Interference pigment with high color intensity and method of manufacturing the same

100 g of synthetic mica flakes having a particle size of 5 μm to 50 μm was introduced into 2 L of demineralized water, followed by stiffing these components to prepare a slurry. Next, the slurry was heated to 75° C., and a HCl solution was added thereto when the slurry reached 75° C., thereby adjusting the pH of the slurry to 3.5. Next, 340 g of an FeCl 3 solution (FeCl 3 content: 20.0 wt %) was weighed and titrated into the slurry at a constant rate over the course of 4 hours while the pH of the slurry was maintained through addition of a 10% to 50% diluted NaOH solution. After titration of the solution, the slurry was refluxed for 10 minutes, followed by adjusting the pH of the slurry to 6.8 using a 10% to 30% diluted NaOH solution.

Next, 400 g of a MgO•SiO 2 solution (MgO•SiO 2 content: 15.0 wt %) was weighed and titrated into the slurry at a constant rate over the course of 1 hour while the pH of the slurry was maintained at 6.8 using the HCl solution. After the pH of the slurry is adjusted to 3.5 by adding the HCl solution thereto, the slurry was additionally stirred for 15 minutes while refluxing the same.

Next, 400 g of an FeCl 3 solution (FeCl 3 content: 20.0 wt %) was weighed and titrated into the slurry at a constant rate over the course of 5 hours while the pH of the slurry was maintained at 3.5 using a NaOH solution. After titration of the solution, the slurry was additionally stirred for 30 minutes while refluxing the same.

After refluxing the slurry, the pH of the slurry was adjusted to 8.0 to 8.5 using a 10% to 30% diluted NaOH solution, followed by refluxing the slurry for 30 minutes and stirring the same. After completion of stirring, the final slurry was filtered and subjected to dehydration and washing with demineralized water two times, followed by drying the slurry at 120° C. for 10 hours, thereby obtaining an intermediate product as a remaining material in powder form.

Finally, 11 g of the obtained intermediate product was calcined at 800° C. for 12 minutes, thereby obtaining a bronze colored powder.

100 g of synthetic mica flakes having a particle size of 5 μm to 50 μm was introduced to 2 L of demineralized water, followed by stiffing these components, thereby preparing a slurry. Next, the slurry was heated to 75° C., and a HCl solution was added thereto when the slurry reached 75° C., thereby adjusting the pH of the slurry to 3.5. Next, 345 g of an FeCl 3 solution (FeCl 3 content: 20.0 wt %) was weighed and titrated into the slurry at a constant rate over the course of 4 hours, while the pH of the slurry was maintained through addition of a 10% to 50% diluted NaOH solution. After titration of the solution, the slurry was refluxed for 10 minutes, followed by adjusting the pH of the slurry to 6.8 using a 10% to 30% diluted NaOH solution.

Next, 450 g of a MgO•SiO 2 solution (MgO•SiO 2 content: 15.0 wt %) was weighed and titrated into the slurry at a constant rate over the course of 4 hours, the pH of the slurry was maintained at 6.8 using a 10% HCl solution. After the pH of the slurry was adjusted to 3.5 by adding the HCl solution thereto, the slurry was additionally stirred for 15 minutes while refluxing the same.

Next, 450 g of an FeCl 3 solution (FeCl 3 content: 20.0 wt %) was weighed and titrated into the slurry at a constant rate over the course of 5 hours while the pH of the slurry was maintained at 3.0 using a 10% to 50% diluted NaOH solution. After titration of the solution, the slurry was additionally stirred for 30 minutes while refluxing the same.

After refluxing the slurry, the pH of the slurry was adjusted to 8.0 to 8.5 using a 10% to 30% diluted NaOH solution, followed by refluxing the slurry for 30 minutes and stirring the same. After completion of stirring, the final slurry was filtered and subjected to dehydration and washing with demineralized water two times, followed by drying the slurry at 120° C. for 10 hours, thereby obtaining an intermediate product as a remaining material in powder form.

Finally, 11 g of the powder was calcined at 800° C. for 12 minutes, thereby obtaining a powder having a copper tone.

100 g of synthetic mica flakes having a particle size of 5 μm to 50 μm was introduced into 2L of demineralized water, followed by stirring these components so as to prepare a slurry. Next, the slurry was heated to 75° C., and a HCl solution was added thereto when the slurry reached 75° C., thereby adjusting the pH of the slurry to 3.5.

Next, 600 g of an FeCl 3 solution (FeCl 3 content: 20.0 wt %) was weighed and titrated into the slurry at a constant rate over the course of 5 hours while the pH of the slurry was maintained at 3.5 using a 10% to 50% diluted NaOH solution. After titration of the solution, the slurry was refluxed for 10 minutes, followed by adjusting the pH of the slurry to 6.8 using a 10% to 30% diluted NaOH solution.

