DETAILED ACTION
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 .
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.
Election/Restrictions
Claim 2 stands withdrawn from further consideration pursuant to 37 CFR 1.142(b) as being drawn to a nonelected invention, there being no allowable generic or linking claim. Election was made without traverse in the reply filed on 14 May 2026.
Claim Interpretation
As previously noted, claim 11 recites the limitations “the remaining process water is recovered and used to adjust a pH for water treatment.” The specification provides no definition or examples of what is meant by the phrase “to adjust a pH for water treatment.” Therefore, this limitation in the claim will be interpreted broadly and encompass any use of the water in a process in which the pH of an aqueous mixture is adjusted.
Claim Amendments
Applicant’s amendments to the claims filed 2 September 2026 have been entered and considered for this action.
The prior rejections under 35 USC § 112 are withdrawn.
Claim Rejections - 35 USC § 103
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.
Claims 1, 4-5, 8-11 and 14-15 are rejected under 35 U.S.C. 103 as being unpatentable over Xu et al. (CN 112430736 A) in view of Ryu et al. (KR 102033607 B1), Yamaguchi et al. (JP 2014156648 A), Ming et al. (CN 103073031 A) and Yaws' Handbook of Properties for Environmental and Green Engineering (Solubility in Water - Inorganic Compounds, 2008, Retrieved from <URL: https://app.knovel.com/hotlink/itble/rcid:kpYHPEGE01/id:kt005XW7X1/yaws-handbook-properties/solubility-in-water-inorganic> ). The previously provided English machine translations of Xu (CN 112430736 A), Ming (CN 103073031 A), Ryu (KR 102033607 B1) and Yamaguchi (JP 2014156648 A) are referenced in the analysis below.
Regarding claim 1, Xu teaches a method for recovery of high value-added resources from lithium sludge and a fluoride source comprising:
adding a fluoride precipitant to lithium sludge, followed by precipitation and separation, to prepare lithium fluoride, which is an insoluble lithium compound (Sodium fluoride is added to the filtrate after impurity removal [from waste lithium-ion battery powder slurry], and lithium fluoride residue is obtained by filtration; [0006]-[0007]).
Xu does not teach the fluoride source being a fluoride sludge or the remaining steps (a-2) to (a-6) recited in the instant claim.
However, Ryu also teaches a method for recovery of high value-added resources from lithium sludge comprising:
reacting a lithium-containing solution with an aluminum compound to prepare Li-Al layered double hydroxide (LDH), which is an insoluble lithium compound (adding an aluminum compound to a lithium solution to form a lithium-aluminum layered double hydroxide and separating an unreacted aluminum containing liquid; [0033]);
subjecting the Li-Al layered double hydroxide (LDH), which is an insoluble lithium compound, to a sulfation reaction with a sulfuric acid compound to prepare a conversion product (sulfating the lithium-aluminum layered double hydroxide to produce lithium sulfate and separating an aluminum compound residue; [0022]); and,
water leaching the lithium contained in the conversion product to prepare a lithium concentrate (A high-concentration lithium sulfate aqueous solution can be prepared by dissolving the lithium sulfate formed through step (b) above in water; [0054]),
wherein the sulfuric acid compound is sulfuric acid or aluminum sulfate ([0045]).
Ryu also teaches that the lithium recovery rate by lithium phosphate precipitation is limited because lithium phosphate has a solubility in water of 0.034 g/100 mL, and that the method of using lithium-aluminum compounds can increase recovery of lithium ([0015]).
Yaws teaches that the solubility of lithium fluoride is 0.134 g/ 100 mL, which is even greater than that of lithium phosphate.
Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to apply the method of Ryu to the filtrate obtained following lithium fluoride precipitation according to the method of Xu. One of ordinary skill in the art would have been motivated to do so in order to recover lithium from the filtrate that would otherwise remain unrecovered by the method of Xu due to the significant solubility of lithium fluoride.
Ryu also teaches that the lithium concentrate can serve as a raw material to prepare lithium salts, such as lithium carbonate and lithium hydroxide ([0054]).
Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to recirculate the lithium concentrate as a lithium raw material in the step of preparing the lithium fluoride in the method of modified Xu. One of ordinary skill in the art would have been motivated to do so because it would enable them to convert the lithium to lithium fluoride and then to lithium hydroxide, as taught by Xu ([0008]-[0009]), which is a use suggested by Ryu.
