Method for making an aminated siliceous adsorbent

Patent metadata

Field	Value
Publication number	US-11759764-B2
Application number	US-202218088507-A
Country	US
Kind code	B2
Filing date	Dec 23, 2022
Priority date	Feb 5, 2020
Publication date	Sep 19, 2023
Grant date	Sep 19, 2023

Abstract

An aminated siliceous adsorbent, which is the reaction product of dried acidified rice husk ash having disordered mesopores and an amino silane, wherein amine functional groups are present on an external surface and within the mesopores of the dried acidified rice husk ash, and wherein the aminated siliceous adsorbent has a carbon content of 24 to 30 wt. %, based on a total weight of the aminated siliceous adsorbent. A method of making the aminated siliceous adsorbent and a method of capturing CO2 from a gas mixture with the aminated siliceous adsorbent.

First claim

The invention claimed is:

1. A method of making an aminated siliceous adsorbent, the method comprising:
ashing an acid treated rice husk at 600 to 800° C. for 1 to 12 hours to form a rice husk ash;
acid treating the rice husk ash with an inorganic acid to form an acidified rice husk ash;
drying the acidified rice husk ash to form a dried acidified rice husk ash having disordered mesopores; and
aminating the dried acidified rice husk ash with an amino silane, to form the aminated siliceous adsorbent;
wherein the aminated siliceous adsorbent has a carbon content of 24 to 30 wt. %, based on a total weight of the aminated siliceous adsorbent.

2. The method of claim 1 , wherein the dried acidified rice husk ash has an oxygen content of 40 to 46 wt. % and a silicon content of 34 to 40 wt. %, each based on a total weight of the dried acidified rice husk ash.

3. The method of claim 1 , wherein the amino silane contains one amino group per molecule.

4. The method of claim 1 , wherein the amino silane is of formula (I)

wherein
R 1 is an optionally substituted alkoxy, an optionally substituted aryloxy, or a halo;
R 2 is an optionally substituted alkyl, an optionally substituted aryl, or an optionally substituted arylalkyl;
R 3 and R 4 are independently hydrogen, an optionally substituted alkyl, an optionally substituted aryl, or an optionally substituted arylalkyl;
n is an integer of 2 to 16; and
x is 0, 1, or 2.

5. The method of claim 4 , wherein R 1 is methoxy or ethoxy, R 2 is methyl, ethyl, phenyl, or benzyl, R 3 and R 4 are each hydrogen, n is 2 or 3, and x is 0 or 1.

6. The method of claim 1 , wherein the amino silane is 3-aminopropyl triethoxysilane.

7. The method of claim 1 , wherein the aminated siliceous adsorbent has a surface area of 90 to 110 m 2 /g.

8. The method of claim 1 , wherein the aminated siliceous adsorbent has a pore volume of 0.14 to 0.22 cm 3 /g.

9. The method of claim 1 , wherein the aminated siliceous adsorbent has a mean pore diameter of 2.7 to 3.3 nm.

10. The method of claim 1 , wherein the aminated siliceous adsorbent has a CO 2 uptake capacity of 0.4 to 0.46 mmol/g at 298 K and 1 atm, a CO 2 uptake capacity of 0.5 to 0.6 mmol/g at 273 K and 1 atm, and a H 2 uptake capacity of 1 to 1.4 mmol/g at 77 K and 1 atm.

11. The method of claim 1 , wherein the aminated siliceous adsorbent has an ideal selectivity of CO 2 /N 2 of 20 to 24, CO 2 /H 2 of 10 to 14, and an ideal selectivity of CO 2 /CH 4 of 6 to 10.

12. The method of claim 1 , wherein the amino silane is 3-aminopropyl triethoxysilane.

13. The method of claim 1 , wherein the aminated siliceous adsorbent has an oxygen content of 35 to 41 wt. %, a silicon content of 28 to 34 wt. %, and a nitrogen content of 0.5 to 6 wt. %, each based on a total weight of the aminated siliceous adsorbent.

14. The method of claim 1 , wherein drying the acidified rice husk ash includes heating at 75 to 125° C. for 6 to 48 hours.

15. The method of claim 14 , wherein acid treating the rice husk ash includes treating the rice husk ash with hydrochloric acid.

16. The method of claim 15 , wherein aminating the dried acidified rice husk ash includes aminating with the amino silane at 100 to 140° C. for 12 to 48 hours.

Assignees

• Univ King Fahd Pet & Minerals

Inventors

• Basheer Chanbasha
• Aljundi Isam H
• Bakdash Rashed Saed

Classifications

• B01J20/28059 Primary

  being less than 100 m2/g · CPC title

• B01J20/24 Primary

  Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives · CPC title

• B01J20/28061

  being in the range 100-500 m2/g · CPC title

• B01J20/28083

  being in the range 2-50 nm, i.e. mesopores · CPC title

• B01J20/3078

  Thermal treatment, e.g. calcining or pyrolizing · CPC title