Notice of Pre-AIA or AIA Status
The present application, filed on or after March 16, 2013, is being examined under the first inventor to file provisions of the AIA .
Continued Examination Under 37 CFR 1.114
A request for continued examination under 37 CFR 1.114, including the fee set forth in 37 CFR 1.17(e), was filed in this application after final rejection. Since this application is eligible for continued examination under 37 CFR 1.114, and the fee set forth in 37 CFR 1.17(e) has been timely paid, the finality of the previous Office action has been withdrawn pursuant to 37 CFR 1.114. Applicant's submission filed on 08/28/2025 has been entered.
Status of Rejections
The rejection(s) of claim(s) 216-217 is/are obviated by applicant’s cancellation.
All previous rejections are withdrawn in view of applicant’s amendments/arguments.
New grounds of rejection are necessitated by applicant’s amendments.
Claims 131, 136, 143-144, 147-148, 152, 154, 158-160, 168 and 202-215 are pending and under consideration for this Office Action.
Claim Rejections - 35 USC § 103
The text of those sections of Title 35, U.S. Code not included in this action can be found in a prior Office action.
Claims 131, 136, 143-144, 147-148, 152, 154, 158-160, 168, 202-211 and 215 are rejected under 35 U.S.C. 103 as being unpatentable over Harrison (WO 2011133165 A1) in view of Ma et al. (CN 105251436 A, citations based on translation), and further in view of Shi et al. (“Synthesis and properties of Li1.6Mn1.6O4 and its adsorption application”, Hydrometallurgy, 2011) and Yang et al. (CN 107376827 A, citations based on translation); claim 131 evidenced by Chung et al. (U.S. 2011/0174739) and claim 160 evidenced by Mauritz et al. (“State of Understanding of Nafion”, Chem. Rev., 2004).
Regarding claim 131, Harrison teaches an integrated process for producing a lithium salt from a liquid resource (see e.g. Abstract, method for preparing lithium carbonate from lithium chloride containing brines), comprising:
d) providing a crystallizer and treating a lithium eluate in said crystallizer with a precipitant to precipitate said lithium salt and create a residual eluate (see e.g. Fig. 2, reactor/crystallizer 68 in which a lithium chloride solution 30 is treated with sodium carbonate 66 as a precipitant to precipitate lithium carbonate and create a remaining aqueous solution containing sodium chloride, i.e. residual eluate; Paragraph 0042);
e) providing an electrochemical cell in fluid communication with said crystallizer (see e.g. Fig. 2, electrochemical cell 32 in communication with reactor/crystallizer 68 via outlet paths 70 and 76 and recycle line 77; Paragraph 0043, lines 1-4 and 16-17), wherein said electrochemical cell comprises (i) a first electrochemically reducing electrode and (ii) a second electrochemically oxidizing electrode (see e.g. Paragraphs 0024-0025, cathode and anode of electrochemical cell); and
f) subjecting said residual eluate to an electric current in said electrochemical cell, wherein said electrical current causes electrolysis of said residual eluate to produce an acidified solution and a basified solution (see e.g. Fig. 2, sodium chloride stream 60, including recycled stream 77, subject to electrolysis, i.e. application of electrical current, in electrochemical cell 32, producing basified sodium hydroxide stream 62, and chlorine and hydrogen gases 64,65 that maybe be used to form a hydrochloric acid, i.e. acidified solution; Paragraphs 0038, 0040 and 0045);
wherein the liquid resource comprises lithium ions and one or more divalent ions selected from magnesium and calcium (see e.g. Paragraph 0020, lines 1-4, and Paragraph 0005, lines 1-4).
