DETAILED ACTION
Status of Claims
Claims 1-14 and 34-36 are pending.
Claims 15-33 are cancelled.
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 .
Status of Objections and Rejections
The previous grounds of rejection under 35 U.S.C. 112b are withdrawn in view of Applicant’s amendment.
The previous grounds of rejection under 35 U.S.C. 103 for claims 1, 5-8 and 14 stand.
New grounds of rejection are necessitated by amendment.
Claim Objections
Claim 34 is objected to because of the following informalities: there is no spacing between the 4 and electrode (page 4). Appropriate correction is required.
Claim Rejections - 35 USC § 103
In the event the determination of the status of the application as subject to AIA 35 U.S.C. 102 and 103 (or as subject to pre-AIA 35 U.S.C. 102 and 103) is incorrect, any correction of the statutory basis (i.e., changing from AIA to pre-AIA ) for the rejection will not be considered a new ground of rejection if the prior art relied upon, and the rationale supporting the rejection, would be the same under either status.
The following is a quotation of 35 U.S.C. 103 which forms the basis for all obviousness rejections set forth in this Office action:
A patent for a claimed invention may not be obtained, notwithstanding that the claimed invention is not identically disclosed as set forth in section 102, if the differences between the claimed invention and the prior art are such that the claimed invention as a whole would have been obvious before the effective filing date of the claimed invention to a person having ordinary skill in the art to which the claimed invention pertains. Patentability shall not be negated by the manner in which the invention was made.
The factual inquiries for establishing a background for determining obviousness under 35 U.S.C. 103 are summarized as follows:
1. Determining the scope and contents of the prior art.
2. Ascertaining the differences between the prior art and the claims at issue.
3. Resolving the level of ordinary skill in the pertinent art.
4. Considering objective evidence present in the application indicating obviousness or nonobviousness.
This application currently names joint inventors. In considering patentability of the claims the examiner presumes that the subject matter of the various claims was commonly owned as of the effective filing date of the claimed invention(s) absent any evidence to the contrary. Applicant is advised of the obligation under 37 CFR 1.56 to point out the inventor and effective filing dates of each claim that was not commonly owned as of the effective filing date of the later invention in order for the examiner to consider the applicability of 35 U.S.C. 102(b)(2)(C) for any potential 35 U.S.C. 102(a)(2) prior art against the later invention.
Claim(s) 1, 5-8 and 14 is/are rejected under 35 U.S.C. 103 as being unpatentable over Calvo et al. (US 2014/0076734).
Water Science School (2018) is herein cited as evidence.
Regarding claim 1, Calvo discloses an electrochemical method for recovering lithium from an aqueous solution containing sodium (abstract, [0036]) (= a method of extracting lithium from an aqueous solution having lithium and dissolved sodium), the method comprising:
Providing electrodes which are highly selective for lithium (abstract), [0009] (= providing a pair of electrodes in contact within the aqueous solution, the pair of electrodes being configured for lithium selectivity);
Extracting lithium through intercalation into a first electrode in the aqueous solution (abstract, [0007], [0046]) (= extracting lithium from the aqueous solution by electrochemical intercalation into a first electrode of the pair of electrodes); and
Recovering lithium from a diluted aqueous solution (abstract), [0007] (= recovering the lithium extracted into a first electrode into a freshwater solution). Calvo discloses the recovery solution including a diluted aqueous solution containing LiCl in an amount of 10mM [0007], [0009] and [0081] (e.g. diluted lithium chloride or potassium chloride). As evidenced by Water Science School, a solution containing less than 1,000 ppm of dissolved solids (e.g. salts) is considered freshwater therefore Calvo discloses a freshwater solution since the ranges of Calvo overlap the guidelines for a freshwater solution (LiCl 42.394 g/mol).
