IP Library Granted Patent US 10,729,641
Granted Patent B2
US 10,729,641 · App. 14/738,346 · Granted Aug 4, 2020

Ordered macroporous materials

Inventors: Laurent Vidal (Paris, FR); Andreas Stein (Saint Paul, MN); David Josephson (St. Louis Park, MN)
Assignees: REGENTS OF THE UNIVERSITY OF MINNESOTA; L'OREAL
A61K8/891A61K8/0279A61K8/19A61K8/25A61K8/8152A61Q1/02C01G23/047C01G49/02C09C1/02C09C1/043C09C1/24C09C1/3081C09C1/3684C09C1/407C09C3/12A61K2800/26A61K2800/412A61K2800/436A61K2800/624A61K2800/651C01P2004/03C01P2006/16C01P2006/17
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Quick Facts
Patent No.
US 10,729,641
App. No.
14/738,346
Granted
Aug 4, 2020
Kind
B2
Abstract

The present invention relates to an inorganic material comprising particles of three-dimensional ordered macroporous structure comprising spherical pores, said pores having an average pore diameter ranging from 50 nm to 10 μm, the pore diameter varying by no greater than 20%, the surface of said pores being coated by an absorber agent of the visible wavelength spectrum, said particles having an average largest dimension ranging from 1 to 50 μm, and wherein said particles are coated with at least a hydrophobic component. The invention further relates to a process for preparing said inorganic material.

Claims (32)

1. An inorganic material comprising particles of three-dimensional ordered macroporous structure comprising spherical pores,

said pores having an average pore diameter ranging from 50 nm to 10 μm,

the pore diameter varying by no greater than 20%,

the surface of said pores being coated by an absorber agent of the visible wavelength spectrum,

said particles having an average largest dimension ranging from 1 to 40 μm, and wherein

said particles are coated through an infiltration step followed by a heating step with at least a hydrophobic component selected from the group consisting of polydimethylsiloxanes (PDMS), phenyltrimethicones, phenyldimethicones, trimethylsiloxyphenyl dimethicones, phenyl trimethylsiloxy diphenylsiloxanes, diphenyl dimethicones, diphenyl methyldiphenyl trisiloxanes, and mixtures thereof, and

said hydrophobic component coating the inorganic material on its external surface and its internal surfaces of the pores within the particles.

2. An inorganic material according to claim 1 , wherein the inorganic material is a metallic oxide of metal having a valency between 1 and 6, the metal being selected from the group consisting of titanium, iron, copper, magnesium, calcium, barium, aluminium, zinc, zirconium, strontium, silicon, tin, bismuth, and cerium.

3. An inorganic material according to claim 1 , wherein the inorganic material is a metallic oxide selected from the group consisting of TiO 2 , Al 2 O 3 , ZnO, MgO, CaO, and Si x O y with x and y comprised independently from another between 0.1 and 2.

4. An inorganic material according to claim 1 , wherein the inorganic material is a metallic oxide selected from the group consisting of SiO 2 , TiO 2 , and Al 2 O 3 .

5. An inorganic material according to claim 1 , wherein the average pore diameter ranges between 50 nm and 1 μm.

6. An inorganic material according to claim 1 , wherein the average pore diameter ranges between 0.2 and 0.6 μm.

7. An inorganic material according to claim 1 , wherein the pore diameter varies by no greater than 5%.

8. An inorganic material according to claim 1 , wherein the absorber agent is selected from the group consisting of polyphenols, melanines, eumelanines, aromatic azomethines, heteroaromatic azomethines, carbon black, and black metallic oxides.

9. An inorganic material according to claim 1 , wherein the absorber agent is present in an amount ranging from 1% to 20% by weight relative to the total weight of the particles without any coating with a hydrophobic component.

10. An inorganic material according to claim 1 , wherein the absorber agent is present in an amount ranging from 3 to 10% by weight relative to the total weight of the particles without any coating with a hydrophobic component.

11. An inorganic material according to claim 1 , wherein the average largest dimension of the particles ranges from 5 to 10 μm.

12. An inorganic material according to claim 1 , wherein the hydrophobic component is a polydimethylsiloxane.

13. A process for manufacturing an inorganic material comprising particles of three-dimension ordered macroporous structure comprising spherical pores;

said pores having an average pore diameter ranging from 50 nm to 10 μm,

the pore diameter varying by no greater than 20%,

the surface of said pores being coated by an absorber agent of the visible wavelength spectrum, and

said particles having an average largest dimension ranging from 1 to 40 μm, the process comprising the steps of:

(i) providing a colloidal crystal formed of a regular array of monodisperse organic polymer particles as a template,

(ii) adding a precursor thereof, so as to produce a solid into the interstices between the monodisperse particles of the colloidal crystal and to form a solid continuous phase and a composite colloidal crystal thereof, wherein the material can optionally comprise at least one absorber agent of the visible wavelength spectrum and/or at least one precursor of an absorber agent of the visible wavelength spectrum,

(iii) removing the monodisperse particles so as to form a regular array of pores in the solid continuous phase, and

(iv) applying a coating through an infiltration step followed by a heating step onto the surface of the particles, said coating comprising at least one hydrophobic component selected from the group consisting of polydimethylsiloxanes (PDMS), phenyltrimethicones, phenyldimethicones, trimethylsiloxyphenyl dimethicones, phenyl trimethylsiloxy diphenylsiloxanes, diphenyl dimethicones, diphenyl methyldiphenyl trisiloxanes, and mixtures thereof,

said hydrophobic component coating the inorganic material on its external surface and its internal surfaces of the pores within the particles.

14. The process according to claim 13 , wherein step (iv) consists in dispersing the particles as obtained in step (iii) in a solution containing a hydrophobic component, spinning the obtained impregnated particles and carrying out a heating step at a temperature ranging from 100 to 800° C.

15. An inorganic material according to claim 1 , wherein the heating step is conducted at a temperature of 300° C. to 600° C.

16. An inorganic material according to claim 1 , wherein the hydrophobic component is fixed on said particles through said heating step.

17. An inorganic material according to claim 1 , wherein the inorganic material is a metallic oxide selected from the group consisting of TiO 2 , Fe 2 O 3 , Al 2 O 3 , CuO, ZnO, ZrO 2 , MgO, CaO, BaO, SiO 2 , SnO 2 , Bi 2 O 3 , CeO 2 , SrO 2 , BaTiO 3 , Bi 4 Ti 3 O 12 , Bi 12 SiO 20 , and Si x O y , with x and y comprised independently from another between 0.1 and 2.

Assignments (4)
CONFIRMATORY LICENSE Recorded Oct 26, 2015
From: REGENTS OF THE UNIVERSITY OF MINNESOTA
To: ENERGY, UNITED STATES DEPARTMENT OF
Reel/Frame 036985/0141 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 28, 2015
From: STEIN, ANDREAS
To: REGENTS OF THE UNIVERSITY OF MINNESOTA
Reel/Frame 036673/0379 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 28, 2015
From: JOSEPHSON, DAVID
To: REGENTS OF THE UNIVERSITY OF MINNESOTA
Reel/Frame 036673/0409 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Sep 28, 2015
From: VIDAL, LAURENT
To: L'OREAL
Reel/Frame 036673/0448 →
Continuity (1)
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