glass flakes (average thickness: 1 μm, standard deviation of the thickness: around 40%) in DI water (around 3% by weight) (DI: deionized water: fully demineralized) is classified on a 100 μm sieve, and the sieve undersize is sieved in turn on a 63 μm sieve. This sieving procedure is repeated twice with the residue obtained on the 63 μm sieve, to give a glass flake fraction whose particle size distribution (MALVERN Mastersizer MS 2000) is as follows: D.sub.10=50 μm, D.sub.50=82 μm, D.sub.90=132 μm, Span ΔD=1.00.

Example 2

(6) 200 g of glass flakes from example 1 are suspended in 2000 ml of deionized water and the suspension is heated to 80° C. with turbulent stirring. The pH of the suspension is adjusted to 1.9 using dilute HCl and then a first layer of “SnO.sub.2” is precipitated onto the glass flakes. This layer is formed by addition of a solution consisting of 3 g of SnCl.sub.4×5H.sub.2O (in 10 ml of concentrated HCl plus 50 ml of deionized water), with simultaneous metering of 10% NaOH in order to keep the pH constant, over a period of 1 hour. In order to complete the precipitation, the suspension is stirred for a further 15 minutes. Thereafter the pH is lowered to 1.6 using dilute HCl, and a solution of 200 ml of TiCl.sub.4 (400 g TiCl.sub.4/l deionized water) is then metered into this suspension. The pH is kept at a constant 1.6 by counter-addition of 10% NaOH. This is followed by stirring for 15 minutes more and by filtration, the filter cake being rinsed with deionized water. The filter cake is then subjected to initial drying at 100° C. and to calcining at 750° C. for 30 minutes. A highly lustrous effect pigment is obtained which shows a red interference color. Microscopic investigation of the coated pigments shows extraordinary consistency in the color of the pigments.

Example 3

(7) 200 g of glass flakes from example 1 are coated by the method of example 2 with TiO.sub.2, but with metered addition of only 167 ml of TiCl.sub.4. The product after calcining is a highly lustrous effect pigment having a golden interference color. Microscopic investigation, in the same way as in example 2, shows an extraordinary consistency in color of the pigments.

Comparative Example 4

(8) Commercially available golden pearlescent “Reflecks Dimension Sparkling Gold” pigments from BASF Catalysts.

Comparative Example 5

(9) Commercially available golden pearlescent “RonaStar Golden Sparks” pigments from Merck.

(10) TABLE-US-00003 TABLE 3 Characteristic size distribution values for some inventive and comparative examples: Pigment D.sub.10 D.sub.50 D.sub.90 Span ΔD Ronastar Golden Sparks 34.0 78.4 148.7 1.46 (comparative example 4) Reflecks Dimension 35.6 84.3 175.9 1.66 Sparkling Gold (comparative example 5) Example 3 49.8 81.5 130.7 0.99

(11) Below, the inventive effect pigments of example 3, with a narrow span and high color purity, were compared in a detailed analysis with the commercially available pearlescent pigments of the comparative examples. All of the pearlescent pigments in the form of an applicator drawdown have a golden interference color which is perceptible visually to the observer.

(12) The starting point for the determination of the color purity of the inventive effect pigments were digital color microscope images of dried applicator drawdowns (produced with a paint containing 6% by weight pigments in nicrocellulose varnish (% by weight figure is based on the total weight of the paint) and knife-coated in a wet film thickness of 76 μm onto a BYK-Gardner black-white drawdown chart (byko-chart 2853), and subsequently dried at room temperature). These images were recorded using the Axioskop 2 microscope and the AxioCam digital camera from Zeiss. This equipment allowed the preparation, with the aid of the AxioVision 4.6 image-recording and image-processing software, of color-neutral digital images with a 12-bit depth of color.

(13) In order to obtain distortion-free statistical data, around 20 individual micrographs were taken at randomly selected locations on the applicator drawdowns. Over 100 individual evaluable pigments were imaged in this procedure.

(14) In FIG. 2 the color loci of the individual measurements of the three samples are plotted in the a*,b* diagram. It is clearly evident that the inventive effect pigments, in contrast to the commercially available products, have the lowest scattering in the a*-b* color space, i.e., have the purest color. The color values are situated closely together in the red-yellow quadrant of the a*-b* color space. The greatest scattering, i.e., the pigments colored with the least uniformity, is observed for the pigments of comparative example 4. This is also apparent even with the naked eye from the applicator drawdowns. A somewhat narrower scattering, but nevertheless a distribution over the green-yellow and red-yellow quadrants of the a*-b* color space, is present in the case of the Merck Ronastar pigments (Merck, Darmstadt, Germany).

