IP Library › Granted Patent US 12,350,644
Granted Patent B2
US 12,350,644 · App. 17/865,721 · Granted Jul 8, 2025

Product for PFAS adsorption

Inventors: Bo Wang (Union City, CA); Thomas Scott Cortner (Spring, TX); Dennis Parker (Victor, ID)
Assignee: Active Minerals International, LLC
B01J20/22B01J20/12B01J20/28004B01J20/28016B01J20/28059B01J20/28061B01J20/3204B01J20/3219B01J20/3259B01J20/3295C02F1/288C02F1/281C02F1/285C02F2101/36
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Quick Facts
Patent No.
US 12,350,644
App. No.
17/865,721
Granted
Jul 8, 2025
Kind
B2
Abstract

A product for adsorbing one or more PFAS from a liquid is disclosed. The product may comprise attapulgite that has been surface functionalized with (a) a quaternary amine surface coating solution that comprises a mono-quaternary amine compound or a di-quaternary amine compound and (b) a mercapto surface coating solution that comprises a surface coating agent that includes one or more mercapto groups that chemically bond to the attapulgite surface. When the quaternary amine surface coating solution includes the mono-quaternary amine compound, the product is free of di-quaternary amines. When the quaternary amine surface coating solution includes the di-quaternary amine compound, the product is free of mono-quaternary amines. Also disclosed is a method of producing the product and a method of adsorbing a PFAS in a liquid using the product.

Claims (68)

1. A product for adsorbing at least one PFAS in a liquid, the product comprising attapulgite that has been surface functionalized with: (a) a quaternary amine surface coating solution that includes a mono-quaternary amine compound or a di-quaternary amine compound, the mono-quaternary amine compound comprising one or more mono-quaternary amines that attach to the attapulgite surface, the di-quaternary amine compound comprising one or more di-quaternary amines that attach to the attapulgite surface, and (b) a surface coating agent that includes one or more mercapto groups that chemically bond to the attapulgite surface,

wherein when the quaternary amine surface coating solution includes one or more mono-quaternary amine compounds, the product or the attapulgite is free of di-quaternary amines,

wherein when the quaternary amine surface coating solution includes one or more di-quaternary amine compounds, the product or the attapulgite is free of mono-quaternary amines,

wherein the product or the attapulgite has a surface area in the range of 45-160 m 2 /g as measured using the BET method,

wherein the product or the attapulgite has a particle size distribution having a d 50 of 6-30 microns, and

wherein the product comprises:

85-94 wt. % of the attapulgite;

2.5-15 wt. % of the (i) mono-quaternary amine(s) or (ii) di-quaternary amine(s); and

1-8 wt. % of the surface coating agent.

2. The product of claim 1 , wherein the surface coating agent is mercapto silane.

3. The product of claim 1 , wherein the product is in powder form and/or free of extrusion.

4. The product of claim 1 , wherein the product has a PFAS removal efficiency for the at least one PFAS of 70-100%, in 12-25 hours in the liquid at a loading of 0.5-2 g of the product per liter of the liquid.

5. The product of claim 1 , wherein the product is free of oleyl amine and octyl amine.

6. The product of claim 1 , wherein the product or the attapulgite is free of residual acid.

7. The product of claim 1 , wherein:

the surface area is in a range of 50-100 m 2 /g; and

the d 50 is in a range of 10-25 microns.

8. The product of claim 1 , wherein the d 50 is in a range of 12-23 microns.

9. The product of claim 1 , wherein the product has a PFAS removal efficiency for the at least one PFAS of 90-100%, in 12-25 hours in the liquid at a loading of 0.5-2 g of the product per liter of the liquid.

10. A method of producing a product for adsorbing at least one PFAS from a liquid, the method comprising:

selecting an attapulgite as feed material, wherein prior to surface treatment, the attapulgite selected as the feed material contains 7-16 wt. % moisture when measured at a temperature of 104° C.;

surface treating the attapulgite with a quaternary amine surface coating solution, the quaternary amine surface coating solution including (i) a mono-quaternary amine compound, the mono-quaternary amine compound comprising one or more mono-quaternary amines that attach to the surface of the attapulgite, or (ii) a di-quaternary amine compound, the di-quaternary amine compound comprising one or more di-quaternary amines that attach to the surface of the attapulgite; and

surface treating the attapulgite with a mercapto surface coating solution, the mercapto surface coating solution including a surface coating agent that includes one or more mercapto groups that chemically bond to the surface of the attapulgite,

wherein the product produced or surface treated attapulgite has a surface area in the range of 45-160 m 2 /g as measured using the BET method,

wherein when the quaternary amine surface coating solution includes the mono-quaternary amine compound, the product or surface treated attapulgite is free of di-quaternary amines,

wherein when the quaternary amine surface coating solution includes the di-quaternary amine compound, the product or surface treated attapulgite is free of mono-quaternary amines.

11. The method of claim 10 ,

wherein the weight percentage of components of the product includes:

85-94 wt. % attapulgite;

2.5-15 wt. % of (i) one or more mono-quaternary amines or (ii) one or more di-quaternary amines; and

1-8 wt. % surface coating agent that includes the one or more mercapto groups,

wherein the product is free of oleyl amine and octyl amine.