Next, 400 g of a MgO•SiO 2 solution (MgO•SiO 2 content: 15.0 wt %) was weighed and titrated into the slurry at a constant rate over the course of 2 hours, the pH of the slurry was maintained at 6.8 using the HCl solution. After the pH of the slurry was adjusted to 3.5 by adding the HCl solution thereto, the slurry was additionally stirred for 15 minutes while refluxing the same.

Next, 570 g of an FeCl 3 solution (FeCl 3 content: 20.0 wt %) was weighed and titrated into the slurry at a constant rate over the course of 5 hours while the pH of the slurry was maintained at 3.5 using a 10% to 50% diluted NaOH solution. After titration of the solution, the slurry was additionally stirred for 30 minutes while refluxing the same.

After refluxing the slurry, the pH of the slurry was adjusted to 8.0 to 8.5 using a 10% to 30% diluted NaOH solution, followed by refluxing the slurry for 30 minutes and stirring the same. After completion of stirring, the final slurry was filtered and subjected to dehydration and washing with demineralized water two times, followed by drying the slurry at 120° C. for 10 hours, thereby obtaining an intermediate product as a remaining material in powder form.

Finally, 11 g of the powder was calcined at 850° C. for 30 minutes, thereby obtaining a powder having a russet tone.

100 g of glass flakes having a particle size of 15 μm to 100 μm was introduced into 2 L of demineralized water, followed by stirring these components, thereby preparing a slurry. Next, the slurry was heated to 75° C., and a HCl solution was added thereto when the slurry reached 75° C., thereby adjusting the pH of the slurry to 3.5.

Next, 250 g of an FeCl 3 solution (FeCl 3 content: 20.0 wt %) was weighed and titrated into the slurry at a constant rate over the course of 4 hours while the pH of the slurry was maintained at 3.5 using a 10% to 50% diluted NaOH solution. After titration of the solution, the slurry was refluxed for 10 minutes, followed by adjusting the pH of the slurry to 6.8 using a 10% to 30% diluted NaOH solution.

Next, 280 g of a MgO•SiO 2 solution (MgO•SiO 2 content: 15.0 wt %) was weighed and titrated into the slurry at a constant rate over the course of 6 hours while the pH of the slurry was maintained at 3.5 using a 10% diluted HCl solution. The HCl solution was then added to the slurry, thereby adjusting the pH of the slurry to 3.5.

Next, 400 g of an FeCl 3 solution (FeCl 3 content: 20.0 wt %) was weighed and titrated into the slurry at a constant rate over the course of 5 hours while the pH of the slurry was maintained at 3.5 using a 10% to 50% diluted NaOH solution. After titration of the solution, the slurry was additionally stirred for 30 minutes while refluxing the same.

After completion of refluxing, the final slurry was filtered and subjected to dehydration and washing with demineralized water two times, followed by drying the slurry at 120° C. for 10 hours, thereby obtaining an intermediate product which as a remaining material in powder form.

Finally, 11 g of the powder was calcined at 600° C. for 12 minutes, thereby obtaining a powder having a russet tone.

100 g of glass flakes having a particle size of 20 μm to 200 μm was introduced into 2L of demineralized water, followed by stirring these components, thereby preparing a slurry. Next, the slurry was heated to 75° C., and a HCl solution was added thereto when the slurry reached 75° C., thereby adjusting the pH of the slurry to 3.5.

Next, 300 g of an FeCl 3 solution (FeCl 3 content: 20.0 wt %) was weighed and titrated into the slurry at a constant rate over the course of 4 hours while the pH of the slurry was maintained at 3.5 using a 10% to 50% diluted NaOH solution. After titration of the solution, the slurry was refluxed for 10 minutes, followed by adjusting the pH of the slurry to 6.8 using a 10% to 30% diluted NaOH solution. Next, 300 g of a MgO•SiO 2 solution (MgO•SiO 2 content: 15.0 wt %) was weighed and titrated into the slurry at a constant rate over the course of 6 hours while the pH of the slurry was maintained at 3.5 using a 10% diluted HCl solution. The HCl solution was added to the slurry, thereby adjusting the pH of the slurry to 3.5.

Next, 500 g of an FeCl 3 solution (FeCl 3 content: 20.0 wt %) was weighed and titrated into the slurry at a constant rate over the course of 5 hours while the pH of the slurry was maintained at 3.5 using a 10% to 50% diluted NaOH solution. After titration of the solution, the slurry was additionally stirred for 30 minutes while refluxing the same.

After completion of refluxing, the final slurry was filtered and subjected to dehydration and washing with demineralized water two times, followed by drying the slurry at 120° C. for 10 hours, thereby obtaining an intermediate product as a remaining material in powder form.

Finally, 11 g of the powder was calcined at 600° C. for 12 minutes, thereby obtaining a powder having a russet tone.

