Method for producing silica sol

Patent metadata

Field	Value
Publication number	US-11518682-B2
Application number	US-202016818114-A
Country	US
Kind code	B2
Filing date	Mar 13, 2020
Priority date	Mar 28, 2019
Publication date	Dec 6, 2022
Grant date	Dec 6, 2022

Abstract

The present invention provides a means capable of suppressing the formation of fine particles in a method for producing a silica sol. The present invention relates to a method for producing a silica sol, including synthesizing a silica sol by, in a reaction liquid containing an alkoxysilane or a condensate thereof, water, and an alkali catalyst, allowing the alkoxysilane or condensate thereof to react with the water in the presence of the alkali catalyst, wherein the alkali catalyst is not additionally supplied after the start of the synthesis until the finish time of the synthesis, and during 90% or more of the time between when 5 minutes have elapsed from the time point when the electrical conductivity of the reaction liquid reaches a local maximum for the first time and the finish time of the synthesis, the proportion of the value of the electrical conductivity of the reaction liquid is more than 90% relative to the value of the electrical conductivity at the time when 5 minutes have elapsed from the time point when the local maximum is reached.

First claim

What is claimed is:

1. A method for producing a silica sol, comprising synthesizing a silica sol by, in a reaction liquid containing an alkoxysilane or a condensate thereof, water, and an alkali catalyst, allowing the alkoxysilane or condensate thereof to react with the water in the presence of the alkali catalyst, wherein
the alkali catalyst is not additionally supplied after a start of the synthesis until a finish time of the synthesis,
during 90% or more of the time between when 5 minutes have elapsed from a time point when an electrical conductivity of the reaction liquid reaches a local maximum for a first time from start of a reaction and the finish time of the synthesis, a proportion of a value of the electrical conductivity of the reaction liquid is more than 90% relative to the value of the electrical conductivity at the time when 5 minutes have elapsed from the time point when the local maximum is reached, and
the method further comprises, during at least part of the time between a start time of the synthesis and the finish time of the synthesis, lowering a temperature of the reaction liquid stepwise or continuously.

2. The method for producing a silica sol according to claim 1 , comprising, during an entire time between when 5 minutes have elapsed from the time point when the electrical conductivity of the reaction liquid reaches a local maximum for the first time and the finish time of the synthesis, lowering the temperature of the reaction liquid continuously.

3. The method for producing a silica sol according to claim 1 , wherein, relative to a total amount of the alkoxysilane or condensate thereof added between when 5 minutes have elapsed from the time point when the electrical conductivity of the reaction liquid reaches a local maximum for the first time and the finish time of the synthesis, the proportion (%) of the amount of the alkoxysilane or condensate thereof added during this period in a state where the proportion of the value of the electrical conductivity of the reaction liquid is more than 90% relative to the value of the electrical conductivity at the time when 5 minutes have elapsed from the time point when the electrical conductivity of the reaction liquid reaches a local maximum for the first time is 90 mass % or more.

4. The method for producing a silica sol according to claim 1 , wherein the alkoxysilane or condensate thereof is added at a constant addition rate between the start time of the synthesis and the finish time of the synthesis.

5. The method for producing a silica sol according to claim 1 , wherein, relative to a total amount of the alkoxysilane or condensate thereof added between the start time of the synthesis and the finish time of the synthesis, the proportion (%) of an amount of the alkoxysilane or condensate thereof added between the start time of the synthesis and the time point when the electrical conductivity of the reaction liquid reaches a local maximum for the first time is less than 20 mass %.

6. The method for producing a silica sol according to claim 1 , comprising preparing the reaction liquid by mixing:
a liquid (B) containing the alkoxysilane or condensate thereof and a second organic solvent; and
a liquid (C1) containing the water and having a pH of 5.0 or more and less than 8.0; with
a liquid (A) containing the alkali catalyst, the water, and a first organic solvent.

7. The method for producing a silica sol according to claim 1 , comprising preparing the reaction liquid by mixing:
a liquid (B) containing the alkoxysilane or condensate thereof and a second organic solvent; and
a liquid (C2) containing the water and not containing the alkali catalyst; with
a liquid (A) containing the alkali catalyst, the water, and a first organic solvent.

8. The method for producing a silica sol according to claim 1 , wherein
silica particles included in the silica sol have a volume average particle size of 10 nm or more and 200 nm or less, and
the proportion of a number of fine particles having a particle size that is 40% or less of the volume average particle size and is 30 nm or less is 10% or less of a total number of the silica particles.

9. The method for producing a silica sol according to claim 1 , wherein the alkali catalyst is ammonia.

Assignees

• Fujimi Inc

Inventors

• Kawasaki Yusuke
• Tsubota Shogo
• Ito Masaaki
• Shinoda Jun
• Ashitaka Keiji

Classifications

• C01B33/145 Primary

  Preparation of hydroorganosols, organosols or dispersions in an organic medium · CPC title

• C01B33/141

  Preparation of hydrosols or aqueous dispersions · CPC title

• C01B33/14

  Colloidal silica, e.g. dispersions, gels, sols · CPC title

• C01P2004/62

  Submicrometer sized, i.e. from 0.1-1 micrometer · CPC title

• C01P2004/64

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