Ryu further teaches that the filtrate remaining after the precipitation of the Li-Al layered double hydroxide can be processed in subsequent steps to make it reusable ([0042]), but does not teach reacting the filtrate with calcium fluoride.
However, Yamaguchi is also interested in recovery of metals from waste battery materials (abstract) and teaches that fluoride impurities can be removed by adding a calcium compound to separate the mixture into a calcium fluoride precipitate and a solution ([0036] and [0037]).
Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to react the filtrate remaining after the preparation of the Li-Al layered double hydroxide (LDH) in the method of modified Xu with a calcium compound to separate the filtrate into a calcium fluoride precipitate and residual process water, as taught by Yamaguchi. One of ordinary skill in the art would have been motivated to do so in order to remove fluoride ions from this solution so that it can be reused, as suggested by Ryu.
Regarding the fluoride precipitant being a fluoride sludge, Ming also teaches a method of preparing lithium fluoride by precipitation, and further teaches that the sodium fluoride precipitant is derived from a by-product of phosphate fertilizer ([0008]-[0010]) and mixed with water ([0025]), which will form a solution or slurry that is considered a fluoride sludge. Ming further teaches that using the by-product of fertilizer production reduces production costs and saves fluorite, a strategic resource ([0017]).
Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to use as the fluoride precipitant in the method of modified Xu a fluoride sludge, as taught by Ming. One of ordinary skill in the art would have been motivated to do so in order to reduce production costs and save the strategic resource of fluorite, as taught by Ming.
Regarding claim 4, modified Xu teaches the method of claim 1, where Xu teaches the lithium sludge is formed by treatment of battery powder with sulfuric acid ([0011]) and filtered, and will therefore be a solution which comprises lithium sulfate.
Regarding claim 5, modified Xu teaches the method of claim 1, where Ming teaches the fluoride sludge comprises sodium fluoride ([0023]).
Regarding claim 8, modified Xu teaches the method of claim 1, where the mass ratio of lithium in the lithium sludge to sodium fluoride in the fluoride sludge is 1:7-9, which corresponds to a molar ratio of lithium to fluoride of 1:(1.16-1.49), which lies in the instantly claimed range.
Regarding claim 9, modified Xu teaches the method of claim 1, where Ryu teaches the aluminum compound is sodium aluminate ([0065]), and can also be aluminum sulfate, aluminum hydroxide, alumina, or combinations thereof ([0039]).
Regarding claim 10, modified Xu teaches the process of claim 1, where Yamaguchi teaches that the use of calcium compounds to precipitate calcium fluoride can reduce the concentration of fluoride ions to below 0.001 g/L ([0059] and Table 5), which is equivalent to less than 1 ppm.
Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to perform the method of modified Xu where the calcium compound is added in an amount such that the residual process water after the precipitation of calcium fluoride is 1 ppm or less. One of ordinary skill in the art would have been motivated to do so in order to remove substantially all the fluoride from solution prior to reusing it.
It is also noted that the courts have also found that “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.” In re Aller, 220 F.2d 454, 456, 105 USPQ 233, 235 (CCPA 1955). See MPEP 2144.05 II. Therefore, the claimed range of fluoride concentration in the remaining process water merely represents an obvious variant and/or routine optimization of the values of the cited prior art.
Regarding claim 11, modified Xu teaches the process of claim 1, where Ryu teaches that the filtrate remaining after the precipitation of the Li-Al layered double hydroxide, the residual process water, can be processed in subsequent steps to make it reusable ([0042]).
Xu teaches various steps in which the pH of aqueous mixture are adjusted (e.g., [0026] and [0027]). It is also noted that simple use of this residual water is likely to alter the pH of nearly any solution to which it is added.
Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to recover and use the residual process water to adjust a pH for water treatment by reusing it in the process of modified Xu. One of ordinary skill in the art would have been motivated to do so in order to reduce resource use and because Ryu suggests reusing the water obtained following precipitation.
Regarding claim 14 and 15, modified Xu teaches the method of claim 1, where Ryu teaches the reaction temperature during the sulfation reaction between the Li-Al double layered hydroxide and the sulfuric acid compound is 290 °C and the reaction time is 2 hours ([0066]).
