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 .
Election/Restrictions
Applicant’s election without traverse of the species “wherein the leaching agent does not comprise an oxidizing agent or a reducing agent”, encompassed by claims 5 and 20, in the reply filed on March 30th, 2026 is acknowledged.
Claims 3-4 are withdrawn from further consideration pursuant to 37 CFR 1.142(b) as being drawn to a nonelected species, there being no allowable generic or linking claim. Election was made without traverse in the reply filed on March 30th, 2026.
Claim Objections
Claim 17 is objected to because of the following informalities:
The claim recites “[bis(2-ethylhexyl) hydrogen phosphate”, which contains an opening bracket ‘[‘ without a corresponding closing bracket ‘]’. The phrase should be edited to either include a corresponding closing bracket or to omit the bracket altogether.
Appropriate correction is required.
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 8 is 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.
Claim 8 recites the limitations “the copper salts”, “the aluminum salts”, and “the iron salts” in line 4. There is insufficient antecedent basis for this limitation in the claim. The claim previously recited “a copper salt, an aluminum salt, or an iron salt” in line 2. Because “the copper salts”, “the aluminum salts”, and “the iron salts” are each pluralized, it is unclear whether, for example, i) “the aluminum salts” must comprise or be the same as “a copper salt” as previously recited, and whether, for example, ii) “the aluminum salts” must themselves be plural. Notwithstanding the foregoing, “the copper salts”, “the aluminum salts”, and “the iron salts” will be interpreted to be any single or combination of more than one copper salt, aluminum salt, and iron salt, respectively, as individual claims are given their broadest reasonable interpretation in light of the specification. See MPEP § 2111.
Claim Rejections - 35 USC § 102
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 the appropriate paragraphs of 35 U.S.C. 102 that form the basis for the rejections under this section made in this Office action:
A person shall be entitled to a patent unless –
(a)(1) the claimed invention was patented, described in a printed publication, or in public use, on sale, or otherwise available to the public before the effective filing date of the claimed invention.
Claims 1-2, 7-8, 10, 12, 15, and 18-19 are rejected under 35 U.S.C. 102(a)(1) as being anticipated by Fraser (U.S. Patent No. 10,995,014, 2021).
Regarding claim 1, Fraser teaches a method for producing a cathode material precursor (Fraser, Fig. 2, Col. 14, line 65 - Col. 20, line 6) comprising:
leaching a black mass from a recycled lithium-ion battery stream with a leaching agent (Fraser, Fig. 2, H2SO4 and H2O2; Col. 15, lines 7-16) to obtain an aqueous acidic leach solution of metal salts comprising a nickel salt, a cobalt salt, a manganese salt, a lithium salt, and a plurality of impurity salts (Fraser, Table 2.0),
filtering the aqueous acidic leach solution to remove insoluble materials (Fraser, Col. 15, lines 7-16),
reducing amounts of the plurality of impurity salts in the filtered aqueous acidic leach solution by electrodeposition (Fraser, Col. 16, lines 31-34, electrowinning), by ion exchange (Fraser, Col. 17, lines 25-30) and by treating the filtered aqueous acidic leach solution with an aqueous base (Fraser, Col. 16, line 66 - Col. 17, line 3, “NMC hydroxides produced downstream were used as the neutralization agent”) and an oxygen-containing gas and removing insoluble materials (Fraser, Col. 17, lines 3-5, “The reactors were air sparged to ensure all iron was oxidized to the ferric form. Iron and aluminum precipitated as hydroxides.”),
adjusting amounts of the metal salts in the impurity reduced treated aqueous acidic leach solution to form an adjusted aqueous acidic leach solution (Fraser, Col. 18, lines 9-11, “Water was flashed in the evaporator to concentrate the solution to ~10-15/L Li prior to the subsequent cooling crystallization steps.”), and
coprecipitating the metal salts from the adjusted aqueous acidic leach solution (Fraser, Col. 18, lines 14-17, “As the solution was flash cooled, more water was evaporated which facilitated the crystallization of mainly nickel, manganese and cobalt as hydrated sulfates while leaving the primary impurities predominantly in the mother liquor.”).
Regarding claim 2, Fraser teaches the method of claim 1, as discussed above, wherein the leaching agent comprises sulfuric acid (Fraser, Fig. 2, H2SO4).
