Method for synthesizing pre-hydrolyzed alkyl polysilicate

Patent metadata

Field	Value
Publication number	US-10647820-B2
Application number	US-201716065720-A
Country	US
Kind code	B2
Filing date	Oct 30, 2017
Priority date	Nov 18, 2016
Publication date	May 12, 2020
Grant date	May 12, 2020

Abstract

The present invention relates to a two-step synthesis method of a pre-hydrolyzed alkyl polysilicate. In the method, a silica precursor hydrated to 90 to 100% is added to maximize a condensation reaction rate, and a silica precursor hydrated to 25 to 70% is additionally added to terminate a condensation reaction, so that a condensation reaction time may be remarkably shortened relative to a conventional one-step synthesis method and may be shortened even without the use of a condensation catalyst, so that the catalyst purchase cost and the catalyst separation step in the process may not be required, thus having a simple process and reducing the production cost. Also, the amount and time point of the silica precursor additionally added may be controlled, thereby easily controlling the gelation reaction time and the weight average molecular weight, and synthesizing the pre-hydrolyzed alkyl polysilicate excellent in storage stability and processabilty.

First claim

The invention claimed is:

1. A method for synthesizing a pre-hydrolyzed alkyl polysilicate, the method comprising:
1) adding a first silica precursor to perform a first condensation reaction; and
2) adding a second silica precursor to perform a second condensation reaction,
wherein the first silica precursor is hydrated to 90 to 100%, and the second silica precursor is hydrated to 25 to 75%.

2. The method of claim 1 , wherein the first silica precursor is hydrated with 1.8 to 2 equivalents of water.

3. The method of claim 1 , wherein the second silica precursor is hydrated with 0.5 to 1.5 equivalents of water.

4. The method of claim 1 , wherein the first condensation reaction rate is faster than the second condensation reaction rate.

5. The method of claim 1 , wherein the silica precursor is at least one selected from the group consisting of tetra methyl ortho silicate (TMOS), tetra ethyl ortho silicate (TEOS), methyl triethyl ortho silicate, dimethyl diethyl ortho silicate, tetra propyl ortho silicate, tetra isopropyl ortho silicate, tetra butyl ortho silicate, tetra secondarybutyl ortho silicate, tetra tertiarybutyl ortho silicate, tetra hexyl ortho silicate, tetra cyclohexyl ortho silicate and tetra dodecyl ortho silicate.

6. The method of claim 1 , wherein the mass ratio of the added first silica precursor and second silica precursor is 10:1 to 10:3.

7. The method of claim 1 , wherein the second silica precursor is added after 1 to 3 hours from adding the first silica precursor.

8. The method of claim 1 , wherein the total condensation reaction time of the synthesis method is 3 to 10 hours.

9. The method of claim 1 , wherein the first and second condensation reactions are performed without a condensation catalyst.

Assignees

• Lg Chemical Ltd

Inventors

• Lee Kyu Reon
• Oh Kyoung Shil
• Lee Je Kyun

Classifications

• C08G77/04

  Polysiloxanes · CPC title

• C08G77/06

  Preparatory processes · CPC title

• C08G77/02 Primary

  Polysilicates · CPC title