(15) TABLE-US-00004 TABLE 4 ΔC*.sub.90 quantile Pigment ΔC*.sub.90 quantile Ronastar Golden Sparks 9.2 (comparative example 4) Reflecks Dimension Sparkling Gold 16.2 (comparative example 5) Example 3 2.5

(16) The 90% quantile of the color difference distribution is the lowest for the inventive effect pigments of inventive example 3, whereas the commercially available comparison products exhibit significantly higher values.

Example 6

(17) 200 g of glass flakes from example 1 are suspended in 2000 ml of deionized water and the suspension is heated to 80° C. with turbulent stirring. The pH of the suspension is adjusted to 1.9 using dilute HCl and then a first layer of “SnO.sub.2” is precipitated onto the glass flakes. This layer is formed by addition of a solution consisting of 3 g of SnCl.sub.4×5H.sub.2O (in 10 ml of concentrated HCl plus 50 ml of deionized water), with simultaneous metering of 10% NaOH in order to keep the pH constant, over a period of 1 hour. In order to complete the precipitation, the suspension is stirred for a further 15 minutes. Thereafter the pH is lowered to 1.6 using dilute HCl, and a solution of 185 ml of TiCl.sub.4 (400 g TiCl.sub.4/l deionized water) is then metered into this suspension. The pH is kept at a constant 1.6 by counter-addition of 10% NaOH. Thereafter the pH is raised to 7.5 using 5% NaOH, and stirring takes place for 15 minutes. A waterglass solution (207 g of waterglass solution, 27% SiO.sub.2, mixed with 207 g of deionized water) is then introduced slowly into the suspension, and the pH is kept constant at 7.5. This is followed by stirring for 20 minutes more, and the pH is lowered again to 1.9. Then a second layer of “SnO.sub.2” is deposited on the SiO.sub.2 surface. This layer is formed by addition of a solution consisting of 3 g of SnCl.sub.4×5H.sub.2O (in 10 ml of concentrated HCl plus 50 ml of deionized water), with simultaneous metered addition of a 10% NaOH, in order to keep the pH constant, over a period of 1 hour. In order to complete the precipitation, the suspension is stirred for a further 15 minutes. After that the pH is lowered to 1.6 using dilute HCl, and a solution of 189 ml of TiCl.sub.4 (400 g TiCl.sub.4/l deionized water) is then metered into the suspension. In the course of this procedure, the pH is kept constant at 1.6 by counter-addition of 10% NaOH. This is followed by stirring for 15 minutes more and by filtration, the filter cake being rinsed with deionized water. The filter cake is then subjected to initial drying at 100° C. and to calcining at 750° C. for 30 minutes. An extremely highly lustrous effect pigment is obtained which exhibits a color flop, with a change from a green interference color for steep viewing angles into a blue interference color at a shallow viewing angle.

(18) Presented below are cosmetic applications with the inventive effect pigments:

Example 7: Body Powder

(19) TABLE-US-00005 INCI Name Product Name % W/W Supplier A 100.00 Mica Silk Mica ad 100 www.vwr.com Talc Talc Powder 18.00 www.riedeldehaen.com Boron Nitride Softouch CCS 102 5.00 www.advceramics.com Nylon 12 Orgasol 2002 D/Nat 8.00 www.atofinachemicals.com Magnesium Stearate Magnesium Stearate 6.00 www.sigmaaldrich.com Methylparaben, Propylparaben Rokonsal SSH-1 0.30 www.biochema.com Mica (and) Iron Oxides Prestige ® Soft Bronze 9.00 www.eckart.net Effect pigment of example 2/3 — 0.10-15.00 Mica (and) Titanium Dioxide Prestige ® Magic Orange 9.00 www.eckart.net B Tridecyl Stearate (and) Tridecyl Trimellitate Lipovol MOS-130 2.00 www.lipochemicals.com (and) Dipentaerythrityl Hexacaprylate/Hexacaprate

(20) Preparation:

(21) 1. Mix components of phase A

(22) 2. Add phase B to phase A

(23) 3. Mix and dispense into suitable container

Example 8: Cream Eye Shadow

(24) TABLE-US-00006 INCI Name Product Name % W/W Supplier A 100.00 Castor Oil Castor Oil ad 100 www.riedeldehaen.com Octyl Palmitate Liponate EHP 6.00 www.lipochemicals.com Cocos Nucifera (Coconut) Oil Lipovol C-78 7.00 www.lipochemicals.com Bees Wax Ewacera 12 6.00 www.wagnerlanolin.com Isopropyl Lanolate Ewalan IP 5.00 www.wagnerlanolin.com Persea Gratissima (Avocado) Oil and Avocado Butter 7.00 www.impag.de Hydrogenated Avocado Oil Magnesium Stearate Magnesium Stearate 3.00 www.sigmaaldrich.com Bis-Hydroxyethoxypropyl Dimethicone Dow Corning 5562 7.00 www.dowcorning.com Carbinol Fluid Dimethicone/Vinyl Dimethicone Dow Corning 9701 5.00 www.dowcorning.com Crosspolymer and Silica Cosmetic Powder Phenoxyethanol (and) Methylparaben Uniphen P-23 0.30 www.induchem.com (and) Ethylparaben (and) Butylparaben B Mica (and) Iron Oxides Prestige ® Soft Breeze 21.00 www.eckart.net Effect pigment of example 2/3 — 0.10-20.00

(25) Preparation:

(26) 1. Mix phase A and heat to 85° C.

(27) 2. Mix phase B

(28) 3. Add phase B to phase A with stirring

(29) 4. In suitable container, allow to cool to room temperature

Example 9: Foundation

(30) TABLE-US-00007 INCI Name Product Name % W/W Supplier A 100.00 Hydrogenated Polydecene Ritadecene 20 9.00 www.ritacorp.com Caprylic/Capric Triglyceride Liponate GC-K 5.00 www.lipochemicals.com Prunus Amygdalus Dulcis (Sweet Sweet Almond Oil 4.00 www.jandekker.com Almond) Oil Caprylyl Trimethicone SilCare Silicone 31M50 4.00 www.clariant.com Caprylyl Methicone SilCare Silicone 41M16 3.00 www.clariant.com Steareth-2 Volpo S2 1.60 www.croda.com Steareth-20 Sympatens AS/200 G 2.40 www.kolb.ch B Talc Talc Powder 4.50 www.vwr.com Mica (and) Iron Oxides Prestige ® Soft Beige 4.00 www.eckart.net Mica (and) Titanium Dioxide Prestige ® Soft Silver 1.00 www.eckart.net Effect pigment of example 2/3 — 0.05-1.00 C Glycerin Pricerine 9090 5.00 www.brenntag.com Water Aqua ad 100 Ammonium Acryloyldimehtyltaurate/VP Aristoflex AVC 0.40 www.simon-undwerner.com Copolymer D Propylene Glycol (and) Diazolidinyl Urea Nipaguard PDU 0.40 www.simort-undwerner.com (and) Methylparaben (and) Propylparaben

(31) Preparation:

(32) 1. Heat phase A to 70° C. with stirring

(33) 2. Add components of phase B to phase A

(34) 3. Mix phase C until Aristoflex is dissolved

(35) 4. Heat the mixture to 70° C.

(36) 5. Add phase C to phase AB

(37) 6. Allow to cool to 40° C., and add phase D

Example 10: Lip Gloss

(38) TABLE-US-00008 INCI Name Product Name % W/W Supplier A 100.00 Hydrogenated Polyisobutene (and) Versagel ME 750 ad 100 www.penreco.com Ethylene/Propylene/Styrene Copolymer (and) Butylene/Ethylene/Styrene Copolymer Simmondsia Chinensis (Jojoba) Seed Oil Jojoba Oil - 2.00 www.biochemica.com Natural/Golden Caprylyl Trimethicone Silcare Silicone 31M50 7.00 www.clariant.com Stearyl Dimethicone Silcare Silicone 41M85 3.20 www.clariant.com Hydrogenated Polydecene Nexbase 2002 4.00 www.jandekker.com Isopropyl Myristate Isopropyl Myristate 4.50 www.vwr.com B Effect pigment of example 2/3 — 0.01-2.00 Propylparaben Propyl-4-hydroxybenzoate 0.20 www.sigmaaldrich.com

(39) Preparation:

(40) 1. Heat phase A to 85° C.