Regarding claim 7, Fraser teaches the method of claim 1, as discussed above, wherein the filtered aqueous acidic leach solution is treated with an aqueous base and an oxygen gas and insoluble materials are removed (Fraser, Col. 16, line 66 - Col. 17, line 5) prior to adjusting the amounts of the metal salts (Fraser, Col. 18, lines 9-11; this step occurs after the aqueous base and oxygen gas treatment).
Regarding claim 8, Fraser teaches the method of claim 7, as discussed above, wherein the plurality of impurity salts comprises an iron salt (Fraser, Col. 17, lines 3-4), and wherein treating the filtered aqueous acidic leach solution with the aqueous base and the oxygen-containing gas reduces the amount of the iron salt (Fraser, Col. 17, lines 4-9, impurity metal hydroxides are separated by filtration).
Regarding claim 10, Fraser teaches the method of claim 1, as discussed above, wherein the plurality of impurity salts comprises a copper salt and wherein amounts of the copper salt are reduced by electrodeposition (Fraser, Col. 16, lines 31-34, electrowinning).
Regarding claim 12, Fraser teaches the method of claim 1, as discussed above, wherein the plurality of impurity salts comprises a magnesium salt (Fraser, Table 2.0) and wherein amounts of the magnesium salt are reduced by ion exchange (Fraser, Col. 17, lines 31-36; Col. 4, lines 6-19).
Regarding claim 15, Fraser teaches the method of claim 7, as discussed above, wherein the plurality of impurity salts comprises a zinc salt and wherein amounts of the zinc salt are reduced by ion exchange (Fraser, Col. 17, lines 25-36).
Regarding claim 18, Fraser teaches the method of claim 1, as discussed above, wherein reducing the amounts of the plurality of impurity salts removes approximately 0% of the nickel salt, the cobalt salt, or the manganese salt (Fraser, Col. 17, lines 13-15, “The cake fed to the re-leach circuit was mixed with a sulfuric acid solution which dropped the pH to about 1.5 to dissolve any residual NMC solids present in the cake” (emphasis added).).
Regarding claim 19, Fraser teaches the method of claim 1, as discussed above, wherein, after reducing the amount of the plurality of impurity salts, the impurity-reduced aqueous acid leach solution has a pH < 4 (Fraser, Col. 17, lines 16-19, “Within the same reactor train the system was basified to increase the pH to about 4 to 5.5 to facilitate the re-precipitation of iron and aluminum.” If base was added to increase the pH to about 4 to 5.5, then the pH was < 4 prior to basification.), and wherein the method further comprises increasing the pH of the impurity-reduced aqueous leach solution to a pH > 4 prior to adjusting amounts of the metal salts (Fraser, Col. 17, lines 16-19, as above; Although Fraser undergoes an additional step of reducing the amount of the plurality of impurity salts via ion exchange prior to adjusting amounts of the metal salts, as detailed in Col. 17, lines 25-37, the claim does not require there to be no additional step of reducing the amount of the plurality of impurity salts after reaching a pH of > 4 in aqueous acidic leach solution.).
Claims 14 and 17 are rejected under 35 U.S.C. 102(a)(1) as being anticipated by Fraser (U.S. Patent No. 10,995,014, 2021), as applied to claims 12 and 15 above, and further evidenced by Lanxess (“Produce information - Lewatit® VP OC 1026”, 2011).
Regarding claim 14, Fraser teaches the method of claim 12, as discussed above, wherein ion exchange comprises passing the filtered aqueous leach solution through a column comprising a Lewatit VP OC 1026 ion exchange resin (Fraser, Col. 17, lines 31-33). While Fraser does not explicitly teach that this resin is impregnated with a dialkyl phosphonic acid, Lanxess clarifies that this is the case (Lanxess, Page 1, Paragraph 1, “Lewatit® VP OC 1026 is a crosslinked polystyrene based macroporous resin which contains Di-2-ethylhexyl-phosphat [sic] (D2EHPA).”). As Fraser’s method uses an acidic leach solution below the maximum pH recommended by Lanxess (Fraser, Col. 17, lines 28-30, pH of approximately 3; Lanxess, Paragraphs 1 and 4, pH should be less than 4), the phosphate would be protonated in Fraser’s method and would therefore comprise a dialkyl phosphonic acid.