Harrison does not teach a) providing an ion exchange unit, wherein said ion exchange unit comprises a hydrogen-enriched ion exchange material comprising an ion exchange material that has been treated with an acid, wherein the hydrogen-enriched ion exchange material is contained within one or more packed beds; b) contacting said hydrogen-enriched ion exchange material in said ion exchange unit with said liquid resource, wherein hydrogen ions from said hydrogen-enriched ion exchange material are exchanged with lithium ions form said liquid resource to produce a lithium-enriched ion exchange material in said ion exchange unit; and c) treating said lithium-enriched ion exchange material in said ion exchange unit with an acid solution, wherein said lithium ions from said lithium-enriched ion exchange material are exchanged with hydrogen ions from said acid solution to produce the lithium eluate; wherein the pH of said liquid resource is maintained in an acceptable range that is from 1 to 9. Harrison does however teach that the lithium eluate may generally come from methods known in the art for isolation of lithium chloride from brines (see e.g. Paragraph 0020).
Ma teaches a method of extracting lithium from a liquid lithium resource such as a salt lake brine (see e.g. Paragraphs 0002 and 0005, and Paragraph 0037, line 1) comprising providing several packed beds each containing a hydrogen-enriched ion exchange material obtained by acid treating an ion exchange material (see e.g. Fig. 1, adsorption towers A-E filled with particles of lithium ion sieve, i.e. ion exchange, adsorbent 1, e.g. LiMnO2.5, acid washed to create a desorbed hydrogen rich adsorbent material, e.g. HMnO2.5; Paragraphs 0029-0030 and 0036), contacting the hydrogen-enriched ion exchange material with the brine solution having a pH of 7-8.5, causing ion exchange between hydrogen in the material and lithium in the lithium-containing brine to produce a lithium-enriched ion exchange material (see e.g. Paragraphs 0019 and 0038, pretreated brine pumped through adsorption towers to adsorb the lithium therein with the ion sieve adsorbent, which operates by ion exchange of hydrogen in the material with lithium in the solution, as evidenced by Chung, see e.g. Chung Paragraphs 0031 and 0041), and treating the lithium-enriched ion exchange material with an acid solution, causing ion exchange between hydrogen in the acid solution and the lithium adsorbed in the ion exchange material to produce a lithium eluate, which would contain lithium chloride when using an exemplary hydrochloric acid solution (see e.g. Paragraph 0020 and Paragraph 0039, lines 4-7, acidic solution pumped through tower to desorb lithium ions in the adsorbent and dissolve into the acidic solution, which occurs by ion exchange between hydrogen in the acidic solution and the lithium in the ion-sieve adsorbent, as evidenced by Chung, see e.g. Chung Paragraphs 0031 and 0057), wherein the eluate may then be sent to subsequent processing to prepare a salt such as lithium carbonate (see e.g. Paragraph 0040, lines 1-2), the method enabling a large amount of lithium adsorption and transfer over a long lifetime with economic and environmental benefits (see e.g. Paragraphs 0010, 0023 and 0065).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the process of Harrison to comprise producing the lithium chloride eluate from brine using the ion exchange unit and process of Ma as an exemplary method known in the art for isolation of lithium chloride from brine that also enables adsorption and transfer of a large amount of lithium over a long lifetime with economic and environmental benefits.
Harrison as modified by Ma above, does not explicitly teach the ion exchange material performing greater than about 1000 cycles, wherein each cycle comprises b), i.e. adsorption of Li ions, and c), i.e. desorption of Li ions. Ma does however teach being capable of having a longer life of adsorption-desorption cycles, reducing cost and improving efficiency (see e.g. Ma Paragraphs 0010 and 0065), and particularly performing better, with a 60% reduction in dissolution loss, than an alternative single column system that accumulated a lot of dissolution loss over hundreds of cycles of use (see e.g. Ma Paragraphs 0046, lines 1-6, and Paragraph 0057), implying the capability of the ion exchange system of Ma to be used stably on a scale of at least hundreds of cycles. Ma further teaches the ion exchange material comprising an LMO-type ion sieve adsorbent such as Li1.6Mn1.6O4 (see e.g. Ma Paragraphs 0008, 0036 and 0045).