12. The method of claim 10 ,

Wherein the quaternary amine surface coating solution further includes water,

wherein the mercapto surface coating solution further includes a solvent,

wherein the surface coating agent comprises mercapto silane.

13. The method of claim 10 , wherein the surface treating of the attapulgite with a mercapto surface coating solution is subsequent to the surface treating of the attapulgite with a quaternary amine surface coating solution.

14. The method of claim 13 , wherein the quaternary amine surface coating solution further includes water.

15. The method of claim 10 , wherein the product or surface treated attapulgite has a particle size distribution having a d 50 of 6-30 microns.

16. The method of claim 9 , wherein the product has a PFAS removal efficiency for the at least one PFAS of 70-100%, in 12-25 hours in the liquid at a loading of 0.5-2 g of the product per liter of the liquid.

17. The method of claim 10 , wherein:

the attapulgite selected as the feed material contains 9-14 wt. % moisture; and

the product has a particle size distribution having a d 50 of 10-25 microns.

18. The method of claim 10 , wherein:

the product has a particle size distribution having a d 50 of 12-23 microns; and/or

the product has a PFAS removal efficiency for the at least one PFAS of 95-100%, in 12-25 hours in the liquid at a loading of 0.5-2 g of the product per liter of the liquid.

19. A method for adsorbing at least one PFAS in a liquid, the method comprising:

contacting the liquid with a product comprising attapulgite that has been surface functionalized with (a) a quaternary amine surface coating solution that includes a mono-quaternary amine compound or a di-quaternary amine compound, the mono-quaternary amine compound comprising one or more mono-quaternary amines that attach to the attapulgite surface, the di-quaternary amine compound comprising one or more di-quaternary amines that attach to the attapulgite surface, and (b) a surface coating agent that includes one or more mercapto groups that chemically bond to the attapulgite surface; and

separating the product from the liquid to recover a resultant liquid that has a lower amount of PFAS than the liquid had prior to the mixing,

wherein the weight percentage of the components of the product includes: 85-94 wt. % attapulgite, 2.5-15 wt. % of (i) one or more mono-quaternary amines or (ii) one or more di-quaternary amines, and 1-8 wt. % surface coating agent that includes the one or more mercapto groups,

wherein when the quaternary amine surface coating solution includes one or more mono-quaternary amine compounds, the product or the attapulgite is free of di-quaternary amine compounds,

wherein when the quaternary amine surface coating solution includes one or more di-quaternary amine compounds, the product or the attapulgite is free of mono-quaternary amine compounds,

wherein the product or the attapulgite has a surface area in the range of 45-160 m 2 /g as measured using the BET method,

wherein the removal efficiency of the product for a PFAS is 10-100%, at a loading of 0.5-2 g of the product per liter of the liquid.

20. The method of claim 19 , wherein the liquid includes water, edible oil, wastewater, process water, or combinations thereof.

21. The method of claim 19 , wherein the surface coating agent comprises mercapto silane.

22. The method of claim 19 , wherein when the contacting is for 12-25 hours, the removal efficiency of the product for the PFAS is 70-100%, at the loading of 0.5-2 g of the product per liter of the liquid.

23. The method of claim 19 , wherein when the contacting is for 12-25 hours, the removal efficiency of the product for the PFAS is 80-100%, at the loading of 0.5-2 g of the product per liter of the liquid.

24. The method of claim 19 , wherein when the contacting is for 12-25 hours, the removal efficiency of the product for the PFAS is 95-100% at the loading of 0.5-2 g of the product per liter of the liquid.

25. A product for adsorbing at least one PFAS in a liquid, the product comprising attapulgite that has been surface functionalized with: (a) a quaternary amine surface coating solution that includes a mono-quaternary amine compound or a di-quaternary amine compound, the mono-quaternary amine compound comprising one or more mono-quaternary amines that attach to the attapulgite surface, the di-quaternary amine compound comprising one or more di-quaternary amines that attach to the attapulgite surface, and (b) a surface coating agent that includes one or more mercapto groups that chemically bond to the attapulgite surface,

wherein when the quaternary amine surface coating solution includes one or more mono-quaternary amine compounds, the product is free of di-quaternary amines,

wherein when the quaternary amine surface coating solution includes one or more di-quaternary amine compounds, the product is free of mono-quaternary amines,

wherein the product or the attapulgite has a surface area in the range of 45-160 m 2 /g as measured using the BET method,

wherein the product or the attapulgite has a particle size distribution having a d 50 of 6-30 microns, and

wherein the product or the attapulgite has a porosity of 40-90% and a pore volume of 0.7-1.5 mL/g.

26. The product of claim 25 , wherein the surface coating agent is mercapto silane.

27. The product of claim 25 , wherein the product is free of oleyl amine and octyl amine.

28. The product of claim 25 , wherein the product or the attapulgite is free of residual acid.

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 18, 2022
From: WANG, BO; CORTNER, THOMAS SCOTT; PARKER, DENNIS
To: ACTIVE MINERALS INTERNATIONAL, LLC
Reel/Frame 060534/0487 →
Continuity (1)
Related Publication 20240017240A1 · Jan 18, 2024
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