(41) 2. Add phase B to phase A, mix and then dispense into suitable container

Example 11: Lip Liner

(42) TABLE-US-00009 INCI Name Product Name % W/W Supplier A 100.00 Hydrogenated Coco-Glycerides Softisan 100 12.35 www.sasolwax.com Candelilla Wax Ewacera 42 14.00 www.wagnerlanolin.de Magnesium Stearate Magnesium Stearate 6.00 www.sigmaaldrich.com Stearic Acid Kortacid 1895 8.50 www.akzonobel.com Hydrogenated Coconut Oil Lipex 401 8.00 www.karlshamns.com Cetyl Palmitate Walrath synthetic 7.00 www.kahlwax.de Caprylic/Capric Triglyceride Liponate GC-K 3.50 www.lipochemicals.com Soybean Glycerides (and) Butyrospermum Lipex L'sens ad 100 www.karlshamns.com Parkii Tocopheryl Acetate D,L-Alpha- 0.25 www.dsm.com Tocopherol acetate Methylparaben; Propylparaben Rokonsal SSH-1 0.30 www.biochema.com B Mica (and) Titanium Dioxide (and) Ferric Prestige ® Sapphire 7.50 www.eckart.net Ferrocyanide Mica (and) Iron Oxides Prestige ® Copper 7.50 www.eckart.net Mica (and) Titanium Dioxide Prestige ® Soft Silver 5.00 www.eckart.net Effect pigment of example 2/3 — 0.10-10.00

(43) Preparation:

(44) 1. Heat phase A to 85° C.

(45) 2. Add phase B to phase A, mix and then dispense into suitable container

Example 12: Lip-Stick

(46) TABLE-US-00010 INCI Name Product Name % W/W Supplier A 100.00 Carnauba Wax Ewacera 34 4.50 www.wagnerlanolin.de Bees Wax Ewacera 12 3.50 www.wagnerlanolin.de Candelilla Wax Ewacera 42 4.00 www.wagnerlanolin.de Microcrystalline Wax Parcera MW 7.20 www.paramelt.com Cetyl Palmitate Walrath synthetic 2.00 www.kahlwax.de Hydrogenated Coco-Glycerides Softisan 100 5.00 www.sasolwax.com Petrolatum Penreco Blond 5.80 www.penreco.com Cetearyl Octanoate Luvitol EHO 10.70 www.basf.com Tocopheryl Acetate D,L-Alpha- 0.50 www.dsm.com Tocopherol acetate Castor Oil Castor Oil ad 100 www.riedeldehaen.com B Mica (and) Iron Oxide Prestige ® Fire-red 16.00 www.eckart.net Effect pigment of example 2/3 — 0.01-5.00 Methylparaben, Propylparaben Rokonsal SSH-1 0.20 www.biochema.com

(47) Preparation:

(48) 1. Heat phase A to 85° C.

(49) 2. Add phase B to phase A; after mixing at 75° C. dispense into suitable container

Example 13: Liquid Eyeliner

(50) TABLE-US-00011 INCI Name Product Name % W/W Supplier A 100.00 Water Aqua ad 100 Water/carbon black dispersion MBD 201 3.00 www.geotech.nl Acrylates Copolymer Covacryl E14 10.00 www.lcw.fr Magnesium Aluminium Silicate Veegum HV 1.00 www.cherbsloeh.de B Propylene Glycol 1,2 Propanediol 3.00 www.vwr.com Triethanolamine Triethanolamine 1.40 www.vwr.com C Xanthan Gum Keltrol T 0.30 www.cpkelco.com D Effect pigment of example 2/3 — 0.10-5.00 Mica Silk Mica 2.00 www.vwr.com E Stearic Acid Kortacid 1895 2.80 www.akzonobel.de Glyceryl Stearate Aldo MS K FG 0.80 www.lonza.com Oleyl Alcohol HD-Ocenol 90/95 V 0.50 www.biesterfeld.com Phenoxyethanol (and) Methylparaben Uniphen P-23 0.50 www.induchem.com (and) Ethylparaben (and) Butylparaben F Dimethicone (and) Trisiloxane Dow Corning 2-1184 Fluid 5.00 www.dowchemicals.com

(51) Preparation:

(52) 1. Disperse Veegum into phase A

(53) 2. Stir for 15 minutes

(54) 3. Add phase B to phase A

(55) 4. Add phase C to phase AB

(56) 5. Stir for 10 minutes

(57) 6. Add phase D to phase ABC and heat to 75° C.

(58) 7. Heat phase E to 75° C.