Regarding claim 5, Calvo discloses the method applied to a diverse aqueous solution containing lithium including sea water and lake water [0070]. Calvo discloses enriching the Li:Na ratio in dilute solution from at least 2 fold to at least 2000-fold [0062], [0069]. Calvo does not explicitly disclose the ratio for each of sea water and lake water, however, given the range of Calvo and the inclusion of either sea water or lake water, the claimed range of recovery is 50:1 or greater in lake water and 1:1 in sea water would have been obvious to one of ordinary skill in the art by performing routine experimentation.
Regarding claim 6, Calvo discloses lake water comprising for example 62.6 g/L sodium [0144]. Although the amount is for a lake water composition, it would have been obvious to apply the same or similar concentration to sea water. Generally, differences in concentration will not support the patentability of subject matter encompassed by the prior art unless there is evidence indicating such concentration is critical. Where the general conditions of a claim are disclosed in the prior art, it is not inventive to discover the optimum or workable ranges by routine experimentation.
Regarding claim 7, Calvo discloses a lake water example comprising Li: 1.3 g/L and Na: 62.6 g/L (= 0.021). The instant claim does not indicate for example the ratio as a molar ratio, concentration ratio, etc. The ratio of Calvo is close enough to the claimed range that one of ordinary skill in the art would expect the same or similar predictable result.
Regarding claim 8, Calvo discloses constant current control [0079].
Regarding claim 14, Calvo discloses wherein a voltage applied in the electrochemical intercalation is within a water stable window of the aqueous solution for lithium extraction and recovery [0078].
Claim(s) 2 is/are rejected under 35 U.S.C. 103 as being unpatentable over Calvo et al. (US 2014/0076734) in view of Zhao et al. (“Li extraction from high Mg/Li ratio brine with LiFePO4/FePO4 as electrode materials”, Hydrometallurgy, 133, 2013).
Regarding claim 2, Calvo discloses LiFePO4 [0015]. Calvo does not disclose wherein the pair of electrodes comprise FePO4 electrodes.
In the same or similar field of Li extraction, Zhao discloses using a LiFePO4/FePO4 as electrode materials (abstract). Zhao discloses excellent reversibility of the cells on repeated cycling due to the similarities between LiFePO4 and FePO4 (pg. 76, lines 1-2). Zhao discloses the electrode materials such that the positive electrode is lithium-saturated at the charged state while the negative electrode is lithium-absent (pg. 76, left column, 2nd paragraph).
Before the effective filing date of the claimed invention, it would have been obvious to one of ordinary skill in the art to produce a method wherein the pair of electrodes comprise FePO4 electrodes because in a similar field of endeavor, Zhao discloses excellent reversibility of the cells on repeated cycling due to the similarities between LiFePO4 and FePO4 (pg. 76, lines 1-2). It would have been obvious to simply substitute one know electrode with another to produce the same or similar predictable result (e.g. extraction of lithium).
Claim(s) 3 is/are rejected under 35 U.S.C. 103 as being unpatentable over Calvo et al. (US 2014/0076734), in view of Zhao et al. (2013) and in further view of Kim et al. (“An electrochemical cell for selective lithium capture from seawater”, Environmental Science & Technology, 2015, 49, 9415-9422).
Regarding claim 3, Calvo in view of Zhao does not disclose wherein at least the first electrode has an outer layer of a hydrophilic material.
In the same or similar field of extracting lithium, Kim discloses a method comprising providing a pair of electrodes including LiFePO4 in an aqueous solution, extracting lithium from the aqueous solution by electrochemical intercalation and recovering the lithium extracted. Kim discloses that the LiFePO4 electrode comprises a polydopamine (pD) coating with hydrophilic functional groups to enhance the wettability in aqueous environments which provided improved electrochemical performance including exhibiting larger capacities, smaller overpotentials and better cycling performance (p. 9418, left column, 2nd paragraph).