Shi teaches an Li1.6Mn1.6O4 ion sieve for recovery of lithium from brine (see e.g. Abstract) wherein the absorption process becomes less cost-effective and is defined to be unstable when total loss of dissolved Mn is higher than 70% to be cost effective before replacement, meaning that the ion sieve with an average loss ratio of 0.5% per cycle may operate for greater than 140 cycles (see e.g. Page 102, Col. 2, lines 1-6, and Page 103, Col. 2, under “3.5.3”, lines 15-22).
Yang teaches a method for preparing a manganese-based lithium ion sieve (see e.g. Paragraph 0002), wherein particles of the H1.6Mn1.6O4 manganese-based lithium ion sieve, i.e. ion exchange particles, are coated with zirconium dioxide (see e.g. Paragraphs 0007-0009, core-shell structure of zirconium dioxide coating shell over manganese-base lithium ion sieve), thereby reducing the dissolution rate to 0.15% and loss of manganese and improving the structural stability of the lithium ion sieve (see e.g. Paragraphs 0007 and 0010). This 0.15% dissolution rate in combination with the 60% dissolution loss reduction taught by Ma would result in the ion exchange material being operable for greater than 1166 cycles before reaching the 70% total loss defined by Shi.
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the manganese-based ion exchange material of modified Harrison to be coated with zirconium dioxide as taught by Yang to improve the structural stability of the ion exchange material and reduce the base dissolution rate and loss of manganese to as low as 0.15%, in addition to the 60% reduction already taught by Ma, and would have further been obvious to have modified the method of modified Harrison to have said ion exchange material perform greater than 1166 adsorption/desorption cycles, until the total manganese ion loss is higher than 70%, as taught by Shi as a suitable operating parameter for the ion exchange material to be cost-effectively used before replacement. MPEP § 2143(I)(A) states that “combining prior art elements according to known methods to yield predictable results” may be obvious. The claimed elements were known in the prior art and one skilled in the art could have combined the elements as claimed by known methods with no change in their respective functions, and the combination would yield nothing more than predictable results.
Regarding claim 136, Harrison as modified by Ma teaches step b) further comprising treating said hydrogen-enriched ion exchange material with a base (see e.g. Ma Paragraph 0060, lines 1-9, supplemental basic alkali solution added online to the streams entering each tower during adsorption, thereby treating the hydrogen-enriched ion exchange material used for said adsorption).
Regarding claim 143, Harrison as modified by Ma teaches said process further comprising providing a thermal evaporation unit in fluid communication with said ion exchange unit and said crystallizer, wherein said thermal evaporation unit comprises a heating element (see e.g. Ma Paragraph 0040, lines 1-2, lithium eluate from tower sent to further processes steps to produce lithium carbonate; see e.g. Harrison Paragraph 0021, lines 1-6, lithium chloride solution, i.e. eluate, may first be concentrated by evaporation, such as steam evaporation, which inherently requires a heating element).
Regarding claim 144, Harrison as modified by Ma teaches said process further comprising providing a purification unit in fluid communication with said ion exchange unit and said crystallizer; and prior to step d), said lithium eluate being passed into said purification unit to produce a purified eluate that is subject to steps d) to f) (see e.g. Ma Paragraph 0040, lines 1-2, lithium eluate from tower sent to further processes steps to produce lithium carbonate; see e.g. Harrison Paragraph 0020, lithium chloride solution, i.e. eluate, may first undergo purification).
Regarding claims 147-148 and 211, modified Harrison teaches said lithium salt being lithium carbonate (see e.g. Harrison Paragraph 0042, lines 7-8).
Regarding claim 152, Harrison as modified by Ma and Shi teaches said ion exchange material being Li1.6Mn1.6O4 (see e.g. Ma Paragraphs 0008, 0036 and 0045; see e.g. Shi Abstract)
Regarding claim 154, Harrison as modified by Ma and Yang teaches said ion exchange material comprising coated ion exchange particles (see e.g. Ma Paragraph 0036, line 2, lithium ion sieve, i.e. ion exchange, adsorbent particles; see e.g. Yang Paragraphs 0007-0009, core-shell structure of zirconium dioxide coating shell over manganese-base lithium ion sieve).