(59) 8. Add phase E to phase ABCD

(60) 9. Allow to cool to 60° C., and add phase F

Example 14: Mascara

(61) TABLE-US-00012 INCI Name Product Name % W/W Supplier A 100.00 Water Aqua ad 100 Propylene Glycol 1,2-Propanediol 1.50 www.vwr.com Effect pigment of example 2/3 — 0.10-8.00 Cosmetic Black Oxide C 33-134 Cosmetic Black Oxide 7.00 www.sunchemical.com Caprylic/Capric Triglyceride Liponate GC-K 2.00 www.lipochemicals.com Hydroxyethylcellulose Cellosize HEC QP-52000H 0.30 www.dow.com Magnesium Alumium Silicate Veegum HV 1.80 www.rtvanderbilt.com B Carnauba Wax Ewacara 34 3.00 www.wagnerlanolin.de Bees Wax Ewacara 12 3.00 www.wagnerlanolin.de Glyceryl Stearate Imwitor 960 K 3.00 www.sasolwax.com Cetyl Alcohol Cetyl Alcohol 3.80 www.vwr.com Polysorbate 60 Tween 60 V 1.00 www.uniqema.com PVP/VA Copolymer Luviskol VA 64 2.00 www.basf.com C Water Aqua 4.00 BHT Tenox BHT Kosher 0.10 www.eastman.com Methylparaben Methyl-4-hydroxybenzoate 0.20 www.sigmaaldrich.com

(62) Preparation:

(63) 1. Heat phase A to 85° C. with stirring

(64) 2. Heat phase B to 85° C.

(65) 3. Add phase B to phase A

(66) 4. Allow to cool to 55° C. with stirring

(67) 5. Add phase C, mix, dispense into suitable container

Example 15: Mousse

(68) TABLE-US-00013 INCI Name Product Name % W/W Designated use A 100.00 Cyclopentasiloxane Dow Corning 245 Fluid 8.60 www.dowcorning.com Hydrogenated Polyisobutene MC 30 4.00 www.sophim.com Dimethicone (and) Dimethicone Dow Corning 9041 Silicone ad 100 www.dowcorning.com Crosspolymer Elastomer Blend Squalane Squalane 5.74 www.impag.de Isononyl Isononanoate Dermol 99 10.16 www.alzointernational.com Hydrogenated Jojoba Oil Jojoba Butter LM 2.15 www.desertwhale.com Hydrogenated Jojaba Oil Jojoba Butter HM 1.00 www.desertwhale.com C30-45 Alkyl Methicone (and) C30-45 Dow Corning AMS-C30 Cosmetic 1.15 www.dowcorning.com Olefin Wax Stearyl Dimethicone Dow Corning 2503 Cosmetic Wax 0.47 www.dowcorning.com Cyclopentasiloxane (and) Dow Corning 670 Fluid 5.00 www.dowcorning.com Polypropylsilsesquioxane B Dimethicone/Vinyl Dimethicone Dow Corning 9506 Powder 16.02 www.dowcorning.com Crosspolymer Silica Dimethyl Silylate Covasilic 15 0.17 www.lcw.fr Talc Talc Powder 5.00 www.riedeldehaen.com Mica (and) Titanium Dioxide (and) Iron Prestige ® Soft Beige 5.00 www.eckart.net Oxides Effect pigment of example 2/3 — 0.05-10.00 C Propylene Glycol, Diazolidinyl Urea, Germaben II 0.40 www.ispcorp.com Methylparaben, Propylparaben

(69) Preparation:

(70) 1. Mix phase A, heat until all is melted

(71) 2. Premix phase B with speed mixer (2400 rpm, 1 min)

(72) 3. Add half of melted phase A to phase B, mix in speed mixer (2400 rpm, 30 s)

(73) 4. Add remainder of phase A to phase B and mix in speed mixer (2400 rpm, 30 s)

(74) 5. Add phase C, mix in speed mixer (2400 rpm, 30 s), allow to cool to room temperature

Example 16: Nail Polish

(75) TABLE-US-00014 INCI Name Product Name % W/W Supplier A 100.00 Effect pigment of example 2/3 — 0.05-3.50 B International Lacquers Nailpolish & Butyl acetate (and) Ethyl 100 ad www.internationallacquers.lu Care Base 359 acetate (and) Nitrocellulose (and) Isopropyl Alcohol

(76) Preparation:

(77) 1. Mix phases A and B with stirring

(78) 2. Dispense into suitable container

Example 17: Pressed Eye Shadow

(79) TABLE-US-00015 INCI Name Product Name % W/W Supplier A 100.00 Mica Silk Mica 17.00 www.vwr.com Boron Nitride Softouch CCS 1002 2.50 www.advceramicscos.com Talc Talc Powder ad 100 www.riedeldehaen.com Zinc Stearate Kemilub EZ-V 7.00 www.undesa.com Mica (and) Iron Oxides Prestige ® Bright Fire-red 39.00 www.eckart.net Effect pigment of example 2/3 — 0.05-8.00 B Dimethicone Dow Corning ® 200 Fluid 5 5.00 www.dowcorning.com cst Cyclomethicone (and) Dimethicone Dow Corning ® 9040 5.00 www.dowcorning.com Crosspolymer Elastomer

(80) Preparation:

(81) 1. Mix phase A

(82) 2. Add phase B and homogenize

(83) 3. Press eyeshadow at 150 bar for 30 minutes

Example 18: Pressed Powder

(84) TABLE-US-00016 INCI Name Product Name % W/W Supplier A 100.00 Talc Talc Powder ad 100 www.riedeldehaen.com Zinc Stearate Kemilub EZ-V 5.00 www.undesa.com Methylparaban, Propylparaben Rokonsal SSH-1 0.30 www.biochema.com Polyethylene Asensa CL 111 20.50 www.honeywell.com Silica Syloblanc 34 1.50 www.gracedavision.com Mica (and) Titanium Dioxide Prestige ® Soft Silver 6.00 www.eckart.net Mica (and) Titanium Dioxide (and) Iron Prestige ® Soft Beige 11.00 www.eckart.net Oxides Effect pigment of example 2/3 — 0.05-8.00 B Octyl Palmitate Liponate EHP 3.00 www.lipochemicals.com

(85) Preparation:

(86) 1. Mix phase A

(87) 2. Add phase B and homogenize

(88) 3. Press eyeshadow at 150 bar for 30 minutes

Example 19: Shower Gel

(89) TABLE-US-00017 INCI Name Product Name % W/W Supplier A 100.00 Effect pigment of example 2/3 — 0.01-1.00 Water Aqua ad 100 Blue 1 (0.5% aqueous solution) FD&C Blue No. 1 0.10 www.sunchemicals.com Acrylates/C10-30 Alkyl Acrylate Carbopol ETD 2020 1.00 www.noveon.com Crosspolymer Propylene Glycol 1,2-Propanediol 1.00 www.vwr.com B TEA- Lauryl Sulfate Texapon T 42 22.00 www.cognis.com Cocamide Dea Rewomid DC 212 S 3.00 www.degussa.com Cocamidopropyl Betaine Tego Betain F 50 4.00 www.cognis.com Disodium EDTA Edeta BD 0.05 www.basf.com C Triethanolamine Triethanolamine 0.30 www.vwr.com Phenoxyethanol, Ethylhexylglycerin Euxyl PE 9010 0.60 www.schuelke-mayr.com

(90) Preparation:

(91) 1. Disperse Carbopol in phase A

(92) 2. Heat to 65° C.

(93) 3. Gradually add ingredients from phase B

(94) 4. Allow to cool with stirring, at 40-45° C. add phase C

Example 20: Styling Soft Wax

(95) TABLE-US-00018 INCI Name Product Name % W/W Supplier A 100.00 Effect pigment of example 2/3 — 0.01-2.00 Water Aqua ad 100 Propylene Glycol 1,2 Propanediol 2.00 www.vwr.com Glycerin Pricerine 9090 7.00 www.uniqema.ccm Methoxy PEG/PPG-7/3 Aminopropyl Abil Soft AF 100 0.50 www.degussa.com Dimethicone B Isosteareth-20 Procol IS-20 14.50 www.protameen.com Laureth-4 Genapol LA 040 10.00 www.clariant.com Paraffinum Liquidium Paraffinum Liquidium 6.00 www.heess.de C12-15 Alkyl Benzoate Sympatens- LBZ 8.00 www.kolb.ch C Phenoxyethanol (and) Methylparaben (and) Phenonip 0.40 www.clariant.com Butylparaben (and) Ethylparaben (and) Propylparaben (and) Isobutylparaben Fragrance Cool Floral OA D 0.10 www.bell-europe.com

(96) Preparation:

(97) 1. Heat phases A and B separately to 90° C.

(98) 2. Add phase B to phase A with stirring

(99) 3. Allow to cool to 55° C.