Before the effective filing date of the claimed invention, it would have been obvious to one of ordinary skill in the art to produce a method comprising a hydrophilic material as an outer layer to an electrode because Kim discloses in a similar method to Calvo, coating the LiFePO4 with a hydrophilic material such as pD for improving electrochemical performance.
Claim(s) 4 is/are rejected under 35 U.S.C. 103 as being unpatentable over Calvo et al. (US 2014/0076734), in view of Zhao et al. (2013), in view of Kim et al. (“An electrochemical cell for selective lithium capture from seawater”, Environmetal Science & Technology, 2015, 49, 9415-9422) and in further view of Mizukami et al. (US 2008/0248360).
Regarding claim 4, Calvo, Zhao in view of Kim disclose the claimed invention as described above. Kim discloses coating the electrode with a hydrophilic material such as polydopamine. The combination fails to disclose the hydrophilic material comprising TiO2.
Mizukami discloses a substrate within an electrochemical environment comprising a hydrophilic material comprising TiO2 [0027]. Mizukami discloses that the hydrophilic material may also include organic materials [0027].
Before the effective filing date of the claimed invention, it would have been obvious to one of ordinary skill in the art to produce a method comprising TiO2 as the hydrophilic material because Mizukami discloses TiO2 as a hydrophilic surface coating material and as Kim discloses the use of polydopamine as a hydrophilic coating material. It would have been obvious to one of ordinary skill in the art to simply substitute one known hydrophilic material with another to produce the same or similar predictable result.
Claim(s) 9-10 and 36 is/are rejected under 35 U.S.C. 103 as being unpatentable over Calvo et al. (US 2014/0076734) in view of Marothu et al. (“Electromembrane Extraction – A novel extraction technique for pharmaceutical, chemical, clinical and environmental analysis, Journal of Chromatographic Science, 2013).
Regarding claims 9-10 and 36, Calvo discloses constant voltage application or a current pulse. Calvo fails to disclose the claimed pulsed voltage [0148].
In the field of electrochemical extraction, Marothu discloses pulsing a voltage to provide a stable system by decreasing the thickness of the double layer at the interfaces and improve the extractability by eliminating the mass transfer barrier (as applied to claim 9). Marothu discloses applying a potential difference for a short time and long enough for analytes to extract. The pulse is short enough that the thickness of the boundary layer is minimized. Marothu discloses that when the voltage is turned off, the ions accumulated on the interfaces are dispersed again throughout the solution and the double layer disappears (pg. 622, Figure 4) (as applied to claim 10). Marothu additionally discloses the extraction of metals (pg. 626, left column).
Before the effective filing date of the claimed invention it would have been obvious to one of ordinary skilled in the art to produce a method comprising pulsing the voltage because Marothu discloses that a pulsed voltage improves the extractability in an electrochemical system. Marothu discloses a variety of matrices and a variety of extractable analytes (e.g. lithium). Regarding the claimed time period in seconds, Marothu discloses the pulsing with a short time period. Marothu does not explicitly disclose the duration as seconds, however, Marothu discloses that the off time and on time periods are selected to control the accumulation of ions, double layer and boundary layer. Therefore it would have been obvious to adjust the time period of pulsing the voltage to control the extraction of ions in solution.
Claim(s) 34 is/are rejected under 35 U.S.C. 103 as being unpatentable over Calvo et al. (US 2014/0076734) in view of Moreau et al. (“Structure and stability of sodium intercalated phases in olivine FePO4, Chem. Mater., 22, 4126-4128, 2010).
Regarding claim 34, Calvo discloses LiFePO4 as an electrode material. Calvo does not disclose the claimed NaFePO4.
In the same or similar field of lithium and other salts (e.g. sodium), Moreau discloses NaFePO4 as an electrode material that is capable of ion intercalation (title, pg. 4126, left column, first paragraph). Moreau discloses the similarities between LiFePO4 and NaFePO4 as states that the compounds are equivalent olivine structures. Moreau discloses that NaFePO4 shows promise as an electrochemical electrode material given its good cycling properties (pg. 4128, right column, 3rd paragraph).