Regarding claim 158, Harrison as modified by Ma teaches said acid solution comprising hydrochloric acid or sulfuric acid (see e.g. Ma Paragraph 0039, line 5).
Regarding claim 159, modified Harrison teaches said electrochemical cell comprising an ion-conducting membrane that is a cation conducting membrane (see e.g. Harrison Paragraph 0027, lines 1-2, cation-selective membrane).
Regarding claim 160, modified Harrison teaches said cation conducting membrane comprising a sulfonated tetrafluoroethylene-based fluoropolymer-copolymer (see e.g. Harrison Paragraph 0027, lines 3-4, Nafion membrane, which comprises a sulfonated tetrafluoroethylene-based fluoropolymer-copolymer, as evidenced by Mauritz, see e.g. Mauritz Page 4535, Col. 1, lines 1-5).
Regarding claim 168, modified Harrison teaches said precipitant being a carbonate salt (see e.g. Harrison Paragraph 0042, lines 7-9, sodium carbonate).
Regarding claim 202, modified Harrison teaches prior to step d), said lithium eluate being passed into said thermal evaporation unit, and wherein water is removed from said lithium eluate to produce a concentrated lithium eluate, wherein the concentrated lithium eluate is subject to steps d) to f) (see e.g. Harrison Paragraph 0021, lines 1-6, lithium chloride solution, i.e. eluate, may first be concentrated by removing water via evaporation, such as steam evaporation).
Regarding claim 203, modified Harrison further teaches recycling said acidified solution (see e.g. Harrison Paragraphs 0040 and 0045, hydrochloric acid from the electrochemical cell can be used elsewhere in the process). Modified Harrison does not teach said acid solution of step c) comprising said acidified solution as a result of said recycling. Harrison does however teach said acidified solution comprising hydrochloric acid (see e.g. Harrison Paragraphs 0040 and 0045), which is one of the exemplary acid solutions taught by Ma for the elution step in the ion exchange unit (see e.g. Ma Paragraph 0039, line 5).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the acid solution in step c) of modified Harrison to comprise the recycled acidified solution as an alternate or additional suitable acid-containing feed in the process that can benefit from the recycled hydrochloric acid. MPEP § 2143(I)(B) states that “simple substitution of one known element for another to obtain predictable results” may be obvious. Further, MPEP § 2143(I)(A) states that “combining prior art elements according to known methods to yield predictable results” may be obvious. The claimed elements were known in the prior art and one skilled in the art could have combined the elements as claimed by known methods with no change in their respective functions, and the combination would yield nothing more than predictable results.
Regarding claim 204, modified Harrison further teaches recycling said acidified solution from said electrochemical cell (see e.g. Harrison Paragraphs 0040 and 0045, hydrochloric acid from the electrochemical cell can be used elsewhere in the process), but does not teach it being recycled to said ion exchange unit of step c). Harrison does however teach said acidified solution comprising hydrochloric acid (see e.g. Harrison Paragraphs 0040 and 0045), which is one of the exemplary acid solutions taught by Ma for the elution step in the ion exchange unit (see e.g. Ma Paragraph 0039, line 5).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the acid solution in step c) of modified Harrison to comprise the recycled acidified solution as an alternate or additional suitable acid-containing feed in the process that can benefit from the recycled hydrochloric acid solution. MPEP § 2143(I)(B) states that “simple substitution of one known element for another to obtain predictable results” may be obvious. Further, MPEP § 2143(I)(A) states that “combining prior art elements according to known methods to yield predictable results” may be obvious. The claimed elements were known in the prior art and one skilled in the art could have combined the elements as claimed by known methods with no change in their respective functions, and the combination would yield nothing more than predictable results.
