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 .
Priority
Applicant’s claim to foreign priority in application no. CN202111133678.3, filed September 27, 2021, is acknowledged.
Claim Rejections - 35 USC § 112
The following is a quotation of 35 U.S.C. 112(b):
(b) CONCLUSION.—The specification shall conclude with one or more claims particularly pointing out and distinctly claiming the subject matter which the inventor or a joint inventor regards as the invention.
The following is a quotation of 35 U.S.C. 112 (pre-AIA ), second paragraph:
The specification shall conclude with one or more claims particularly pointing out and distinctly claiming the subject matter which the applicant regards as his invention.
Claim 1, and dependent Claims 2-9, are rejected under 35 U.S.C. 112(b) or 35 U.S.C. 112 (pre-AIA ), second paragraph, as being indefinite for failing to particularly point out and distinctly claim the subject matter which the inventor or a joint inventor (or for applications subject to pre-AIA 35 U.S.C. 112, the applicant), regards as the invention.
Regarding Claim 1, the claim recites “taking solid phase to obtain manganese dioxide and graphite residue”. It is unclear what is meant by “taking”. It is unclear if the MnO2 or graphite residue to remain or not in the solution.
Regarding Claim 6, the claim recites “the leaching process”. There is insufficient antecedent basis for this limitation.
Regarding Claim 7, the claim recites ‘performing solid-liquid separation’ multiple times, but it is unclear how many times solid-liquid separation is actually required to satisfy the claim limitations. The claim also recites ‘to liquid phase’, and it is unclear if ‘liquid phase’ refers to the liquid phase of claim one, or a different liquid phase, and if the multiple recitations of ‘to liquid phase’ refer to different liquid phases or all of the same liquid phase. It is further unclear from the claim construction if calcium salt is being added twice or not, and whether or not all the chemicals are added together or during separate steps. It is unclear if Claim 7 is referring to multiple additional steps or one additional step of reaction and solid-liquid separation.
Regarding Claim 9, it is unclear (see Claim 7 112b rejection) which ‘liquid phase’ the claim is referring to as both Claim 1 and Claim 9 have multiple recitations of ‘liquid phase’.
Regarding Claim 10, the claim recites “the reagent”. There is insufficient antecedent basis for this limitation.
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.
Claims 1-2, 4-5 and 10 are rejected under 35 U.S.C. 103 as being unpatentable over Wang (cited by Applicant in IDS filed February 9, 2024, CN 111206148 A, English Translation provided) in view of McNally (US 20220223932 A1), Arakawa (US 20180073098 A1) and Szolga (US 20220205064 A1).
Regarding Claim 1, Wang discloses a method for selectively recovering valuable metals in waste lithium battery (Abstract), comprising:
(1) adding sulfate salts such as sodium sulfate or ammonia sulfate to waste lithium battery powder, roasting (calcinating), and performing water leaching to obtain lithium carbonate solution and filter residue (Abstract; para. [0011]; para. [0021]);
(2) adding sulfuric acid to the filter residue for leaching, and performing solid-liquid separation (pressure filtration reads on solid-liquid separation) (Abstract, para. [0041]; para. [0060], see step 4); and
(3) extracting and reverse extracting the liquid phase to obtain nickel and cobalt sulfate solution and manganese sulfate solution (Abstract; para. [0042]; para. [0052] and para. [0060], step 5; see extraction with P507 and P204, followed by stripping and formation of pure sulfate solutions of nickel, cobalt and manganese).
Wang fails to disclose adding an iron-containing compound to the filter residue with the sulfuric acid.
McNally teaches adding iron sulfate to sulfuric acid as a reducing agent in order to reduce cobalt, nickel and manganese, thereby increasing the solubility of these metals in the leaching solution while reducing the need for other additional reducing agent, such that the metals can then be selectively recovered (para. [0017]-[0018]; para. [0025], wherein acid is sulfuric acid).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have added iron sulfate to the sulfuric acid and filter residue, as taught by McNally, for the invention disclosed by Wang, in order to increase the solubility of cobalt, nickel and manganese in the leaching solution, while reducing the need for other additional reagent (see teachings above).
Wang and is silent towards obtaining solid phase manganese dioxide and graphite residue from solid-liquid separation.
Arakawa teaches wherein Mn ions from lithium ion battery material solution precipitate to form MnO2 when leached in sulfuric acid, which is then removed by solid-liquid separation, thereby obtaining a leached sulfate solution ready for selective recovery of nickel, cobalt and manganese (Abstract; para. [0047]-[0048]; para. [0036]; para. [0038]).