(100) 4. Add phase C and dispense into a suitable container

Example 21: Sun Protection Cream

(101) TABLE-US-00019 INCI Name Product Name % W/W Supplier A 100.00 Sorbitan Stearate (and) Methyl Glucose Sympatens-O/2500 G 5.00 www.kolb.ch Sesquistearte Stearic Acid Kortacid 1895 4.00 www.akzonobel.com Octyldodecanol Eutanol G 9.00 www.cognis.com Caprylic/Capric Triglyceride Liponate GC-K 10.00 www.lipochemicals.com Cetearyl Alcohol Lanette O 2.00 www.cognis.com Macadamia ternifolia Seed Oil Macadamia Nut Oil 3.20 www.jandekker.com Octyl Methoxycinnamate Parsol MCX 1.00 www.dsm.com Butyl Methoxydibenzoylmethane Parsol 1789 5.00 www.roche.com B Effect pigment of example 2/3 — 0.05-3.00 Water Aqua ad 100 Glycerin Pricerine 9090 3.20 www.uniqema.com C Phenoxyethanol (and) Methylparaben Uniphen P-23 0.40 www.induchen.com (and) Ethylparaben (and) Butylparaben Fragrance Nivamar BM 0.15 www.bell-europe.com

(102) Preparation:

(103) 1. Heat phases A and B separately to 80° C.

(104) 2. Add phase A to phase B with stirring

(105) 3. Allow to cool to 45° C.

(106) 4. Add phase C

Example 22: Transparent Lipstick

(107) TABLE-US-00020 INCI Name Product Name %W/W Supplier A 100.00 Ethylenediamine/Hydrogenated Dimer Sylvaclear A2614V 28.00 www.arizonachemical.com Dilinoleate Copolymer Bis-Di-C14-18 Alkyl Amide Bis-Stearyl Ethylenediamine/Neopentyl Sylvaclear C75V 28.00 www.arizonachemical.com Glycol/Hydrogenated Dimer Dilinoleate Paraffinum Liquidum Paraffinum Liquidum 13.80 www.heess.de Macadamia Integrifolia Seed Oil Floramac Hawaiian ad 100 www.floratech.com Macadamia Oil-Refined Isopropyl Myristate Isopropyl Myristate 6.00 www.vwr.com C12-15 Alkyl Benzoate Sympatens-LBZ 6.00 www.kolb.ch Caprylic/Capric Triglyceride Miglyol 812 7.00 www.sasolwax.com Propylparaben Propyl-4-hydroxybenzoate 0.20 www.sigmaaldrich.com B Effect pigment of example 2/3 — 0.01-3.50

(108) Preparation:

(109) 1. Heat phase A to 85° C.

(110) 2. Add phase B to phase A and mix

(111) 3. Dispense into lipstick mold at 75° C.

Example 23: Body Lotion Water-In-Silicone

(112) TABLE-US-00021 INCI Name Product Name %W/W Supplier A 100.00 Cyclopentasiloxane (and) Dimethiconol Dow Corning 1501 11.50 www.dowcorning.com Cyclopentasiloxane Dow Corning 245 5.75 www.dowcorning.com Cyclopentasiloxane (and) PEG/PPG/- Dow Corning 5225 C 13.80 www.dowcorning.com 18/18 Dimethicone C 30-45 Alkyl Methicone Dow Corning Cosmetic Wax 3.45 www.dowcorning.com AMS-C30 Effect pigment of example 2/3 — 0.05-3.50 C Polysorbate 20 Tween 20 0.60 www.uniqema.com Phenoxyethanol (and) Methylparaben Uniphen P-23 0.35 www.induchem.com (and) Ethylparaben (and) Butylparaben Sodium Chloride Sodium Chloride 0.75 www.vwr.com Water Aqua ad 100

(113) Preparation:

(114) 1. Mix phase A and heat to 75° C.

(115) 2. Mix phase B and heat to 70° C.