Claim 3 is rejected under 35 U.S.C. 103 as being unpatentable over Xu et al. (CN 112430736 A) in view of Ryu et al. (KR 102033607 B1), Yamaguchi et al. (JP 2014156648 A), Ming et al. (CN 103073031 A) and Yaws' Handbook of Properties for Environmental and Green Engineering (Solubility in Water - Inorganic Compounds, 2008, Retrieved from <URL: https://app.knovel.com/hotlink/itble/rcid:kpYHPEGE01/id:kt005XW7X1/yaws-handbook-properties/solubility-in-water-inorganic>), as applied to claim 1 above, and further in view of Choi (KR 20160122031 A) and Lipson (US 2021/0320293 A1). The previously provided English machine translations of Xu (CN 112430736 A), Ming (CN 103073031 A), Ryu (KR 102033607 B1), Yamaguchi (JP 2014156648 A), and Choi (KR 20160122031 A) are referenced in the analysis below.
Regarding claim 3, modified Xu teaches the method of claim 1, where Xu teaches the lithium sludge is generated in the process of recycling waste lithium secondary batteries ([0001] and [0006]), and Ming teaches the fluoride sludge is generated from in the fertilizer industry. Neither Ming nor Xu teach the lithium sludge being generated in the process of manufacturing lithium secondary batteries or the fluoride sludge being generated in the semiconductor and display industries.
However, Choi teaches that fluoride sludge generated in the semiconductor and display industries is also a useful sources of fluoride ions that can be recycled ([0009], [0011], [0037]). Choi further teaches that these waste materials can be converted to sodium fluoride ([0011]).
Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to replace in the method of modified Xu the fluoride sludge (waste-derived sodium fluoride) from the fertilizer industry taught by Ming with the fluoride sludge (waste-derived sodium fluoride) from the semiconductor and display industries taught by Choi. One of ordinary skill in the art would have been motivated to do so in order to recycle this useful resource, as taught by Choi, while also preserving the strategic resource of fluorite, as taught by Ming.
Additionally, Lipson teaches that it is important to recover cathode active materials, which include lithium, from not only recycled battery waste, but also from the lithium battery manufacturing process ([0006] and [0008]-[0009]).
Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to apply the method of modified Xu not only to sludge generated from the process of recycling waste lithium secondary batteries, but also to sludge generated in the manufacture of lithium secondary batteries. One of ordinary skill in the art would have been motivated to do so because Lipson teaches that there is an ongoing need to recover materials from such waste ([0006]).
Claim 6 is rejected under 35 U.S.C. 103 as being unpatentable over Xu et al. (CN 112430736 A) in view of Ryu et al. (KR 102033607 B1), Yamaguchi et al. (JP 2014156648 A), Ming et al. (CN 103073031 A) and Yaws' Handbook of Properties for Environmental and Green Engineering (Solubility in Water - Inorganic Compounds, 2008, Retrieved from <URL: https://app.knovel.com/hotlink/itble/rcid:kpYHPEGE01/id:kt005XW7X1/yaws-handbook-properties/solubility-in-water-inorganic>), as applied to claim 1 above, and further in view of Jafari et al. (Journal of Energy Storage, 2020, 31, 101564). The previously provided English machine translations of Xu (CN 112430736 A), Ming (CN 103073031 A), Ryu (KR 102033607 B1) and Yamaguchi (JP 2014156648 A) are used in the analysis below.
Regarding claim 6, modified Xu teaches the process of claim 1, but does not teach the concentration of lithium ion in the lithium sludge.
However, Xu does teach that the lithium sludges is prepared from 1 kg or waste lithium ion battery powder, 3 L (3 kg) of water, 1.3 kg of sulfuric acid and 1.2 kg of hydrogen peroxide solution ([0036]).
Furthermore, Jafari teaches a method for recovering lithium-containing battery powder that is 3.6% lithium by mass. Using Jafari’s battery powder in the method of Xu would give a lithium sludge that contains 3.6 g of lithium in a 6.5 kg mixture, which is equivalent to a lithium ion concentration of 550 ppm.
Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to use in the method of modified Xu a lithium sludge with a lithium ion concentration of 550 pm. One of ordinary skill in the art would have been motivated to do so because while Xu is silent on the preparation of the battery powder, Jafari teaches a method of generating said powder and preparing the mixture taught by Xu using Jafari’s battery powder would provide a mixture with this ion concentration.
