Method of preparing acicular metal-silica composite aerogel particles and acicular metal-silica composite aerogel particles prepared thereby
A method of preparing acicular metal-silica composite aerogel particles by adjusting an aspect ratio of the acicular shape through the adjustment of concentrations of an acidic solution, a solution including a metal salt, and a water glass solution which are reactants, and acicular metal-silica composite aerogel particles prepared thereby. The method prepares acicular metal-silica composite aerogel particles in a short period of time under mild conditions of low temperature and atmospheric pressure, the process is simple, and production costs are reduced in comparison to a conventional preparation method, and thus, productivity and economic efficiency are excellent. When the acicular metal-silica composite aerogel particles are used as an additive of a polymer resin, physical properties, such as viscosity and thixotropy, are improved.
1. A method of preparing acicular metal-silica composite aerogel particles, the method comprising:
(1) adding an acidic solution and a water glass solution to a reactor;
(2) forming an acicular intermediate by a precipitation reaction by adding a solution including a metal salt to the reactor after the addition of the water glass solution;
(3) adding a basic catalyst to the reactor including the acicular intermediate to increase pH and perform a gelation reaction; and
(4) washing, performing solvent substitution, and drying after (3),
wherein:
a concentration of the acidic solution is in a range of 1.0 M to 3.0 M;
a concentration of the metal salt is in a range of 1.0 to 3.0 M; and
a concentration of the water glass solution is in a range of 0.33 M to 1.0 M.
2. The method of claim 1 , wherein:
a ratio of the concentration of the acidic solution to the concentration of the water glass solution is 3:1, and
a ratio of the concentration of the acidic solution to the concentration of the metal salt solution is 1:1.
3. The method of claim 1 , wherein the acicular metal-silica composite aerogel particles have an aspect ratio of 1:20 to 1:25.
4. The method of claim 1 , wherein the acicular metal-silica composite aerogel particles have a thixotropic index of 5 to 7.
5. The method of claim 1 , wherein a silica aerogel is bonded to a surface of the acicular intermediate in the acicular metal-silica composite aerogel particles.
6. The method of claim 1 , wherein the precipitation reaction and the gelation reaction are performed at a temperature of 50° C. to 100° C.
7. The method of claim 1 , wherein the precipitation reaction and the gelation reaction are performed at a pressure of 1 bar to 1.2 bar.
8. The method of claim 1 , wherein the precipitation reaction and the gelation reaction are independently performed for 1 hour to 5 hours.
9. The method of claim 1 , wherein the acidic solution is sulfuric acid (H 2 SO 4 ).
10. The method of claim 1 , wherein the metal salt comprises calcium (Ca).
11. The method of claim 1 , wherein the metal salt comprises at least one ion selected from the group consisting of chloride, bromide, iodide, nitrate, nitrite, sulfate, acetate, sulfite, acetylacetonate, and hydroxide.
12. The method of claim 1 , wherein the basic catalyst comprises at least one hydroxide selected from the group consisting of sodium hydroxide (NaOH), potassium hydroxide (KOH), calcium hydroxide (Ca(OH) 2 ), barium hydroxide (Ba(OH) 2 ), ammonium hydroxide (NH 4 OH), sodium carbonate (Na 2 CO 3 ), and magnesium hydroxide (Mg(OH) 2 ).
13. The method of claim 1 , wherein the basic catalyst is added in an amount such that the pH is increased to be in a range of 7 to 9.
14. The method of claim 1 , wherein the solvent substitution is performed with a polar organic solvent.
15. The method of claim 14 , wherein the polar organic solvent includes ethanol, methanol, or isopropanol.
16. The method of claim 15 , wherein the polar organic solvent includes ethanol.