(116) 3. Add phase B slowly to phase A, with homogenization, and allow to cool with stirring

Example 24: Tinted Day Cream

(117) TABLE-US-00022 INCI Name Product Name % W/W Supplier A 100.00 Mica (and) Titanium Dioxide (and) Iron Prestige ® Soft Beige 1.00 www.eckart.net Oxides Mica (and) Titanium Dioxide Prestige ® Soft Red 2.00 www.eckart.net Effect pigment of example 2/3 — 0.05-3.00 Silica Syloblanc 34 3.00 www.gracedavision.com Glycerin Pricerine 9090 5.00 www.uniqema.com Allantoin Allantoin 0.40 www.3v.com Mica Silk Mica 3.00 www.vwr.com Boron Nitride Boroneige #1501 1.50 www.esk.com Water ad 100 Xanthan Gum Keltrol T 0.20 www.cpkelco.com B Glyceryl Stearate (and) Lipomulse 165 2.00 www.lipochemicals.com PEG-100 Stearate Ceteryl Alcohol (and) Cetearyl Glucoside Montanov 68 2.20 www.seppic.com Dimethicone Dow Corning 200 1.00 www.dowcorning.com Fluid/350 cst Cetearyl Isononanoate Tego Soft CI 5.10 www.degussa.com Octyldodecanol Eutanol G 4.00 www.cognis.com Butyrospernum Parkii (Shea Butter) Shea Butter 3.80 www.jandekker.com C Phenoxyethanol (and) Methylparaben Uniphen-23 0.40 www.permcos.com (and) Ethylparaben (and) Butylparaben Fragrance Sensuality 0.10 www.drom.de

(118) Preparation:

(119) 1. Mix phase A, disperse Keltrol

(120) 2. Heat to 80° C.

(121) 3. Heat phase B to 80° C.

(122) 4. Add phase B slowly to phase A

(123) 5. Allow to cool to 40° C., and add phase C

Example 25: Hair Mascara

(124) TABLE-US-00023 INCI Name Product Name % W/W Supplier A 100.00 Polyquaternium-16 Luviquat FC 905 (Luviquat 2.70 www.basf.com Exellence) Propylene Glycol 1,2-Propanediol 1.80 www.vwr.com Methylparaben Methyl-4-hydroxybenzoate 0.20 www.sigmaaldrich.com Aqua Water ad 100 B Cetearyl Alcohol Lanette O 5.00 www.cognis.com Dimethicone Dow Corning 200 Fluid/350 cst 1.00 www.dowcorning.com Ceteareth-25 Cremophor A 25 2.00 www.basf.com Propylparaben Propyl-4-hydroxybenzoate 0.10 www.sigmaaldrich.com C Hydroxypropylcellulose Klucel G 0.50 www.herc.com Magnesium Aluminium Silicate Veegum HV 0.50 www.rtvanderbilt.com Aqua Water 19.00 D Effect pigment of example 2/3 — 0.10-8.00 Phenoxyethanol (and) Phenonip 0.20 www.clariant.com Methylparaban (and) Butylparaben (and) Ethylparaben (and) Propylparaben (and) Isobutylparaben Fragrance Blue Shadow OKO 0.05 www.bell-europe.com

(125) Preparation:

(126) 1. Heat phases A and B separately to 80° C.

(127) 2. Add phase B slowly to phase A

(128) 3. In separate vessel, stir Klucel and Veegum into the water of phase C

(129) 4. Allow phase AB to cool to 40° C.

(130) 5. Add phases C and D

Example 26: Perfume Powder Stick

(131) TABLE-US-00024 INCI Name Product Name % W/W Supplier A 100.00 Dimethicone/Vinyl Dimethicone Dow Corning 9701 Cosmetic ad 100 www.dowcorning.com Crosspolymer and Silica Powder Talc Talc Powder 29.00 www.riedeldehaen.com Amorphoeus Silica Spheron P-1500 1.00 www.cheshamchemicals.co.uk Effect pigment of example 2/3 — 0.05-8.00 B Fragrance Moisturadiance 5.00 www.drom.com

(132) Preparation:

(133) 1. Mix phase A in speed mixer (30 s/2000 rpm)

(134) 2. Add phase B to phase A and mix in speed mixer (30 s/2500 rpm)

(135) 3. Dispense into suitable container

Example 27: Pressed Blush

(136) TABLE-US-00025 INCI Name Product Name % W/W Supplier A 100.00 Mica Silk Mica ad 100 www.vwr.com Nylon 12 Orgasol 2002D/Nat 3.20 www.atofinachemicals.com Boron Nitride Boroneige #1501 3.00 www.esk.com Talc Talc Powder 15.00 www.riedeldehaen.com Zinc Stearate Kemilub EZ-V 2.00 www.undesa.com Effect pigment of example 2/3 — 0.05-8.00 B Octyl Palmitate Liponate EHP 8.00 www.lipochemicals.com

(137) Preparation:

(138) 1. Mix phase A

(139) 2. Add phase B and homogenize

(140) 3. Press blush at 150 bar for 30 s