Regarding claim 205, modified Harrison further teaches recycling said basified solution from said electrochemical cell (see e.g. Harrison Paragraphs 0032, lines 7-10 and Paragraph 0041, lines 1-3, hydroxide stream from electrochemical cell recycled to carbonation reactor/absorber), but does not teach it being recycled to said ion exchange unit of step b). Ma does however teach the ion exchange unit being treated with a base, such as sodium hydroxide, in step b) (see e.g. Ma Paragraph 0060, lines 1-9, supplemental basic alkali solution such as NaOH added online to the streams entering each tower during adsorption), the basified solution of Harrison similarly comprising sodium hydroxide (see e.g. Harrison Paragraph 0038, lines 2-3).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the recycled basified solution of modified Harrison to be sent to the ion exchange unit in step b) as an alternate or additional suitable base-containing feed in the process that can benefit from the recycled sodium hydroxide solution. MPEP § 2143(I)(B) states that “simple substitution of one known element for another to obtain predictable results” may be obvious. Further, MPEP § 2143(I)(A) states that “combining prior art elements according to known methods to yield predictable results” may be obvious. The claimed elements were known in the prior art and one skilled in the art could have combined the elements as claimed by known methods with no change in their respective functions, and the combination would yield nothing more than predictable results.
Regarding claim 206, modified Harrison teaches the purification unit producing the purified lithium concentrate at least by removing impurities from the lithium eluate through chemical precipitation (see e.g. Harrison Paragraphs 0004-0005 and 0020, lithium chloride solution, i.e. eluate, purified by removal of divalent ions, e.g. by precipitation with lime or soda ash).
Regarding claim 207, modified Harrison teaches removing impurities from the lithium eluate through chemical precipitation comprising using hydroxide-containing or carbonate-containing reagents (see e.g. Harrison Paragraphs 0004-0005, magnesium and calcium removed by treatment of solution with lime (Ca(OH)2) or soda ash (Na2CO3)).
Regarding claim 208, modified Harrison teaches removing impurities from the lithium eluate through chemical precipitation comprising using Ca(OH)2 (see e.g. Harrison Paragraphs 0004-0005, magnesium and calcium removed by treatment of solution with lime (Ca(OH)2)).
Regarding claim 209, the limitation of “removing impurities from the lithium eluate through oxidation comprises oxidation using O2, KMnO4, H2O2, Cl2, NaOCl, or other oxidizing agents” further narrows the unselected optional limitation of impurity removal by oxidation of claim 206, and is therefore not required to be met, as long as the other optional limitation is met.
Regarding claim 210, modified Harrison further teaches recycling the basified solution (see e.g. Harrison Paragraphs 0032, lines 7-10 and Paragraph 0041, lines 1-3, hydroxide stream from electrochemical cell recycled to carbonation reactor/absorber), but does not teach it being used to maintain the pH of the liquid resource in the acceptable range. Ma does however teach the pH of the liquid resource being maintained with a base, such as sodium hydroxide, in step b) (see e.g. Ma Paragraph 0037, lines 1-2, and Paragraph 0059, lines 1-3, pH of lithium-containing salt brine adjusted with base such as NaOH), the basified solution of Harrison similarly comprising sodium hydroxide (see e.g. Harrison Paragraph 0038, lines 2-3).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the recycled basified solution of modified Harrison to be used for adjusting and maintaining the pH of the liquid resource as an alternate or additional suitable base-containing feed in the process that can benefit from the recycled sodium hydroxide solution. MPEP § 2143(I)(B) states that “simple substitution of one known element for another to obtain predictable results” may be obvious. Further, MPEP § 2143(I)(A) states that “combining prior art elements according to known methods to yield predictable results” may be obvious. The claimed elements were known in the prior art and one skilled in the art could have combined the elements as claimed by known methods with no change in their respective functions, and the combination would yield nothing more than predictable results.
Regarding claim 215, Harrison as modified by Ma teaches the pH of said liquid resource being maintained by at least adding a base to the liquid resource (see e.g. Ma Paragraph 0037, lines 1-2, and Paragraph 0059, lines 1-3, pH of lithium-containing salt brine adjusted with base such as NaOH, KOH or Ca(OH)2).
