Method for producing disintegrated silica particles

Patent metadata

Field	Value
Publication number	US-10358353-B2
Application number	US-201414908621-A
Country	US
Kind code	B2
Filing date	Aug 1, 2014
Priority date	Aug 1, 2013
Publication date	Jul 23, 2019
Grant date	Jul 23, 2019

Abstract

Silica particles calcined in a calcination step are supplied in a swirling flow generated by a gas introduced in a disintegration container and disintegrated therein, whereby the silica particles can be easily disintegrated and there can be obtained disintegrated silica particles having both low hygroscopicity and high dispersibility in resin. In addition, the introduction of dehumidified air (gas) during the disintegration reduces hygroscopicity and greatly improves dispersibility in resin. Furthermore, performing heating treatment (calcination) again after the disintegration causes the surface modification of the disintegrated silica particles, greatly improving hygroscopicity and dispersibility in resin. The resin composition obtained in this manner including silica particles provides good injectability and filterability when used for an underfill material for semiconductors and an in-plane spacer or sealing spacer of liquid crystal displays.

First claim

The invention claimed is:

1. A method for producing disintegrated silica particles, comprising:
a calcination step of producing calcined silica particles by calcining silica particles in a range from 600 to 1200° C.; and
a disintegration step of producing disintegrated silica particles by supplying the calcined silica particles in a swirling flow generated by a gas introduced in a disintegration container,
wherein in the disintegration step a solid to gas ratio W1/W2 which is a ratio between a supply amount W1 (g/Hr) of the calcined silica particles supplied into the swirling flow to a supply amount W2 (m 3 /Hr) of the introduced gas is in a range of 4.4 to 36.3 g/m 3 .

2. The method for producing disintegrated silica particles according to claim 1 , wherein the gas has a dew point of 0° C. or less.

3. The method for producing disintegrated silica particles according to claim 1 , wherein the gas has a pressure in a range from 0.1 to 1.5 MPa at an introduction section of the disintegration container.

4. The method for producing disintegrated silica particles according to claim 1 , wherein a surface modification step of performing heating treatment in a temperature range from 500 to 1100° C. is provided after the disintegration step.

5. The method for producing disintegrated silica particles according to claim 4 , wherein the surface modification step is performed in a gas atmosphere having a dew point of 0° C. or less.

6. The method for producing disintegrated silica particles according to claim 1 , wherein between the calcination step and the disintegration step, the silica particles calcined in the calcination step is cooled in a gas atmosphere having a dew point of 0° C. or less.

7. The method for producing disintegrated silica particles according to claim 1 , wherein the silica particles calcined in the calcination step are supplied into the disintegration container through an introduction inlet provided on the disintegration container; the introduction inlet and a storage unit for the calcined silica particles are in a single sealed space; and the sealed space is filled with the gas.

8. The method for producing disintegrated silica particles according to claim 1 , wherein an inner surface of the disintegration container is made of silicon carbide (SiC).

9. The method for producing disintegrated silica particles according to claim 8 , wherein the silicon carbide has been calcined at 900° C. or more.

10. The method for producing disintegrated silica particles according to claim 1 , wherein the silica particles are spray-dried silica particles obtained by spray drying a dispersion solution of silica particles having a mean particle size ranging from 10 nm to 1 μm; the spray-dried silica particles have a mean particle size ranging from 1 to 100 μm and having a moisture content ranging from 0.01 to 10% by mass; and
the calcined silica fine particles obtained by the disintegration step have a mean particle size ranging from 5 nm to 0.95 μm.

11. The method for producing disintegrated silica particles according to claim 1 , wherein the silica particles used in the calcination step are silica particles obtained by hydrolysis of a hydrolyzable organic silicon compound represented by the following formula (1) and then particle growth,
R n —SiX 4-n   (1)

(wherein each R represents a substituted or unsubstituted hydrocarbon group having 1 to 10 carbon atoms and may be the same as or different from each other; X represents an alkoxy group having 1 to 4 carbon atoms, a hydroxyl group, halogen, or hydrogen; and n represents an integer from 0 to 3).

12. The method for producing disintegrated silica particles according to claim 11 , wherein, in the preparation of the silica particles, the dispersion solution has a pH from 8 to 13 during the hydrolysis and has a pH from 8 to 13 during the particle growth, in which a range of pH changes of the dispersion solution is a range of ±1.0.

13. A method for producing disintegrated silica particles comprising:
a calcination step of producing calcined silica particles by calcining silica particles in a range from 800 to 1000° C. in an environment having an absolute humidity of 50 g/m 3 or more; and
a disintegration step of producing disintegrated silica particles by supplying the calcined silica particles in a swirling flow generated by a gas introduced in a disintegration container.

14. The method for producing disintegrated silica particles according to claim 13 , wherein, in the calcination step, the silica particles are calcined in a furnace filled with a gas containing water vapor in an amount from 100 g/m 3 to 2000 g/m 3 .

15. The method for producing disintegrated silica particles according to claim 14 , wherein after the calcination step, an inert gas having a dew point of 0° C. or less is injected into the furnace to discharge the gas containing the water vapor.

16. The method for producing disintegrated silica particles according to claim 14 , wherein after the calcination step, a cooling step is provided to cool the silica particles down to 50° C. in the furnace, and in the cooling step, the gas containing the water vapor in the furnace is replaced by an inert gas having a dew point of 0° C. or less.

17. A method for producing disintegrated silica particles, comprising:
a calcination step of producing calcined silica particles by calcining silica particles in a range from 600 to 1000° C.;
a disintegration step of obtaining disintegrated silica particles by generating a swirling flow by a gas introduced in a disintegration container, supplying the calcined silica particles in the swirling flow, and disintegrating the calcined silica particles; and
a surface modification step of heating the disintegrated silica particles in a temperature range from 800 to 1100° C. and obtaining surface-modified disintegrated silica particles,
wherein in the disintegration step a solid to gas ratio W1/W2 which is a ratio between a supply amount W1 (g/Hr) of the calcined silica particles supplied into the swirling flow to a supply amount W2 (m 3 /Hr) of the introduced gas is in a range of 4.4 to 36.3 g/m 3 .

Assignees

• Jgc Catalysts & Chemicals Ltd

Inventors

• Muraguchi Ryo
• Egami Miki
• Kumazawa Mitsuaki
• Taniguchi Masanobu
• Koyanagi Tsuguo
• Komatsu Michio
• Egami Kazutaka

Classifications

• C01B33/18 Primary

  Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof (preparation of aerogels by dehydrating gels C01B33/158; treatment to enhance the pigmenting or filling properties C09C) · CPC title