Claim 7 is rejected under 35 U.S.C. 103 as being unpatentable over Xu et al. (CN 112430736 A) in view of Ryu et al. (KR 102033607 B1), Yamaguchi et al. (JP 2014156648 A), Ming et al. (CN 103073031 A) and Yaws' Handbook of Properties for Environmental and Green Engineering (Solubility in Water - Inorganic Compounds, 2008, Retrieved from <URL: https://app.knovel.com/hotlink/itble/rcid:kpYHPEGE01/id:kt005XW7X1/yaws-handbook-properties/solubility-in-water-inorganic>), as applied to claim 1 above, and further in view of Zhang et al. (CN 110668473 A). The previously provided English machine translations of Xu (CN 112430736 A), Ming (CN 103073031 A), Ryu (KR 102033607 B1), Yamaguchi (JP 2014156648 A), and Zhang (CN 110668473 A) are used in the analysis below.
Regarding claim 7, modified Xu teaches the process of claim 1, but Xu does not teach the concentration of fluoride ion being in the range of 500 ppm to 150,000 ppm.
However, Zhang teaches a similar method for precipitating lithium fluoride by combining lithium sludge and a fluoride precipitant, where that fluoride precipitant is provided as a 3 M NaF solution ([0035]). A solution that is 3 M in NaF will contain 57 g fluoride per liter of solution, which corresponds to approximately 57,000 ppm.
Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to use in the method of modified Xu a solution of fluoride sludge containing 57,000 ppm fluoride, as taught by Zhang, thereby meeting the limitations of claim 7. One of ordinary skill in the art would have been motivated to do so because Zhang teaches that their method is successful at achieving high-purity lithium fluoride powder ([0035]).
Claims 6 and 7 are rejected under 35 U.S.C. 103 as being unpatentable over Xu et al. (CN 112430736 A) in view of Ryu et al. (KR 102033607 B1), Yamaguchi et al. (JP 2014156648 A), Ming et al. (CN 103073031 A) and Yaws' Handbook of Properties for Environmental and Green Engineering (Solubility in Water - Inorganic Compounds, 2008, Retrieved from <URL: https://app.knovel.com/hotlink/itble/rcid:kpYHPEGE01/id:kt005XW7X1/yaws-handbook-properties/solubility-in-water-inorganic>), as applied to claim 1 above, and further in view of Ryu et al. (KR 102242686 B1; hereinafter “Ryu ‘686”). The previously provided English machine translations of Xu (CN 112430736 A), Ming (CN 103073031 A), Ryu (KR 102033607 B1), Yamaguchi (JP 2014156648 A), and Ryu ‘686 (KR 102242686 B1) are referenced in the analysis below.
Regarding claims 6 and 7, modified Xu teaches the process of claim 1, but does not teach the concentration of the lithium ion in the lithium sludge or the fluoride ion in the fluoride sludge.
However, Ryu ‘686 teaches a similar method of precipitating lithium from battery waste using a sodium fluoride precipitant, and further teaches that the concentration of lithium ion in the lithium sludge is 1000 ppm, and that 300 mL of this 1000 ppm lithium solution is combined with 50 mL of fluoride precipitant, where the molar ratio of Li:F is 1:2 (entry B-3, Table 2, translated below). This means that the concentration of the fluoride in the 50 mL NaF slurry must have been 12,000 ppm. Ryu ‘686 further teaches that these concentrations lead to greater than 80% recovery of LiF residual lithium concentrations of less than 200 ppm (Table 2).
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English machine translation of Table 2 from Ryu ‘686. (The table header is an apparent typographical error, as the table contents and accompanying [0159] reveal the precipitant is NaF, not NH4F, in these examples.)
Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to use in the method of modified Xu a lithium sludge with a concentration of 1000 ppm and a fluoride sludge with a concentration of 12,000 ppm, thereby arriving at the inventions of claims 6 and 7. One of ordinary skill in the art would have been motivated to do so because Ryu ‘686 teaches that these concentrations can be used to effectively recover lithium fluoride.
Claim 16 is rejected under 35 U.S.C. 103 as being unpatentable over Xu et al. (CN 112430736 A) in view of Ryu et al. (KR 102033607 B1), Yamaguchi et al. (JP 2014156648 A), Ming et al. (CN 103073031 A) and Yaws' Handbook of Properties for Environmental and Green Engineering (Solubility in Water - Inorganic Compounds, 2008, Retrieved from <URL: https://app.knovel.com/hotlink/itble/rcid:kpYHPEGE01/id:kt005XW7X1/yaws-handbook-properties/solubility-in-water-inorganic>), as applied to claim 1 above, and further in view of Li et al. (Waste Manag. 2010, 30, 2615-2621). The previously provided English machine translations of Xu (CN 112430736 A), Ming (CN 103073031 A), Ryu (KR 102033607 B1) and Yamaguchi (JP 2014156648 A) are used in the analysis below.
