Method for preparing silica nanoparticles

Patent metadata

Field	Value
Publication number	US-2018127601-A1
Application number	US-201615347405-A
Country	US
Kind code	A1
Filing date	Nov 9, 2016
Priority date	Nov 9, 2016
Publication date	May 10, 2018
Grant date	—

Abstract

A method for preparing silica nanoparticles includes the steps of: slowly titrating a sodium silicate solution with an acid solution to obtain a silicic acid-containing solution; continuously stirring the silicic acid-containing solution; slowly titrating the silicic acid-containing solution with the acid solution to obtain a silicic acid-enriched solution; continuously stirring the silicic acid-enriched solution; collecting the silicic acid-enriched solution as a silica nanoparticle precursor solution when a pH value of the silicic acid-enriched solution reaches a target pH value; and subjecting the silica nanoparticle precursor solution to a flame spray pyrolysis or a drying-grinding-calcining treatment.

First claim

1 . A method for preparing a silica nanoparticle precursor solution, comprising the steps of:
a) pre-treating a siliceous rock to form a sodium silicate solution; b) slowly titrating the sodium silicate solution with an acid solution under stirring until a pH value of the sodium silicate solution is reduced by a predetermined value so as to obtain a silicic acid-containing solution; c) continuously stirring the silicic acid-containing solution until a pH value of the silicic acid-containing solution becomes constant; d) slowly titrating the silicic acid-containing solution with the acid solution under stirring until the pH value of the silicic acid-containing solution is reduced by the predetermined value so as to obtain a silicic acid-enriched solution having a silicic acid amount which is greater than that of the silicic acid-containing solution by a predetermined increment; and e) continuously stirring the silicic acid-enriched solution until the pH value of the silicic acid-enriched becomes constant if a pH value of the silicic acid-enriched solution does not reach a target pH value.

2 . The method according to claim 1 , further comprising a step of collecting the silicic acid-enriched solution as the silica nanoparticle precursor solution when the pH value of the silicic acid-enriched solution reaches the target pH value.

3 . The method according to claim 1 , further comprising, after step e), N additional steps of slowly titrating the silicic acid-enriched solution with the acid solution to permit the silicic acid-enriched solution to reach the target pH value, wherein N is an integer larger than 1.

4 . The method according to claim 3 , wherein each of the N additional steps of slowly titrating the silicic acid-enriched solution is performed until the pH value of the silicic acid-enriched solution is reduced by the predetermined value.

5 . The method according to claim 3 , further comprising, between two successive steps of the N additional steps of slowly titrating the silicic acid-enriched solution, a step of continuously stirring the silicic acid-enriched solution until the pH value of the silicic acid-enriched solution becomes constant.

6 . The method according to claim 1 , wherein the predetermined value is about 1.

7 . The method according to claim 1 , wherein the target pH value is about 7.

8 . The method according to claim 1 , wherein the continuously stirring the silicic acid-enriched solution is performed for a period ranging from about 25 minutes to about 35 minutes.

9 . The method according to claim 1 , wherein the acid solution is a hydrochloric acid solution having a concentration ranging from about 3 wt % to about 7 wt %.

10 . The method according to claim 9 , wherein the titrating is performed at a temperature ranging from about 55° C. to about 75° C.

11 . The method according to claim 1 , wherein step a) includes the sub-steps of:
a-1) crushing and grinding the siliceous rock to form siliceous rock powders; and a-2) leaching the siliceous rock powders with an acidic leaching solution at a temperature below a boiling point of the acidic leaching solution to remove non-siliceous components so as to form acid-leached siliceous rock powders.

12 . The method according to claim 11 , wherein the acidic leaching solution is a sulfuric acid solution having a concentration ranging from about 3 M to about 6 M, and sub-step a-2) is performed at a temperature ranging from about 80° C. to about 95° C. for a period ranging from about 22 hours to about 26 hours.

13 . The method according to claim 11 , wherein step a) further includes, after sub-step a-2), a sub-step of a-3) leaching the acid-leached siliceous rock powders with a basic leaching solution at a temperature below a boiling point of the basic leaching solution to obtain the sodium silicate solution.

14 . The method according to claim 13 , wherein the basic leaching solution is a sodium hydroxide solution having a concentration ranging from about 25 wt % to about 35 wt %, and sub-step a-3) is performed at a temperature ranging from about 80° C. to about 95° C. for a period ranging from about 28 hours to about 32 hours.

15 . The method according to claim 1 , wherein the siliceous rock is siliceous mudstone.

16 . A method for preparing silica nanoparticles, comprising the steps of:
a) pre-treating a siliceous rock to form a sodium silicate solution; b) slowly titrating the sodium silicate solution with an acid solution under stirring until a pH value of the sodium silicate solution is reduced by a predetermined value so as to obtain a silicic acid-containing solution; c) continuously stirring the silicic acid-containing solution until a pH value of the silicic acid-containing solution becomes constant; d) slowly titrating the silicic acid-containing solution with the acid solution under stirring until the pH value of the silicic acid-containing solution is reduced by the predetermined value so as to obtain a silicic acid-enriched solution having a silicic acid amount which is greater than that of the silicic acid-containing solution by a predetermined increment; e) continuously stirring the silicic acid-enriched solution until the pH value of the silicic acid-enriched becomes constant if a pH value of the silicic acid-enriched solution does not reach a target pH value; f) collecting the silicic acid-enriched solution as the silica nanoparticle precursor solution when the pH value of the silicic acid-enriched solution reaches the target pH value; and g) subjecting the silica nanoparticle precursor solution to a flame spray pyrolysis or a drying-grinding-calcining treatment to form the silica nanoparticles.

17 . The method according to claim 16 , further comprising, between step f) and g), a step of continuously stirring the silica nanoparticle precursor solution for a period ranging from about 3 hours to about 13 hours.

18 . The method according to claim 16 , wherein the drying-grinding-calcining treatment includes the sub-steps of:
i) drying the silica nanoparticle precursor solution to form a dried silica nanoparticle precursor; ii) grinding the dried silica nanoparticle precursor to form silica nanoparticle precursor powders; and iii) calcining the silica nanoparticle precursor powders at a temperature ranging from about 900° C. to about 1000° C. to obtain the silica nanoparticles.

19 . A paint composition, comprising:
the silica nanoparticles prepared by the method according to claim 16 in an amount ranging from about 0.5 part by weight to about 1 part by weight; a crosslinking agent selected from the group consisting of polyisocyanate, melamine, aziridine, carbodiimide, and combinations thereof in an amount ranging from about 4 parts by weight to about 5 parts by weight; and a balance of a water-based paint based on 100 parts by weight of the paint composition.

Assignees

• Univ Nat Cheng Kung

Inventors

• Chen Yen-Hua
• Lai Pin-Jung
• Liang Chi-Hui

Classifications

• C01B33/32

  Alkali metal silicates ({C01B33/24} , C01B33/26 take precedence) · CPC title

• C09D7/1216 Primary

  Chemistry & Metallurgy · mapped topic

• C01P2004/64

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

• C09D7/1266

  Chemistry & Metallurgy · mapped topic

• B01J2/04

  in a gaseous medium {(if combined with suspending the material in a gas, e.g. fluidised beds B01J2/16)} · CPC title