Method for producing purified alkali silicate aqueous solution and silica sol

Patent metadata

Field	Value
Publication number	US-9938155-B2
Application number	US-201514690946-A
Country	US
Kind code	B2
Filing date	Apr 20, 2015
Priority date	Sep 5, 2011
Publication date	Apr 10, 2018
Grant date	Apr 10, 2018

Abstract

To provide a method for producing an alkali silicate aqueous solution containing a reduced amount of foreign substance of plate-like fine particles and a method for producing a silica sol containing a reduced amount of foreign substance of plate-like fine particles. A method for producing an alkali silicate aqueous solution fulfilling the following condition: the existing amount of plate-like fine particles having a length of one side of 0.2 to 4.0 μm and a thickness of 1 to 100 nm is determined to be 0 to 30%. The method for producing an alkali silicate aqueous solution includes the steps of adjusting a silica concentration of an alkali silicate aqueous solution to 0.5 to 10.0% by mass and filtering the alkali silicate aqueous solution through a filter having a removal rate of particles with a primary particle size of 1.0 μm of 50% or more.

First claim

The invention claimed is:

1. A method for producing a silica sol fulfilling the following condition:
an existing amount of plate-like fine particles having a length of one side of 0.2 to 4.0 μm and a thickness of 1 to 100 nm is determined to be 0 to 30% in accordance with a measurement method A, the method for producing a silica sol comprising the steps of:
preparing an active silicic acid solution by subjecting a purified alkali silicate aqueous solution to cation-exchange;
adding the active silicic acid solution into an alkaline aqueous solution to obtain a mixture; and
heating the mixture to polymerize active silicic acid,
wherein a method for producing the purified alkali silicate aqueous solution comprises the steps of:
adjusting a silica concentration of an alkali silicate aqueous solution to 0.5 to 10.0% by mass; and
filtering the alkali silicate aqueous solution through a filter having a removal rate of particles with a primary particle size of 1.0 μm of 50% or more, and
wherein:
the measurement method A is a method in which 30 mL of an alkali silicate aqueous solution at 25° C. adjusted to have a silica concentration of 4% by mass is passed through a membrane type filter (filtration area: 4.90 cm 2 ) having an absolute pore size of 0.4 μm, then the membrane type filter is observed by a scanning electron microscope at a magnification of 5,000 times, presence of one or more of plate-like fine particles in one visual field of a 15-by-20 μm rectangle is regarded as one count, presence or absence of the count in each of 100 visual fields that are not overlapped with each other is determined, and the total number of the obtained counts is regarded as an existing amount (%) of the plate-like fine particles, and
the filter in the filtering step is a membrane type filter having an absolute pore size of 0.3 to 3.0 μm.

2. The method for producing a silica sol according to claim 1 , wherein the alkali component in the alkaline aqueous solution is at least one selected from the group consisting of an alkali metal ion, an ammonium ion, an amine compound, and a quaternary ammonium ion.

3. A method for producing a silica sol fulfilling the following condition:
an existing amount of plate-like fine particles having a length of one side of 0.2 to 4.0 μm and a thickness of 1 to 100 nm is determined to be 0 to 30% in accordance with a measurement method A, the method for producing a silica sol comprising the steps of:
preparing an active silicic acid solution by subjecting a purified alkali silicate aqueous solution to cation-exchange;
adding the active silicic acid solution into an alkaline aqueous solution to obtain a mixture; and
heating the mixture to polymerize active silicic acid,
wherein a method for producing the purified alkali silicate aqueous solution comprises the steps of:
adjusting a silica concentration of an alkali silicate aqueous solution to 0.5 to 10.0% by mass; and
filtering the alkali silicate aqueous solution through a filter having a removal rate of particles with a primary particle size of 1.0 μm of 50% or more, and
wherein:
the measurement method A is a method in which 30 mL of an alkali silicate aqueous solution at 25° C. adjusted to have a silica concentration of 4% by mass is passed through a membrane type filter (filtration area: 4.90 cm 2 ) having an absolute pore size of 0.4 μm, then the membrane type filter is observed by a scanning electron microscope at a magnification of 5,000 times, presence of one or more of plate-like fine particles in one visual field of a 15-by-20 μm rectangle is regarded as one count, presence or absence of the count in each of 100 visual fields that are not overlapped with each other is determined, and the total number of the obtained counts is regarded as an existing amount (%) of the plate-like fine particles, and
the filtration rate in the filtering step is 13 to 400 liter/min per square meter of filtration area of the filter.

4. The method for producing a silica sol according to claim 3 , wherein the alkali component in the alkaline aqueous solution is at least one selected from the group consisting of an alkali metal ion, an ammonium ion, an amine compound, and a quaternary ammonium ion.

5. The method for producing a silica sol according to claim 1 , wherein the filter is at least one selected from the group consisting of a pleats type filter, a depth type filter, and a diatomaceous earth-containing type filter.

6. The method for producing a silica sol according to claim 1 , wherein the removal rate is 60% or more.

7. The method for producing a silica sol according to claim 1 , wherein the removal rate is 70% or more.

8. The method for producing a silica sol according to claim 1 , wherein the removal rate is 80% or more.

9. The method for producing a silica sol according to claim 1 , wherein the removal rate is 90% or more.

10. The method for producing a silica sol according to claim 1 , wherein the alkali component of the alkali silicate aqueous solution is at least one selected from the group consisting of a sodium ion, a potassium ion, a lithium ion, a rubidium ion, and a cesium ion.

11. The method for producing a silica sol according to claim 3 , wherein the removal rate is 60% or more.

12. The method for producing a silica sol according to claim 3 , wherein the removal rate is 70% or more.

13. The method for producing a silica sol according to claim 3 , wherein the removal rate is 80% or more.

14. The method for producing a silica sol according to claim 3 , wherein the removal rate is 90% or more.

15. The method for producing a silica sol according to claim 3 , wherein the alkali component of the alkali silicate aqueous solution is at least one selected from the group consisting of a sodium ion, a potassium ion, a lithium ion, a rubidium ion, and a cesium ion.

Assignees

• Nissan Chemical Ind Ltd

Inventors

• Ema Kiyomi
• Takakuma Noriyuki
• Nishimura Tohru
• Kawashita Naoki
• Yamaguchi Kouji

Classifications

• B82Y30/00

  Nanotechnology for materials or surface science, e.g. nanocomposites · CPC title

• C09K3/1463

  Aqueous liquid suspensions · CPC title

• C01B33/1485 Primary

  Stabilisation, e.g. prevention of gelling; Purification · CPC title

• C01P2004/64

  Nanometer sized, i.e. from 1-100 nanometer · CPC title

• C01B33/1435

  using ion exchangers · CPC title