Regarding claim 16, modified Xu teaches the method of claim 1, where Ryu teaches water leaching of the conversion product. Ryu does not teach a solid/liquid ratio of the conversion product to water during this step.
However, it is well known in the art that the amount of product that can be leached will depend upon the ratio of the leaching solvent to the material being leached, with higher solid-to-liquid ratios generally resulting in less material leached from the solid. For example, Li teaches that as the as the solid-liquid ratio increases from 16 to 33 g/L the leaching efficiency of lithium in a waste leaching process decreases from ~100% to ~70% (Fig. 8, copied below) . However, lower solid/liquid ratios will result in more solvent waste for a given amount of solids to be leached, and also provide diminishing returns on leaching efficiency.
Therefore, it would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to optimize by routine experimentation the solid/liquid ratio during the water leaching, including into the instantly claimed range, as suggested by Li. One of ordinary skill in the art would have been motivated to do so in order to balance the recovery of lithium from the conversion product with the use of resources in the process.
Response to Arguments
Applicant's arguments filed 2 September 2026 with respect to the rejections under 35 USC § 103 have been fully considered but they are not persuasive.
Applicant argues, pages 10-11, that Ryu teaches away from the proposed combination because presented with the teachings of Ryu one of ordinary skill in the art would abandon Xu’s lithium fluoride precipitation entirely. While one of ordinary skill in the art may have chosen the route suggested by Applicant, it would have rendered the remainder of Xu’s method inoperable by precluding the use of Xu’s lithium fluoride to generate lithium hydroxide ([0023]). The use of Ryu’s method as only as a scavenging method to recover extra lithium would leave the majority of Xu’s method intact.
It is also noted the disclosure of desirable alternatives does not necessarily negate a suggestion for modifying the prior art to arrive at the claimed invention. In In re Fulton, 391 F.3d 1195, 73 USPQ2d 1141 (Fed. Cir. 2004).
In response to applicant's argument that the examiner's conclusion of obviousness is based upon improper hindsight reasoning, it must be recognized that any judgment on obviousness is in a sense necessarily a reconstruction based upon hindsight reasoning. But so long as it takes into account only knowledge which was within the level of ordinary skill at the time the claimed invention was made, and does not include knowledge gleaned only from the applicant's disclosure, such a reconstruction is proper. See In re McLaughlin, 443 F.2d 1392, 170 USPQ 209 (CCPA 1971). In the instant case, the combined teachings of Ryu and Yaw make it clear that the method of Xu could be improved by scavenging residual lithium from the solution following precipitation of lithium fluoride. Therefore, an obviousness rationale based upon such motivation does not require anything gleaned from applicant’s disclosure and is proper.
Conclusion
Applicant's amendment necessitated the new ground(s) of rejection presented in this Office action. Accordingly, THIS ACTION IS MADE FINAL. See MPEP § 706.07(a). Applicant is reminded of the extension of time policy as set forth in 37 CFR 1.136(a).
A shortened statutory period for reply to this final action is set to expire THREE MONTHS from the mailing date of this action. In the event a first reply is filed within TWO MONTHS of the mailing date of this final action and the advisory action is not mailed until after the end of the THREE-MONTH shortened statutory period, then the shortened statutory period will expire on the date the advisory action is mailed, and any nonprovisional extension fee (37 CFR 1.17(a)) pursuant to 37 CFR 1.136(a) will be calculated from the mailing date of the advisory action. In no event, however, will the statutory period for reply expire later than SIX MONTHS from the mailing date of this final action.
Any inquiry concerning this communication or earlier communications from the examiner should be directed to Nicholas A Piro whose telephone number is (571)272-6344. The examiner can normally be reached Mon-Fri, 8:00 am-5:00 pm.
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If attempts to reach the examiner by telephone are unsuccessful, the examiner’s supervisor, Sally Merkling can be reached at (571) 272-6297. The fax phone number for the organization where this application or proceeding is assigned is 571-273-8300.
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/NICHOLAS A. PIRO/
Assistant Examiner, Art Unit 1738
/PAUL A WARTALOWICZ/Primary Examiner, Art Unit 1735
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