Lithium recovery using aqueous sources

Patent metadata

Field	Value
Publication number	US-12280322-B2
Application number	US-202418430935-A
Country	US
Kind code	B2
Filing date	Feb 2, 2024
Priority date	May 4, 2022
Publication date	Apr 22, 2025
Grant date	Apr 22, 2025

Abstract

Described herein are methods of recovering lithium from dilute lithium sources. The methods include extracting lithium from an extraction feed using direct lithium extraction in an extraction stage to yield a lithium intermediate, performing one or more concentration operations, each concentration operation concentrating an input stream to yield an output feed, wherein the input stream is obtained from the lithium intermediate and/or the extraction feed is obtained from the output feed. At least one of the concentration operations includes a membrane separation operation having a plurality of reactors in series each having a semi-permeable membrane, such as a counter-flow reverse osmosis operation. Methods may also include generating a low TDS stream as a permeate from any of the one or more concentration operations, wherein the low TDS stream is recycled or used as fresh water.

First claim

We claim:

1. A method of recovering lithium from a lithium source, comprising:
extracting lithium from an extraction feed using direct lithium extraction in an extraction stage to yield a lithium intermediate;
performing one or more concentration operations, each concentration operation concentrating an input stream to yield an output feed, wherein the input stream is obtained from the lithium intermediate and/or the extraction feed is obtained from the output feed;
generating a low TDS stream as a permeate from any of the one or more concentration operations, wherein the low TDS stream is recycled or used as fresh water,
wherein the one or more concentration operations include a reverse osmosis operation upstream of a counter-flow reverse osmosis operation, wherein the reverse osmosis separates the input stream into a preconcentrated stream and a permeate stream using a semi-permeable membrane, wherein the permeate stream is the low TDS stream,
wherein the one or more concentration operations include a counter-flow reverse osmosis operation, wherein the counter-flow reverse osmosis includes flowing the preconcentrated stream into a plurality of reactors in series, each containing a semi-permeable membrane separating the reactor into a first volume and a second volume, wherein the preconcentrated stream flows as a first stream sequentially into the first volume of each reactor and a second stream flows sequentially into the second volume of each reactor counter-current to the first stream, wherein the first stream exiting the plurality of reactors yields a concentrated stream and the second stream exiting the plurality of reactors yields a dilute brine stream,
wherein the dilute brine stream is recycled into the reverse osmosis operation.

2. The method of claim 1 , wherein the input stream of at least one of the concentration operation is a stream derived from the lithium intermediate and the output feed of said concentration operation is a lithium concentrate.

3. The method of claim 2 , including treating a stream derived from the lithium intermediate in an impurity stage to yield a purified stream and wherein the input stream of at least one of the concentration operations is a stream derived from the purified stream, wherein the impurity stage includes one or more of impurity precipitation, solids removal and divalent impurity selective removal.

4. The method of claim 3 , wherein the impurity stage includes routing the stream derived from the lithium intermediate in an impurity precipitation operation via coagulation-flocculation to yield a precipitate stream, routing the precipitate stream or a derivative thereof to solids removal to yield a filtered precipitate stream and a precipitate and routing the filtered precipitate stream or a derivative thereof to divalent impurity selective removal to yield the purified stream.

5. The method of claim 1 , wherein the at least one concentration operation includes pressurizing the input stream before the counter-flow reverse osmosis operation.

6. The method of claim 5 , wherein the at least one concentration operation includes pressurizing the input stream before the reverse osmosis operation and depressurizing the second stream before flowing it into the second volume of the plurality of reactors.

7. The method of claim 1 , wherein the input stream of at least one of the concentration operation is an aqueous lithium source and the output feed of said concentration operation is the extraction feed.

8. A method of recovering lithium from a lithium source, comprising:
extracting lithium from an extraction feed using direct lithium extraction in an extraction stage to yield a lithium intermediate;
performing one or more concentration operations, each concentration operation concentrating an input stream to yield an output feed, wherein the input stream is obtained from the lithium intermediate and/or the extraction feed is obtained from the output feed;
wherein the one or more concentration operations includes
a first membrane separation operation, having a first semi-permeable membrane, yielding from the input stream a preconcentrated stream and a permeate stream,
a second membrane separation operation, wherein the preconcentrated stream flows into a plurality of reactors in series, each containing a semi-permeable membrane separating the reactor into a first volume and a second volume, wherein the preconcentrated stream flows sequentially as a first stream into the first volume of each reactor, wherein the first stream exiting the plurality of reactors yields the output stream, and wherein the second membrane separation operation yields a dilute brine stream that exits the second volume of at least one of the reactors, wherein the dilute brine stream is recycled into the first membrane separation operation,

wherein the at least one concentration operations includes pressurizing the input stream so that the input stream, preconcentrated stream and first stream are pressurized during the first and second membrane separation operations.

9. The method of claim 8 , wherein the at least one concentration operation includes concentrating a stream derived from the lithium intermediate to yield a lithium concentrate.

10. The method of claim 9 , including treating a stream derived from the lithium intermediate in an impurity stage to yield a purified stream and wherein the input stream of at least one of the concentration operations is a stream derived from the purified stream, wherein the impurity stage includes one or more of impurity precipitation, solids removal and divalent impurity selective removal.

11. The method of claim 10 , wherein the impurity stage includes routing the stream derived from the lithium intermediate in an impurity precipitation operation via coagulation-flocculation to yield a precipitate stream, routing the precipitate stream or a derivative thereof to solids removal to yield a filtered precipitate stream and a precipitate and routing the filtered precipitate stream or a derivative thereof to divalent impurity selective removal to yield the purified stream.

12. The method of claim 8 , wherein the second membrane separation operation includes a second stream that flows sequentially into the second volume of the plurality of reactors, counter-current to the second stream, wherein at least a portion of the first stream is recycled into the second stream, wherein the second stream yields the dilute brine stream.

13. The method of claim 12 , including depressurizing the first stream before recycling it into the second stream of the second membrane separation operation.

14. The method of claim 8 , wherein the at least one concentration operation includes a feed preparation operation that concentrates the aqueous lithium source to yield the extraction feed.

Assignees

• Schlumberger Technology Corp

Inventors

• Sams Gary W
• Perroni Dominic Vincent
• Nirgudkar Prasanna
• Binet Florence
• Shampine Rod William

Classifications

• C22B3/24

  by adsorption on solid substances, e.g. by extraction with solid resins · CPC title

• C25C1/02

  of light metals · CPC title

• C22B3/22

  by physical processes, e.g. by filtration, by magnetic means {, or by thermal decomposition} (treatment or purification of solutions by liquid-liquid extraction C22B3/26) · CPC title

• C22B26/12 Primary

  Obtaining lithium · CPC title

• B01D2317/022

  Reject series · CPC title