Solzga teaches wherein flow filtration or centrifuge (solid-liquid separation) also removes solids and residues such as graphite in order to isolate the manganese, cobalt and nickel liquid leach solution (para. [0078]).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have used solid-liquid separation to remove precipitated MnO2, as taught by Arakawa, and to remove graphite, as taught by Solzga, for the invention disclosed by Wang, in order to achieve a nickel, cobalt, manganese leaching solution free of solid residue and thereby ready for selective extraction and recovery of the elements (see teachings above).
Regarding Claim 2, Wang discloses wherein the sulfate is ammonium sulfate or solidum sulfate (para. [0011]).
Regarding Claim 4 and Claim 5, McNally discloses iron sulfate, such as FeSO4 (Abstract; para. [0017]), which reads on (Claim 4) a divalent (FeSO4) iron compound, and (Claim 5) one of ferrous sulfate.
Regarding Claim 10, Wang discloses wherein the reagent used for extracting is at least one of P204 or P507 (para. [0052]; para. [0060], see steps 5).
Claim 3 is rejected under 35 U.S.C. 103 as being unpatentable over Wang (cited by Applicant in IDS filed February 9, 2024, CN 111206148 A, English Translation provided) in view of McNally (US 20220223932 A1), Arakawa (US 20180073098 A1) and Szolga (US 20220205064 A1), as applied to Claim 1 above, in further view of Jiang (CN 109935922 A, English Translation provided).
Regarding Claim 3, Wang discloses wherein the temperature of water leaching is 30-90C, which reads on the claimed 50-90C range. Wang discloses a preferred liquid-solid ratio range of (1-5):1 (para. [0013]), but fails to disclose the claimed (8-12):1 range.
Jiang discloses a similar invention wherein the liquid-solid ratio in water leaching may more broadly be (3-30):1 in order to achieve the required lithium concentration in the lithium salt solution (para. [0019]). Thus, Jiang teaches wherein the liquid-solid ratio is also a result effective variable, the result being the lithium concentration in the lithium salt solution after water leaching.
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have used a further liquid-solid ratio of (3-30):1, which overlaps the claimed (8-12):1 range, as taught by Jiang, for the invention disclosed by Wang. One would be motivated to do this in order to tailor the lithium concentration in the lithium salt solution (see teaching above), and because the liquid-solid ratio is an art recognized result-effective variable, the result being lithium concentration, and it has been held that discovering an optimum value of a result effective variable involves only routine skill in the art. See MPEP 2144.05.I.
Claim 6 is rejected under 35 U.S.C. 103 as being unpatentable over Wang (cited by Applicant in IDS filed February 9, 2024, CN 111206148 A, English Translation provided) in view of McNally (US 20220223932 A1), Arakawa (US 20180073098 A1) and Szolga (US 20220205064 A1), as applied to Claim 1 above, in further view of Dong (CN 111994925 A, English Translation provided).
Regarding Claim 6, Wang discloses wherein the pH for leaching in step (2) is adjusted to 1.5 and heated to 60C, which reads on the claimed pH range of 0.5-2 and temperature range of 60-90C (para. [0060], step 3; see also para. [0015], wherein temperature may be 30-90C).
McNally further discloses wherein the iron ion concentration in the sulfuric acid may be from 0.005M-0.1M (para. [0024]), and Wang discloses a filter residue solid to liquid ratio of the sulfuric acid leaching solution of 1:(1-7) (para. [0041]). One of ordinary skill would be able to calculate and appreciate that the filter residue to iron compound mass ratio therefore overlaps with the claimed range of 10:(0.5-2). For example, 0.10M iron ions from iron sulfate for 1 L of solution comprising a filter residue to liquid ratio of 1:7 would require 15.2g of iron compound and 142.8 g of filter residue, or a filter reside of 10:(1.06).
In the case where the claimed ranges “overlap or lie inside ranges disclosed by the prior art” a prima facie case of obviousness exists. In re Wertheim, 541 F.2d 257, 191 USPQ 90 (CCPA 1976); In re Woodruff, 919 F.2d 1575, 16 USPQ2d 1934 (Fed. Cir. 1990). See MPEP § 2144.05.I.
Wang only discloses a leaching time up to 6 hours however (para. [0015]), and fails to disclose the claimed 10-20 hour range.
Dong teaches a leaching time of 6-10 hours in order to form soluble sulfates of nickel, cobalt and manganese (para. [0021]-[0022]).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have increased the leaching time to up to 10 hours, as taught by Dong, for the invention disclosed by Wang, in order to ensure the leaching and formation of soluble nickel, cobalt and manganese sulfates (see teaching above). Additionally, one of ordinary skill in the art would appreciate that Dong demonstrates that the leaching time is a result effective variable, the result being the leaching and formation of soluble nickel, cobalt and manganese sulfates, and it has been held that discovering an optimum value of a result effective variable involves only routine skill in the art. See MPEP 2144.05.I.
