Scaly silica particles and hardenable composition containing them

• US 6,534,176 B2
• Filed: 12/06/2000
• Issued: 03/18/2003
• Est. Priority Date: 12/10/1999
• Status: Expired due to Term

• Current Assignee: AGC Si-Tech Co., Ltd. (AGC, Inc.)
• Original Assignee: Asahi Glass Company, Limited (AGC, Inc.), Dohkai Chemical Industry Co., Ltd.
• Inventors: Minohara, Shikou, Ohba, Yoshimi, Inoue, Masaki, Sasaki, Takayoshi, Fujii, Atsunari, Terase, Kunihiko
• Primary Examiner(s): Kiliman, Leszek
• Application Number:
  US09/729,822
• Publication Number:
  US 20010003358A1
• Time in Patent Office: 832 Days
• Field of Search: 428/403, 428/404, 428/407, 106/425, 106/436, 106/444, 106/446, 106/454, 106/482, 106/492, 502/239, 502/243
• US Class Current: 428/403
• CPC Class Codes: C01B 33/12 Silica; Hydrates thereof, e.g. lepidoic silicic acid
• CPC Class Codes: C09J 11/04 inorganic
• CPC Class Codes: Y10T 428/2991 Coated
• CPC Class Codes: Y10T 428/2993 Silicic or refractory material containing [e.g., tungsten oxide, glass, cement, etc.]
• CPC Class Codes: Y10T 428/2996 Glass particles or spheres
• CPC Class Codes: Y10T 428/2998 including synthetic resin or polymer
• CPC Class Codes: Y10T 428/31627 Next to aldehyde or ketone condensation product
• CPC Class Codes: Y10T 428/31656 With metal layer
• CPC Class Codes: Y10T 428/31794 Of cross-linked polyester

Abstract

Scaly silica particles having a laminated structure, consisting essentially of secondary particles of foliar silica, each formed by a plurality of flaky primary particles of scaly silica which are overlaid one on another and aligned face-to-face in parallel with one another, said secondary particles being present independent of one another.

Claims

1. Scaly silica particles having a laminated structure, consisting essentially of:

secondary particles of foliar silica;

wherein each of said secondary particles is formed by a plurality of primary particles of scaly silica which are overlaid one on another and aligned face-to-face in parallel with one another; and

wherein said secondary particles are present independent of one another.

2. The scaly silica particles according to claim 1, which have a pore distribution as measured by a nitrogen adsorption method, such that the pore diameters have a sharp peak at from 2 to 6 nm.

3. The scaly silica particles according to claim 1, wherein the secondary particles of foliar silica are a layered polysilicic acid.

4. The scaly silica particles according to claim 1, wherein the main peak in the X-ray diffraction analysis of the silica particles corresponds to silica X, silica Y or both.

5. A hardenable composition, comprising:

scaly silica particles having a laminated structure, consisting essentially of secondary particles of foliar silica; and

a volatile liquid;

wherein each of said secondary particles is formed by a plurality of primary particles of scaly silica which are overlaid one on another and aligned face-to-face in parallel with one another; and

wherein said secondary particles are present independent of one another.

6. The hardenable composition according to claim 5, further comprising a low-volatile substance which does not substantially evaporate at a temperature at which said volatile liquid evaporates.

7. The hardenable composition according to claim 6, wherein the low-volatile substance is at least one low-volatile substance selected from the group consisting of an organic polymer substance or a precursor substance for forming an organic polymer substance by a polymerization reaction, a substance having adsorbing and desorbing functions, a substance having a catalytic function, a substance having an optical function and a metal compound.

8. The hardenable composition according to claim 5, wherein a content of the scaly silica is from 1 to 80 mass %, as calculated as SiO₂.

9. The hardenable composition according to claim 5, further comprising a heat insulating material.

10. The hardenable composition according to claim 9, wherein the heat insulating material is at least one member selected from the group consisting of microballoons, porous particles and fibrous materials.

11. A hardened product, comprising:

secondary particles of foliar silica formed by a plurality of primary particles of scaly silica overlaid one on another and aligned face-to-face in parallel with one another;

wherein the secondary particles are laminated in parallel with one another.

12. The hardened product according to claim 11, which is formed on a substrate to have a layered structure.

13. The hardened product according to claim 12, further comprising a transparent organic polymer substance;

wherein an average particle size of the secondary particles of foliar silica is less than 1 μ

m; and

wherein said hardened product is substantially transparent;

wherein a transmittance of light having a wavelength of 500 nm is at least 70%, as calculated for a layer thickness of 50 μ

m.

14. A process for producing scaly silica particles suitable for a hardenable composition, comprising:

(1) subjecting either silica hydrogel, silica sol or hydrous silicic acid to hydrothermal treatment in the presence of an alkali metal salt to form tertiary agglomerated particles of scaly silica comprising secondary particles of foliar silica, each formed by a plurality of primary particles of scaly silica which are overlaid one on another and aligned face-to-face in parallel with one another, and tertiary particles formed by the secondary particles which are overlaid one on another three dimensionally irregularly to have pore spaces; and

(2) disintegrating and dispersing the tertiary agglomerated particles of scaly silica to form foliar silica particles consisting essentially of secondary particles containing substantially no tertiary particles;

wherein said hardenable composition consist essentially of secondary particles of foliar silica which have a laminated structure; and

wherein the secondary particles are present independent of one another.

15. The process for producing scaly silica particles according to claim 14, wherein said silica hydrogel has a SiO₂ concentration of from 15 to 75 mass %.

16. The process for producing scaly silica particles according to claim 14, wherein said silica hydrogel is subjected to hydrothermal treatment;

wherein a temperature of the hydrothermal treatment is from 150 to 220°

C.;

wherein the total molar ratio of SiO₂/Me₂O is from 4 to 15 mol/mol; and

wherein Me is an alkali metal.

17. The process for producing scaly silica particles according to claim 14, wherein the disintegration and dispersion of the tertiary agglomerated particles of silica are carried out using a wet system pulverizing apparatus.

18. The process for producing scaly silica particles according to claim 17, wherein the disintegration and dispersion of the tertiary agglomerated particles of silica are carried out using a high speed mechanical stirring wet system pulverizing apparatus employing medium beads.