Polymer-functionalized magnetic particle embodiments for solute separation, and devices and systems for using the same

Patent metadata

Field	Value
Publication number	US-11944982-B2
Application number	US-202016741388-A
Country	US
Kind code	B2
Filing date	Jan 13, 2020
Priority date	Jun 5, 2019
Publication date	Apr 2, 2024
Grant date	Apr 2, 2024

Abstract

Disclosed herein are embodiments of a polymer-functionalized particle for using in isolating and extracting solutes, such as rare earth metals, lithium, and the like. The polymer-functionalized particles exhibit strong resistance to agglomeration and degradation even in high ionic strength and/or temperature environments. A post-particle synthesis method for making the polymer-functionalized particle is disclosed, along with a magnetic separation device and that can be used in system embodiments to facilitate use and regeneration of the polymer-functionalized particles in solute extraction.

First claim

We claim:

1. A polymer-functionalized particle, comprising:
a single magnetic core;
a shell surrounding the single magnetic core, wherein the shell comprises a metal-organic framework material; and
a polymer component that substantially surrounds the shell and the single magnetic core;
wherein the polymer component comprises a functional group selected from a sulfonate group, an ester group, an aldehyde group, an amine group, or an amide group.

2. The polymer-functionalized particle of claim 1 , wherein the single magnetic core comprises iron or an alloy thereof, nickel or an alloy thereof, an iron oxide or an alloy thereof, a nickel oxide or an alloy thereof, or any combination thereof.

3. The polymer-functionalized particle of claim 1 , wherein the single magnetic core comprises iron oxide, cobalt, or nickel.

4. The polymer-functionalized particle of claim 1 , further comprising one or more ligand species associated with the shell.

5. The polymer-functionalized particle of claim 1 , wherein the polymer component is a sulfonate-containing polymer or an amine-containing polymer.

6. The polymer-functionalized particle of claim 1 , wherein the polymer component is poly(4-styrenesulfonic acid) sodium salt or poly(4-styrenesulfonic acid) ammonium salt.

7. The polymer-functionalized particle of claim 1 , wherein the polymer component is a polyethyleneimine polymer having an average molecular weight ranging from 8,000 to 12,000.

8. The polymer-functionalized particle of claim 7 , wherein the polyethyleneimine polymer comprises 25% primary amine groups, 25% secondary amine groups, and 50% tertiary amine groups.

9. The polymer-functionalized particle of claim 1 , wherein the metal-organic framework material comprises chromium, terephthalate, and benzoic acid, or a benzoic acid derivative.

10. The polymer-functionalized particle of claim 1 , wherein the polymer-functionalized particle exhibits colloidal stability in a solution having a pH ranging from 4 to 10, such that a hydrodynamic diameter of the polymer-functionalized particle, and/or an average hydrodynamic diameter of a plurality of polymer-functionalized particles, does not change by 45% or more as compared to a hydrodynamic diameter of an identical particle without the polymer component, and/or an average hydrodynamic diameter of a plurality of identical particles without the polymer component.

11. A system, comprising:
a fluid feed zone comprising a feed source comprising the polymer-functionalized particle of claim 1 , one or more valves, and a residence tube component;
a magnetic separation zone comprising one or more valves and two or more magnetic separation devices, wherein each magnetic separation device comprises (i) a flow tube having a hollow interior; (ii) a collection component positioned within the hollow interior of the flow tube; (iii) a collection matrix material attached to a portion of the collection component; an electromagnet comprising two magnets, wherein the flow tube is positioned between the two magnets;
a solute isolation zone, comprising a mixer, one or more separator components, and a filter;
a magnetic particle regeneration zone, comprising an aqueous salt solution source, one or more mixers, a separator component, and one or more pumps; and
a stripping fluid flow loop, comprising a stripping fluid source, one or more holding tanks, and a pump.

12. The system of claim 11 , wherein (i) the fluid feed zone and the stripping fluid flow loop are fluidly coupled to the magnetic separation zone; (ii) the magnetic separation zone is fluidly coupled to the solute isolation zone; (iii) the solute isolation zone is fluidly coupled to the stripping fluid flow loop and the magnetic particle regeneration zone, which is fluidly coupled to the fluid feed zone.

13. A method for making the polymer-functionalized particle of claim 1 , comprising combining a polymer component solution and a pre-made particle comprising (i) a single magnetic core and (ii) a shell comprising a metal-organic framework material that surrounds the single magnetic core, wherein the polymer component solution comprises a polymer component having a functional group selected from a sulfonate group, and ester group, an aldehyde group, an amine group, or an amide group.

14. A method, comprising:
(i) introducing a feed fluid comprising the polymer-functionalized particle according to claim 1 into a system;
wherein the system comprises
a fluid feed zone comprising a feed source, one or more valves, and a residence tube component;
a magnetic separation zone comprising one or more valves and two or more magnetic separation devices, wherein each magnetic separation device comprises (i) a flowtube having a hollow interior; (ii) a collection component positioned within the hollow interior of the flowtube; (iii) a collection matrix material attached to a portion of the collection component;
and an electromagnet comprising two magnets, wherein the flowtube is positioned between the two magnets;
a solute isolation zone, comprising a mixer, one or more separator components, and a filter;
a magnetic particle regeneration zone, comprising an aqueous salt solution source, one or more mixers, a separator component, and one or more pumps; and
a stripping fluid flow loop, comprising a stripping fluid source, one or more holding tanks, and a pump;
(ii) applying a magnetic field to at least one of the magnetic separation devices of the system as the feed fluid passes through one or more of the magnetic separation devices;
(iii) turning off the magnetic field;
(iv) passing a stripping fluid provided by the stripping fluid source through one or more of the magnetic separation devices;
(v) separating the polymer-functionalized particles from any solutes freed from the polymer-functionalized particles by the stripping fluid;
(vi) isolating the solutes;
(vii) exposing the polymer-functionalized particles to an aqueous salt solution provided by the aqueous salt solution source to provide regenerated polymer-functionalized particles; and
(viii) adding the regenerated polymer-functionalized particles to the feed fluid.

15. The method of claim 14 , further comprising repeating steps (ii) to (viii).

Assignees

• Battelle Memorial Institute

Inventors

• Liu Jian
• Mcgrail B Peter
• Nune Satish
• Thallapally Praveen

Classifications

• B03C1/30 Primary

  Combinations with other devices, not otherwise provided for · CPC title

• B01D15/203 Primary

  Equilibration or regeneration · CPC title

• B03C1/01

  by addition of magnetic adjuvants · CPC title

• B03C1/0335

  using coils · CPC title

• B03C1/288

  disposed at the outer circumference of a recipient · CPC title