Method for producing fine mesoporous silica particles, fine mesoporous silica particles, liquid dispersion of fine mesoporous silica particles, composition containing fine mesoporous silica particles and molded article containing fine mesoporous silica particles

• US 8,999,052 B2
• Filed: 05/18/2010
• Issued: 04/07/2015
• Est. Priority Date: 08/07/2009
• Status: Active Grant

• Current Assignee: Panasonic Corporation (Panasonic Holdings Corporation), University of Tokyo
• Original Assignee: Panasonic Corporation (Panasonic Holdings Corporation), University of Tokyo
• Inventors: Yabe, Hiroki, Yamaki, Takeyuki, Hoshikawa, Yasuto, Okubo, Tatsuya, Shimojima, Atsushi
• Primary Examiner(s): MCDONOUGH, JAMES E
• Application Number:
  US13/389,095
• Publication Number:
  US 20120192762A1
• Time in Patent Office: 1,785 Days
• Field of Search: 106/287.14, 106/287.1, 106/287.13
• US Class Current: 106/287.1
• CPC Class Codes: C01B 33/193 of aqueous solutions of silicates
• CPC Class Codes: C01P 2002/72 by d-values or two theta-values, e.g. as X-ray diagram
• CPC Class Codes: C01P 2002/82 by IR- or Raman-data
• CPC Class Codes: C01P 2004/64 Nanometer sized, i.e. from 1-100 nanometer
• CPC Class Codes: C01P 2006/14 Pore volume
• CPC Class Codes: C01P 2006/16 Pore diameter
• CPC Class Codes: C03C 17/007 containing a dispersed phase, e.g. particles, fibres or flakes, in a continuous phase
• CPC Class Codes: C03C 2217/42 consisting of particles only
• CPC Class Codes: C03C 2217/425 consisting of a porous layer
• CPC Class Codes: C03C 2217/478 Silica
• CPC Class Codes: C03C 2217/732 made of a single layer
• CPC Class Codes: C09C 1/30 Silicic acid
• CPC Class Codes: G02B 2207/107 Porous materials, e.g. for reducing the refractive index
• CPC Class Codes: Y10T 428/2982 Particulate matter [e.g., sphere, flake, etc.]

Abstract

Fine mesoporous silica particles are provided by which not only the functions of low reflectance (Low-n), low dielectric constant (Low-k) and low thermal conductivity but also improved strength of a molded article are achieved. The fine mesoporous silica particles are manufactured by a process including a surfactant composite fine silica particle preparation step and a mesoporous particle formation step. In the silica fine particle preparation step, a surfactant, water, an alkali and a hydrophobic part-containing additive including a hydrophobic part for increasing the volume of micelles are mixed with a silica source to thereby prepare surfactant composite fine silica particles. In the mesoporous particle formation step, the mixture is mixed with an acid and an organosilicon compound to thereby remove the surfactant and hydrophobic part-containing additive from the surfactant composite fine silica particles and provide the surface of each silica fine particle with an organic functional group. The fine mesoporous silica particles have mesopores inside each particle, and are modified on the surface with organic functional groups.

Claims

1. Fine mesoporous silica particles with a plurality of mesopores, comprising a plurality of convexities on particle surfaces of the fine mesoporous silica particles, wherein the fine mesoporous silica particles are modified on surfaces thereof with organic functional groups via siloxane bonds, the convexities are formed by protrusions of particle components and have wall surfaces separate from wall surfaces of the mesopores, the convexities are made principally of silicon oxide, a protruding height of the convexities is at least 1 nm but not more than 30 nm and the fine mesoporous silica particles are obtained by the method comprising:

preparing a surfactant composite fine silica particle in which a surfactant, water, an alkali and a hydrophobic part-containing additive including a hydrophobic part for increasing a volume of micelles are mixed with a silica source to thereby prepare surfactant composite fine silica particles; and

forming a mesoporous particle in which the surfactant composite fine silica particles are mixed with an acid and an organosilicon compound having a siloxane bond in a molecule to thereby remove the surfactant and hydrophobic part-containing additive from the surfactant composite fine silica particles and provide a surface of each silica fine particle with an organic functional group via siloxane bonds.

2. Fine mesoporous silica particles with a plurality of mesopores, comprising a plurality of convexities on particle surfaces of the fine mesoporous silica particles, wherein:

the fine mesoporous silica particles are modified on surfaces thereof with organic functional groups via siloxane bonds;

the convexities are formed by protrusions of particle components and have wall surfaces separate from wall surfaces of the mesopores;

the convexities are made principally of silicon oxide; and

a protruding height of the convexities is at least 1 nm but not more than 30 nm.

3. The fine mesoporous silica particles according to claim 2, wherein the fine mesoporous silica particles have a particle diameter of 100 nm or less.

4. A liquid dispersion of fine mesoporous silica particles, comprising the fine mesoporous silica particles according to claim 2 dispersed in a medium.

5. A composition containing fine mesoporous silica particles, the composition comprising the fine mesoporous silica particles according to claim 2 in a matrix-forming material.

6. A molded article containing fine mesoporous silica particles, obtained by molding the composition containing fine mesoporous silica particles according to claim 5.

7. The fine mesoporous silica particles according to claim 2, wherein the plurality of mesopores are 3.5 nm or more in diameter.

8. The fine mesoporous silica particles according to claim 2, wherein the plurality of mesopores are equally spaced inside each particle.

9. The fine mesoporous silica particles according to claim 2, wherein

the fine mesoporous silica particles have a particle diameter of 100 nm or less;

the plurality of mesopores are 3.5 nm or more in diameter; and

the plurality of mesopores are equally spaced inside each particle.

10. The fine mesoporous silica particles according to claim 2, wherein

the wall surfaces of the convexities and the wall surfaces of the mesopores are discontinuous;

or

the wall surfaces of the convexities and the wall surfaces of the mesopores are continuous and angles of the walls change at boundaries between the mesopores and the convexities.