Process for extraction of lithium

Patent metadata

Field	Value
Publication number	US-2023095612-A1
Application number	US-202117801059-A
Country	US
Kind code	A1
Filing date	Feb 19, 2021
Priority date	Feb 20, 2020
Publication date	Mar 30, 2023
Grant date	—

Abstract

Disclosed herein are methods for the recovery of lithium from lithium-bearing materials. More specifically, disclosed herein are methods comprising heating the lithium-bearing material with a solid roasting agent, forming a water suspension to allow to leach at least a portion of lithium into the water, separating a liquid and solid phase, and then exposing the collected solid phase to acid to allow acid leaching of the remaining amount of lithium.

First claim

1 . A method comprising:
a) heating a mixture of a lithium-bearing material provided in a water-insoluble solid form and a solid roasting agent for a first predetermined time to form a solid composition comprising at least one water-soluble phase and at least one water-insoluble phase, wherein the at least one water-soluble phase comprises a first amount of lithium and wherein the at least one water-insoluble phase comprises a second amount of lithium; wherein the heating is at a heating temperature from about 100° C. to less than about 850° C.; b) suspending the solid composition in a first aliquot of water for a second predetermined time, thereby dissolving the at least one water-soluble phase and forming a first suspension comprising a first solid phase and a first liquid phase, wherein the first liquid phase comprises a first portion of the first amount of lithium and wherein the first solid phase comprises the at least one water-insoluble phase comprising the second amount of lithium; c) recovering the first portion of the first amount of lithium from the first liquid phase; and d) optionally:
i) suspending the first solid phase in a second aliquot of water for a third predetermined time to form a further suspension comprising a further solid phase and a further liquid phase;
ii) recovering a further portion of the first amount of lithium from the further liquid phase; and
iii) if the further liquid phase is not substantially free of the further portion of the first amount of lithium in the further liquid phase subjecting the further solid phase to steps i)-ii).

2 . The method of claim 1 , wherein step d) is present.

3 . The method of claim 1 , wherein any of the steps a)-d) is performed under a pressure from about 0.1 MPa to about 20 MPa.

4 . The method of claim 1 , wherein if the further liquid phase is substantially free of the further portion of the first amount of lithium, the method further comprises a step of recycling the further liquid phase to the first aliquot of water.

5 . The method of claim 1 , wherein the roasting agent comprises one or more compounds comprising one or more of alkali, alkaline-earth metals, or ammonium-based compounds, or a combination thereof.

6 . (canceled)

7 . The method of claim 5 , wherein the one or more compounds comprise at least an amount of NaOH.

8 . The method of claim 1 , wherein the lithium-bearing material comprises α-spodumene, lepidolite, hectorite, jadarite, Li-enriched clays, Li-batteries, waste streams of mining and processing of coal and coal by-products and minerals and oil shale, coal underclay, coal overburden, recycled materials, or any combination thereof, and/or wherein the lithium-bearing material further comprises one or more of aluminum, calcium, iron, silicon, sodium, or at least one of rare earth elements.

9 . (canceled)

10 . The method of claim 8 , wherein the first liquid phase further comprises a first amount of one or more of aluminum, calcium, iron, silicon, sodium, or at least one of rare earth elements.

11 . The method of claim 1 , wherein the mixture comprises a ratio of the roasting agent to the lithium-bearing material between about 0.1:1 to about 10:1, wherein the ratio is calculated by the weight of the roasting agent to the weight of the lithium-bearing material.

12 . The method of claim 1 , wherein the heating comprises a heated chamber comprising one or more heating sources effective to provide the heating temperature, and wherein the one or more heating sources comprise a microwave heating source.

13 . (canceled)

14 . The method of claim 12 , wherein the microwave source has a frequency between about 900 MHz to about 6 GHz, and wherein the microwave source has an energy between about 500 W to about 30 kW.

15 . (canceled)

16 . The method of claim 1 , wherein the first predetermined time is from about 0.5 seconds to about 24 hours; and/or wherein the second predetermined time and/or the third predetermined time is from about 1 min to about 72 hours.

17 . (canceled)

18 . The method of claim 1 , wherein the suspending comprises heating of the first suspension and/or the further suspension if present.

19 . The method of claim 18 , wherein the heating of the first suspension or the further suspension, if present, occurs is at a temperature from about 20° C. to about 100° C.

20 . (canceled)

21 . (canceled)

22 . The method of claim 1 , wherein the first portion of the first amount of lithium is from about 5% to less than 100% of all lithium present in the lithium-bearing material.

23 . The method of claim 1 , wherein a sum of the first portion and the further portion of the first amount of lithium is from about 5% to less than 100% of all lithium present in the lithium-bearing material.

24 . (canceled)

25 . The method of claim 1 , further comprising collecting the first solid phase or the further solid phase if present and then
a) adding a first aliquot of an acid to the first solid phase or the further solid phase if present; and b) suspending the first solid phase or the further solid phase if present in the amount of acid for a fourth predetermined time to form an additional suspension comprising an additional solid phase and an additional liquid phase, wherein the additional liquid phase comprises a first portion of the second amount of lithium and wherein the additional solid phase comprises a second portion of the second amount of lithium.

26 . The method of claim 25 further comprising recovering the first portion of the second amount of lithium from the additional liquid phase.

27 . The method of claim 25 , wherein the fourth predetermined time is from about 1 min to about 72 hours.

28 . The method of claim 25 , wherein b) further comprises mixing the additional suspension and/or wherein b) further comprises keeping the additional suspension at a temperature from about 20° C. to about 300° C.

29 . (canceled)

30 . The method of claim 25 , wherein the additional liquid phase comprises a second amount of one or more of aluminum, calcium, iron, silicon, sodium, or at least one of rare earth elements.

31 . The method of claim 30 further comprising recovering the second amount of one or more of aluminum, calcium, iron, silicon, sodium, or at least one of rare earth elements.

32 . The method of claim 25 , comprising collecting the additional solid phase, wherein the step of collecting comprises the sequence of steps:
i) step of adding a second aliquot of an acid to the additional solid phase to form a further additional suspension comprising a further additional solid phase and a further additional liquid phase, wherein the further additional liquid phase optionally comprises a further portion of the second amount of lithium; ii) separating the further additional liquid phase and further additional solid phase;
if the further additional liquid phase comprises the further portion of the second amount of lithium, the further additional solid phase is further subjected to the steps i)-ii); and
if the further additional liquid phase is substantially free of the further portion of the second amount of lithium, recycling the further additional liquid phase to the first or the second aliquot of the acid.

33 . (canceled)

Assignees

• Penn State Res Found
• Univ North Carolina State

Inventors

• Rezaee Mohammad
• Vaziri Hassas Behzad
• Akbari Hamid
• Agrawal Dinesh
• Slawecki Tania

Classifications

• C01D15/08 Primary

  Carbonates; Bicarbonates · CPC title

• C22B21/0015

  by wet processes (C22B21/02, C22B21/04 and C22B21/06 take precedence) · CPC title

• C22B21/0007

  Preliminary treatment of ores or scrap or any other metal source (Bayer processes C01F) · CPC title

• C22B3/08

  Sulfuric acid {, other sulfurated acids or salts thereof} · CPC title

• C22B3/06

  in inorganic acid solutions {, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions} · CPC title