Evaluation of Chroma

Table 1 shows color space values (a*, b*) of interference pigments prepared in Examples 1 to 5. The color space values were measured using a Konica Minolta Chroma meter CR-400 D65. Here, a* is the degree of red, b* is the degree of yellow, and Δa* and Δb* are changes in color space values between the pigments of Examples and Comparative Examples, which have the same substrate and color.

According to the invention, the interference pigments relate to colors between yellow and red based on the color space values. Higher Δa* and Δb* indicate higher chroma.

Here, the pigments of Comparative Examples are products prepared by coating an Fe 2 O 3 single layer onto a mica matrix or a glass flake matrix, and details are as follows:

1) R-620K: Powder of a bronze color using a mica matrix;

2) R-640K: Powder of a copper color using a mica matrix;

3) R-660K: Powder of a russet color using a mica matrix;

4) AX-660E: Powder of a russet color using a glass flake matrix; and

5) AX-660G: Powder of a russet color using a glass flake matrix.

In addition, the pigments of Examples 1 to 5 were powder coated with an Fe 2 O 3 /MgO•SiO 2 /Fe 2 O 3 multilayer structure, and details are as follows:

Here, color names of bronze, copper and russet are defined as follows:

Bronze: A medium color between yellow and orange;

Copper: A medium color between orange and red; and

Russet: A medium color between red and violet.

Referring to Table 1, from comparison of the results between the pigments of Examples 1 to 5 and Comparative Examples, it can be seen that the color space values (a*, b*) were increased after using a coating layer of the Fe 2 O 3 /MgO•SiO 2 /Fe 2 O 3 structure.

Here, since chroma increases with increasing absolute value of the colorimeter value, it can be seen that the pigments prepared in Examples 1 to 5 had improved chroma.

[Application]

Next, examples, in which the interference pigments obtained in Examples 1 to 5 were applied to paints, plastics, inks and cosmetics, will be described.

(1) Example of Pigment Applied to Paint

In this example, the interference pigment was applied to a coating paint for surfaces of automobiles.

{Basic Paint Composition}

[Polyester Resin]

Hi-Q base for mixing colors, transparent (BC-1000, NOROO Paint & Coatings Co., Ltd.)

Hi-Q LV thinner (DR-950WS, NOROO Paint & Coatings Co., Ltd.)

4 parts by weight of each of the high chroma interference pigments obtained in Examples 1 to 5 and 96 parts by weight of the polyester resin composition were mixed, and 100 parts by weight of a thinner for the polyester resin was added to the mixture to reduce viscosity to a concentration suitable for spray coating (applied at 25° C. for 14˜16 seconds using a Ford Cup #4), followed by coating the resulting material by spray coating, thereby forming a lower coating layer. An uncolored transparent surface paint of the following composition was coated onto the lower coating layer.

{Transparent Surface Paint}

Hi-Q ultraclear (NOROO Paint & Coatings Co., Ltd.)

Hi-Q ultraclear curing agent (CCH-100, NOROO Paint & Coatings Co., Ltd.)

After surface coating, the paint was exposed to air at 40° C. for 30 minutes, followed by holding the paint at 130° C. for 30 minutes for curing.

(2) Example of Pigment Applied to Plastic

A pigment composition used in coloring plastics is as follows:

Polyethylene resin (pellets): 70 parts by weight;

Each of the high chroma interference pigments obtained in Examples 1 to 5: 1 part by weight;

Zinc stearate: 0.2 parts by weight; and

Liquid paraffin: 0.1 parts by weight.

Pellets including the composition were dry-blended and subjected to extrusion.

(3) Example of Pigment Applied to Cosmetic

Lipstick composition: color cosmetics are as follows:

Hydrogenated Castor Oil: 37 parts by weight;

Octyldodecanol: 10 parts by weight;

Diisostearyl Malate: 20 parts by weight;

Ceresin: 5 parts by weight;

Euphorbia Cerifera (Candelilla) Wax: 5 parts by weight;

Dipentaerythritol Hexahydroxystearate/Hexastearate/Hexarosinate: 18.5 parts by weight;

Copernicia Cerifera (Carnauba) Wax: 3 parts by weight;

Isopropyl Lanolate: 1 part by weight;

VP/Hexadecene Copolymer: 1 part by weight;

Each of the high chroma interference pigments obtained in Examples 1 to 5 and coloring material: appropriate amount; and

Antioxidant, Preservative and Air freshener: small amounts.

A lipstick was produced from the composition.

Although the present invention has been described with reference to some embodiments in conjunction with the accompanying drawings, it should be understood that the foregoing embodiments are provided for illustrative purposes only and are not to be in any way construed as limiting the present invention, and that various modifications, changes, alterations, and equivalent embodiments can be made by those skilled in the art without departing from the spirit and scope of the invention. Therefore, the scope of the invention should be limited only by the accompanying claims and equivalents thereof.