Claim 212 is rejected under 35 U.S.C. 103 as being unpatentable over Harrison, Ma, Shi and Yang, as applied to claim 131 above, and further in view of Chon et al. (US 2013/0129586).
Regarding claim 212, modified Harrison teaches all the elements of the process of claim 131 as stated above. Modified Harrison does not teach said lithium salt being lithium phosphate, instead teaching it being lithium carbonate (see e.g. Harrison Paragraph 0042, lines 7-8).
Chon teaches a method of extracting lithium from a lithium bearing solution such as a brine, comprising adding a phosphorus supplying material as a precipitant to precipitate lithium phosphate from the solution (see e.g. Paragraphs 0013 and 0018), the precipitation as lithium phosphate instead of as lithium carbonate enabling more economical and efficient extraction of the lithium from the lithium bearing solution (see e.g. Paragraphs 0038-0040).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the lithium salt produced by modified Harrison to be lithium phosphate instead of lithium carbonate by providing a phosphorus supplying precipitant as taught by Chon to enable more economical and efficient extraction of lithium from the lithium-containing liquid resource.
Claim 213 is rejected under 35 U.S.C. 103 as being unpatentable over Harrison, Ma, Shi and Yang, as applied to claim 131 above, and further in view of Garret et al. (U.S. Patent No. 4,287,163).
Regarding claim 213, modified Harrison teaches all the elements of the process of claim 131 as stated above. Modified Harrison does not teach said lithium salt being lithium sulfate, instead teaching it being lithium carbonate (see e.g. Harrison Paragraph 0042, lines 7-8).
Garrett teaches a method for recovering lithium from brines (see e.g. Abstract), wherein lithium sulfate is precipitated from the brine using a salting-out agent, i.e. precipitant (see e.g. Fig. 1 and Col. 1, lines 47-51, and Col. 2, lines 56-57),
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the lithium salt produced by modified Harrison to be lithium sulfate as taught by Garrett as an alternate lithium salt that can be produced by precipitation of a lithium-containing solution with a precipitant to recover lithium from brines. MPEP § 2143(I)(B) states that “simple substitution of one known element for another to obtain predictable results” may be obvious.
Claim 214 is rejected under 35 U.S.C. 103 as being unpatentable over Harrison, Ma, Shi and Yang, as applied to claim 131 above, and further in view of Sharma (U.S. 2017/0233261).
Regarding claim 214, modified Harrison teaches all the elements of the process of claim 131 as stated above. Modified Harrison does not teach said lithium salt being lithium hydroxide, instead teaching it being lithium carbonate (see e.g. Harrison Paragraph 0042, lines 7-8).
Sharma teaches a method for treating a lithium chloride obtained from a source such as a brine for production of lithium hydroxide (see e.g. Abstract), wherein lithium hydroxide is produced by precipitation of the lithium chloride with sodium hydroxide as a precipitant (see e.g. Paragraphs 0024-0025 and 0027).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have modified the lithium salt produced by modified Harrison to be lithium hydroxide as taught by Sharma as an alternate lithium salt that can be produced by precipitation of a lithium-containing solution with a precipitant in to recover lithium from brines. MPEP § 2143(I)(B) states that “simple substitution of one known element for another to obtain predictable results” may be obvious.
Response to Arguments
Applicant’s arguments, see pages 7-10, filed 08/28/2025, with respect to the rejection(s) of claim(s) 131 under Harrison in view of Ma and Pan, particularly regarding the applicability of the cycle lifetime of the redox lithium ion carrier of Pan to cycles for a lithium ion exchange material, have been fully considered and are persuasive. Therefore, the rejection has been withdrawn. However, upon further consideration, a new ground(s) of rejection is made in view of Harrison, Ma, Shi and Yang.
Conclusion
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/M.S.J./Examiner, Art Unit 1795
/ALEXANDER W KEELING/Primary Examiner, Art Unit 1795