Claims 7-9 are rejected under 35 U.S.C. 103 as being unpatentable over Wang (cited by Applicant in IDS filed February 9, 2024, CN 111206148 A, English Translation provided) in view of McNally (US 20220223932 A1), Arakawa (US 20180073098 A1) and Szolga (US 20220205064 A1), as applied to Claim 1 above, in further view of Cao (CN 111082043 A, English Translation provided), Chen (CN 103627904 A, English Translation provided) and Nishikawa (US 20230107938 A1).
Regarding Claim 7, Wang discloses adding the filter residue in step (1) to liquid phase (sulfuric acid solution) for reaction and performing solid-liquid separation and obtaining nickel cobalt manganese sulfate solution (see Claim 1 above; see also teachings by Arakawa and Szolga above regarding solid-liquid separation).
Wang fails to disclose wherein step (3) further includes adding iron powder to the liquid phase for reduction reaction after solid-liquid separation in step (2) and before extracting.
Wang also does not disclose adding sodium fluoride and calcium salt, and adding aluminum sulfate and calcium salt, to a liquid phase for reaction, to obtain the nickel cobalt manganese sulfate solution.
Wang teaches removing impurities prior to extraction (para. [0070]).
Cao teaches adding iron powder, reacting and filtering (solid-liquid separation) in order to remove copper from leaching solution (para. [0009], step (2)).
Chen further teaches adding calcium carbonate to adjust the pH of the leaching solution, thereby precipitating through neutralization and removing aluminum and iron through solid-liquid separation, and further adding sodium fluoride to remove calcium ions and magnesium ions from the solution through solid-liquid separation (para. [0014]; para. [0019]-[0020]).
Nishikawa teaches adding aluminum sulfate in order to uptake and remove fluorine, such that aluminum and fluorine are removed together (para. [0173]; para. [0180]-[0182]), and wherein addition with calcium carbonate improves these effects wherein the calcium can further be removed by reaction forming calcium sulfate and solid-liquid separation (para. [0182]).
It would have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to have added iron powder to react and remove copper by solid-liquid separation, as taught by Cao, to have added calcium carbonate and sodium fluoride in order to react and remove aluminum and iron by solid-liquid separation, as taught by Chen, and to have then added calcium carbonate and aluminum sulfate in order to filter out and remove the remaining fluorine by solid-liquid separation, as taught by Nishikawa, for the invention disclosed by Wang. One would be motivated to do these steps in order to remove impurities of copper, aluminum, iron and fluorine, prior to extraction of the manganese, cobalt and nickel (see teachings above).
Regarding Claim 8, Chen and Nishikawa disclose wherein the calcium slat is calcium carbonate (Chen, para. [0019]-[0020]; Nishikawa, [0180]-[0182]).
Regarding Claim 9, Wang discloses wherein the filter residue in step (1) is added to the liquid phase (sulfuric acid solution) (see Claim 1 above), and Wang and Chen disclose adjusting the pH in step (3) and prior to extraction (Wang, para. [0060], step 5; Chen904, para. [0019]-[0020]).
Conclusion
The prior art made of record and not relied upon is considered pertinent to applicant's disclosure.
Jiang (cited above, CN 109935922 A, English Translation provided, additional teachings): further discloses mixing lithium battery waste with low-valence sulfates, followed by roasting (calcination) and water leaching to obtain lithium carbonate and leach residue solution (Abstract; para. [0012]-[0013]; [0016]), and subjecting the leaching residue to acid leaching with sulfuric acid for recovery of nickel, cobalt and manganese through solvent extraction with P204 and P507 (para. [0015]; para. [0017]; [0026]).
Any inquiry concerning this communication or earlier communications from the examiner should be directed to CATHERINE P SMITH whose telephone number is (303)297-4428. The examiner can normally be reached Monday - Friday 9:00-4:00 MT.
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If attempts to reach the examiner by telephone are unsuccessful, the examiner’s supervisor, Keith Walker can be reached at (571)-272-3458. The fax phone number for the organization where this application or proceeding is assigned is 571-273-8300.
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CATHERINE P. SMITH
Patent Examiner
Art Unit 1735
/CATHERINE P SMITH/Examiner, Art Unit 1735
/KEITH WALKER/Supervisory Patent Examiner, Art Unit 1735
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