Before the effective filing date of the claimed invention, it would have been obvious to one of ordinary skill in the art to produce a method comprising NaFePO4 because Moreau discloses in the same or similar field of endeavor the use of NaFePO4 as an electrode material for the intercalation of salts which provides good cycling capabilities. It would have been obvious to simply substitute one known electrode material with another to produce the same or similar predictable result.
Claim(s) 35 is/are rejected under 35 U.S.C. 103 as being unpatentable over Calvo et al. (US 2014/0076734), in view of Moreau et al. (2010), in view of Kim et al. (“An electrochemical cell for selective lithium capture from seawater”, Environmetal Science & Technology, 2015, 49, 9415-9422) and in further view of Mizukami et al. (US 2008/0248360).
Regarding claim 35, Calvo in view of Moreau fails to disclose a layer of TiO2.
In the same or similar field of extracting lithium, Kim discloses a method comprising providing a pair of electrodes including LiFePO4 in an aqueous solution, extracting lithium from the aqueous solution by electrochemical intercalation and recovering the lithium extracted. Kim discloses that the LiFePO4 electrode comprises a polydopamine (pD) coating with hydrophilic functional groups to enhance the wettability in aqueous environments which provided improved electrochemical performance including exhibiting larger capacities, smaller overpotentials and better cycling performance (p. 9418, left column, 2nd paragraph).
Kim discloses coating the electrode with a hydrophilic material such as polydopamine. The combination fails to disclose the hydrophilic material comprising TiO2.
Mizukami discloses a substrate within an electrochemical environment comprising a hydrophilic material comprising TiO2 [0027]. Mizukami discloses that the hydrophilic material may also include organic materials [0027].
Before the effective filing date of the claimed invention, it would have been obvious to one of ordinary skill in the art to produce a method comprising TiO2 as the hydrophilic material because Mizukami discloses TiO2 as a hydrophilic surface coating material and as Kim discloses the use of polydopamine as a hydrophilic coating material. It would have been obvious to one of ordinary skill in the art to simply substitute one known hydrophilic material with another to produce the same or similar predictable result.
Allowable Subject Matter
Claims 11-13 are objected to as being dependent upon a rejected base claim, but would be allowable if rewritten in independent form including all of the limitations of the base claim and any intervening claims.
The following is a statement of reasons for the indication of allowable subject matter: The prior art alone or in combination does not disclose or render obvious the combination of claim limitations of claims 1, 9 and 11. The closest prior art includes the teachings of Marothu et al. which discloses pulse application of voltage to extract components in an electrochemical system as described above. Calvo and Marothu fail to disclose a reverse pulse as claimed.
Response to Arguments
Applicant's arguments filed 30 June 2025 have been fully considered.
On pages 5-6 the argument is directed towards the claimed ‘freshwater’ and states that Calvo does not disclose the claimed freshwater. The Examiner respectfully disagrees. Calvo discloses the recovery solution including a diluted aqueous solution containing LiCl in an amount of 10mM [0007], [0009] and [0081] (e.g. diluted lithium chloride or potassium chloride). As evidenced by Water Science School, a solution containing less than 1,000 ppm of dissolved solids (e.g. salts) is considered freshwater therefore Calvo discloses a freshwater solution since the ranges of Calvo overlap the guidelines for a freshwater solution (LiCl 42.394 g/mol).
On page 6-7 the argument is directed towards claim 2 and both electrodes comprising iron phosphate. The Examiner is in agreement and new grounds of rejection are presented above. Similarly, the argument on page 8 refers to the electrode composition. New grounds of rejection are presented above to address the claim limitations.
On page 7 the argument is directed towards the claim pulsing. New grounds of rejection are presented above as necessitated by amendment.
Conclusion
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/Stefanie S Wittenberg/Primary Examiner, Art Unit 1795