Method for recycling supercritical waste liquid generated during process of producing silica aerogel blanket

Patent metadata

Field	Value
Publication number	US-12157672-B2
Application number	US-201816652822-A
Country	US
Kind code	B2
Filing date	Nov 13, 2018
Priority date	Nov 13, 2017
Publication date	Dec 3, 2024
Grant date	Dec 3, 2024

Abstract

Provided is a method for recycling supercritical waste liquid and a method for producing a silica aerogel blanket capable of reducing the production costs and preventing the deterioration in thermal insulation performance of a silica aerogel blanket, the method including adding sulfuric acid to supercritical waste liquid to remove ammonium ions in the form of ammonium sulfate salt, the ammonium ions which are present in the supercritical waste liquid, and reusing supercritical waste liquid from which the ammonium ions are removed.

First claim

The invention claimed is:

1. A method for recycling supercritical waste liquid, comprising:
adding sulfuric acid to a supercritical waste liquid generated in a supercritical drying step during a process of producing a silica aerogel blanket, wherein the supercritical waste liquid comprises ammonium ions (NH 4 + );
precipitating and removing an insoluble salt produced by adding the sulfuric acid to yield a recycled supercritical waste liquid; and
using the recycled supercritical waste liquid to replace at least a portion of an organic solvent in one or more steps in the process of producing a silica aerogel blanket.

2. The method of claim 1 , wherein the supercritical waste liquid further comprises water and an organic solvent.

3. The method of claim 2 , wherein the organic solvent is one or more selected from the group consisting of methanol, ethanol, hexane, and pentane.

4. The method of claim 1 , wherein the sulfuric acid is added such that the pH of the supercritical waste liquid is 2.5 to 9.0.

5. The method of claim 1 , wherein the sulfuric acid is added such that the pH of the supercritical waste liquid is 3.0 to 5.0.

6. The method of claim 1 , wherein the insoluble salt is ammonium sulfate.

7. The method of claim 1 , further comprising:
performing centrifugation on the supercritical waste liquid after adding the sulfuric acid; and
collecting a supernatant liquid after the centrifugation as a recycled supercritical waste liquid.

8. The method of claim 7 , wherein the centrifugation is performed at a rate of 2000 to 3500 rpm for 10 to 30 minutes.

9. The method of claim 7 , further comprising, before the centrifugation, stirring the supercritical waste liquid after adding the sulfuric acid, wherein the stirring time is 1 to 6 hours.

10. The method of claim 7 , further comprising, before the centrifugation, holding the supercritical waste liquid after adding the sulfuric acid, wherein the holding time is 5 to 7 hours.

11. The method of claim 7 , wherein the total process time of the method for recycling the supercritical waste liquid is 10 hours or less.

12. The method of claim 1 , wherein the recovery rate of the recycled supercritical waste liquid is 80% or greater based on the weight of the supercritical waste liquid before the addition of the sulfuric acid.

13. The method of claim 1 , wherein the supercritical waste liquid is obtained by simultaneously applying a plurality of pressure pulses to a solvent contained in a silica gel and supercritical fluid in the supercritical drying step, and at least two of the plurality of pressure pulses have at least one feature of being different frequencies and being different amplitudes.

14. The method of claim 1 , wherein the recycled supercritical waste liquid is used in an amount of 85 wt % or greater based on the total weight of the organic solvent used for producing the silica aerogel blanket.

15. A method for producing a silica aerogel blanket, comprising:
preparing a silica sol;
impregnating a fibrous blanket with the silica sol;
gelling the silica sol to form a silica aerogel;
aging the silica aerogel;
surface modifying the silica aerogel; and
drying the silica aerogel to yield the silica aerogel blanket,
wherein a recycled supercritical waste liquid prepared by the method of claim 1 is used in one or more of the steps.

16. The method of claim 15 , wherein the recycled supercritical waste liquid is used in one or more steps selected from the group consisting of the silica sol preparation step, the aging step, and the surface modification step.

17. The method of claim 16 , wherein the recycled supercritical waste liquid is used in preparing the silica sol, and an amount of the recycled supercritical waste liquid used in the silica sol preparation step is 55 wt % to 100 wt % based on the total weight of the organic solvent used in the silica sol preparation step.

18. The method of claim 15 , wherein the recycled supercritical waste liquid is used in an amount of 85 wt % or greater based on the total weight of the organic solvent used for producing the silica aerogel blanket.

19. The method of claim 15 , wherein the thermal conductivity of the silica aerogel blanket is 20 mW/mK or less.

Assignees

• Lg Chemical Ltd

Inventors

• Kim Mi Ri
• Oh Myung Eun
• Oh Kyoung Shil
• Lee Je Kyun

Classifications

• F16L59/07

  the air layer being enclosed by one or more layers of insulation · CPC title

• C02F2101/16

  Nitrogen compounds, e.g. ammonia · CPC title

• C02F1/5236

  using inorganic agents · CPC title

• C02F1/385

  by centrifuging suspensions (centrifuges B04B) · CPC title

• C01C1/242

  Preparation from ammonia and sulfuric acid or sulfur trioxide · CPC title