Method of producing ultraviolet protective agent composition, and ultraviolet protective agent composition obtained thereby

Patent metadata

Field	Value
Publication number	US-11629063-B2
Application number	US-201615559342-A
Country	US
Kind code	B2
Filing date	Jun 24, 2016
Priority date	Jun 26, 2015
Publication date	Apr 18, 2023
Grant date	Apr 18, 2023

Abstract

A method of producing an ultraviolet protective agent composition, which has high transparency and excellent protection ability against a light of ultraviolet region of wavelengths of 200 to 420 nm, and an ultraviolet protective agent composition obtained by the production method are provided. The method of producing an ultraviolet protective agent composition includes at least step (a) of precipitating iron oxide microparticles by mixing with a microreactor an iron oxide raw material fluid containing at least Fe3+ ion, and an iron oxide precipitation fluid containing at least a basic substance; and step (b) of dispersing the above precipitated iron oxide microparticles in a dispersion medium to obtain iron oxide microparticle dispersion, wherein a haze value of the iron oxide microparticle dispersion is 2.0% or less, and a transmittance of the iron oxide microparticle dispersion for the light of the wavelengths of 200 to 420 nm is 2.0% or less.

First claim

The invention claimed is:

1. An ultraviolet protective agent composition obtained by dispersing iron oxide microparticles in a dispersion medium,
wherein the iron oxide is α-hematite,
wherein a primary particle diameter of the iron oxide microparticles is less than 25 nm, and more than 90% of the iron oxide microparticles are single crystals,
wherein the iron oxide microparticles of single crystals are microparticles in which lattice strips are observed in one direction in the electron microscopic observation, and
wherein a haze value of a dispersion of the iron oxide microparticles is 2.0% or less, and a transmittance of the dispersion of the iron oxide microparticles for the light of the wavelengths of 200 to 420 nm is 2.0% or less.

2. The ultraviolet protective agent composition according to claim 1 , wherein the iron oxide microparticles are microparticles obtained by the following steps:
as a microreactor is used a fluid processing machine equipped with a first processing surface and a second processing surface which are disposed so as to face each other, being capable of approaching to and separating from each other, at least one of which rotates relatively to the other;
at least two fluids to be processed of an iron oxide raw material fluid and an iron oxide precipitation fluid are introduced between the first processing surface and the second processing surface;
a separation force acting in the direction of separating the first processing surface and the second processing surface is generated by an introduction pressure of the fluids to be processed between the first processing surface and the second processing surface, so that the interval between the first processing surface and the second processing surface is maintained minute by a pressure balance between the separation force and a force applied in the direction of approximating the first processing surface and the second processing surface;
the at least two fluids to be processed are merged between the first processing surface and the second processing surface which are maintained with the minute interval, and are passed between the first processing surface and the second processing surface, to form a thin film fluid; and
the at least two fluids to be processed are mixed in the thin film fluid to precipitate the iron oxide microparticles, and the fluid to be processed is discharged from the space between the first processing surface and the second processing surface, and pH of the fluid discharged from the space between the first processing surface and the second processing surface is made to be 6 to 14, to obtain the microparticles.

3. The ultraviolet protective agent composition according to claim 2 ,
wherein the introduction pressure of both fluids to be processed of the iron oxide raw material fluid and the iron oxide precipitation fluid exceeds the standard pressure, and
the temperature of the iron oxide raw material fluid to be introduced between the processing surfaces is higher than the normal boiling point of the iron oxide raw material fluid, and is lower than the boiling point under the introduction pressure.

4. The ultraviolet protective agent composition according to claim 1 , wherein the iron oxide microparticles are microparticles obtained by the following steps:
as a microreactor is used a fluid processing machine equipped with a first processing surface and a second processing surface which are disposed so as to face each other, being capable of approaching to and separating from each other, at least one of which rotates relatively to the other;
at least two fluids to be processed of an iron oxide raw material fluid and an iron oxide precipitation fluid are introduced between the first processing surface and the second processing surface;
a separation force acting in the direction of separating the first processing surface and the second processing surface is generated by an introduction pressure of the fluids to be processed between the first processing surface and the second processing surface, so that the interval between the first processing surface and the second processing surface is maintained minute by a pressure balance between the separation force and the force applied in the direction of approximating the first processing surface and the second processing surface;
the at least two fluids to be processed are merged between the first processing surface and the second processing surface which are maintained with the minute interval, and are passed between the first processing surface and the second processing surface, to form a thin film fluid;
the at least two fluids to be processed are mixed in the thin film fluid to precipitate the iron oxide microparticles, and the fluid to be processed is discharged from the space between the first processing surface and the second processing surface; and
an additional stirring treatment is performed to the fluid discharged from the space between the first processing surface and the second processing surface, and pH of the fluid discharged from the space between the first processing surface and the second processing surface after the stirring treatment is made to be 6 to 14, to obtain the microparticles.

5. A method of producing an ultraviolet protective agent composition, which comprises at least
step (a) of precipitating iron oxide microparticles by mixing with a microreactor an iron oxide raw material fluid containing at least Fe 3+ ion, and an iron oxide precipitation fluid containing at least a basic substance, and
step (b) of dispersing the above precipitated iron oxide microparticles in a dispersion medium to obtain a dispersion of the iron oxide microparticles,
wherein:
the iron oxide is α-hematite,
a primary particle diameter of the iron oxide microparticles is less than 25 nm, and more than 90% of the iron oxide microparticles are single crystals,
the iron oxide microparticles of single crystals are microparticles in which lattice strips are observed in one direction in the electron microscopic observation, and
a haze value of the dispersion of the iron oxide microparticles is 2.0% or less, and a transmittance of the dispersion of the iron oxide microparticles for the light of the wavelengths of 200 to 420 nm is 2.0% or less.

6. The method of producing an ultraviolet protective agent composition according to claim 5 , wherein a transmittance of the dispersion of the iron oxide microparticles for the light of the wavelengths of 650 to 800 nm is 80% or more.

7. The method of producing an ultraviolet protective agent composition according to claim 5 , wherein a secondary particle diameter of the iron oxide microparticles is 50 nm or less.

8. The method of producing an ultraviolet protective agent composition according to claim 5 , wherein a molar absorption coefficient of the dispersion of the iron oxide microparticles for the light of the wavelength of 400 nm is 500 L/(mol·cm) or more, and a molar absorption coefficient of the dispersion of the iron oxide microparticles for the light of the wavelength of 220 nm is 3000 L/(mol·cm) or more.

9. The method of producing an ultraviolet protective agent composition according to claim 5 , wherein the iron oxide microparticles comprise substantially spherical iron oxide microparticles.

10. The method of producing an ultraviolet protective agent composition according to claim 5 , wherein the iron oxide microparticles comprise single crystals of iron oxide microparticles.

11. The method of producing an ultraviolet protective agent composition according to claim 5 , wherein as a microreactor is used a fluid processing machine equipped with the first processing surface and the second processing surface wh

Assignees

• M Technique Co Ltd

Inventors

• Enomura Masakazu
• Honda Daisuke

Classifications

• C09C1/24

  Oxides of iron · CPC title

• A61K8/04

  Dispersions; Emulsions · CPC title

• C01P2006/60

  Optical properties, e.g. expressed in CIELAB-values · CPC title

• A61K8/19 Primary

  containing inorganic ingredients · CPC title

• C09K3/00

  Materials not provided for elsewhere · CPC title