Regarding claim 17 Fraser teaches the method of claim 15, as discussed above, wherein ion exchange comprises passing the filtered aqueous leach solution through a column comprising a Lewatit VP OC 1026 ion exchange resin (Fraser, Col. 17, lines 31-33). While Fraser does not explicitly teach that this resin is impregnated with bis(2-ethylhexyl) hydrogen phosphate, Lanxess clarifies that this is the case (Lanxess, Page 1, Paragraph 1, “Lewatit® VP OC 1026 is a crosslinked polystyrene based macroporous resin which contains Di-2-ethylhexyl-phosphat [sic] (D2EHPA).”). As Fraser’s method uses an acidic leach solution below the maximum pH recommended by Lanxess (Fraser, Col. 17, lines 28-30, pH of approximately 3; Lanxess, Paragraphs 1 and 4, pH should be less than 4), the phosphate would be protonated in Fraser’s method and would therefore comprise bis(2-ethylhexyl) hydrogen phosphate.
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.
Claim 9 is rejected under 35 U.S.C. 103 as being unpatentable over Fraser (U.S. Patent No. 10,995,014, 2021), as applied to claim 7 above.
Regarding claim 9, Fraser teaches the method of claim 7, as discussed above. The embodiment of Fraser relied upon in the rejection of claim 7 above (Fraser, Example 1, Col. 14, line 65 - Col. 20, line 6) does not explicitly teach that the treated aqueous acidic leach solution has a pH of from 5.5 to 6.5. However, Fraser teaches generally that a pH of 5.5 is appropriate to select in this step (Fraser, Col. 7, lines 42-47). It would therefore be obvious to select a pH of about 5.5 for the pH of the treated aqueous acidic leach solution.
Claim 13 is rejected under 35 U.S.C. 103 as being unpatentable over Fraser (U.S. Patent No. 10,995,014, 2021), as applied to claim 12 above, and further in view of Lanxess (“Produce information - Lewatit® VP OC 1026”, 2011).
Regarding claim 13, Fraser teaches the method of claim 12, as discussed above, wherein the filtered aqueous acidic leach solution has a starting pH of approximately 3 prior to ion exchange (Fraser, Col. 17, lines 28-30), which differs from the claimed range of 3.5 to 4.5, and an ending pH of greater than 1 and less than approximately 3 after ion exchange (Fraser, Col. 17, lines 28-30, pH is approximately 3 prior to loading on acidic column; Fraser, Col. 18, lines 1-4, the effluent from ion exchange is further acidified to a pH of 1 prior to NMC crystallization. Together, these observations give a range of ending pH which is less than approximately 3 but greater than 1.), which overlaps with the claimed range of from 2.5 to 3.5.
While Fraser’s starting pH of 3 prior to ion exchange differs from the claimed range of from 3.5 to 4.5, Lanxess teaches that Fraser’s ion exchange material is operable at pH values of less than 4 (Lanxess, Page 1, Paragraphs 1 and 4), which overlaps with the claimed range of from 3.5 to 4.5.
It would have been obvious to a person having ordinary skill in the art before the effective filing date of the invention to have modified Fraser’s method to have the starting pH prior to ion exchange to have a pH of less than 4 but higher than Fraser’s value of 3. Applying a known technique to a known device (method or product) ready for improvement to
yield predictable results is likely to be obvious. See KSR International Co. v. Teleflex Inc., 550 U.S. 398, 415-421, USPQ2d 1385, 1395 – 97 (2007) (see MPEP § 2143, D.). In the instant case, Fraser’s method was ready for improvement because selecting pH values above 3 but below 4 would yield the predictable effect of decreasing the amount of acid required to use in Fraser’s pre-conditioning step (Fraser, Col. 17, lines 28-30) prior to ion exchange while still remaining in a range that would be effective for Fraser’s ion exchange material, as taught by Lanxess (Lanxess, Page 1, Paragraphs 1 and 4).
Additionally, it would have been obvious to one of ordinary skill in the art before the
effective filing date of the invention to have selected the overlapping portions of the pH values before after ion exchange because selection of overlapping portions of ranges has been held to be a prima facie case of obviousness. See MPEP § 2144.05.I.
Claim 16 is rejected under 35 U.S.C. 103 as being unpatentable over Fraser (U.S. Patent No. 10,995,014, 2021), as applied to claim 15 above.
Regarding claim 16, Fraser teaches the method of claim 15, as discussed above, wherein the filtered aqueous acidic leach solution has a starting pH of approximately 3 prior to ion exchange (Fraser, Col. 17, lines 28-30) and an ending pH of greater than 1 and less than approximately 3 after ion exchange (Fraser, Col. 17, lines 28-30, pH is approximately 3 prior to loading on acidic column; Fraser, Col. 18, lines 1-4, the effluent from ion exchange is further acidified to a pH of 1 prior to NMC crystallization. Together, these observations give a range of ending pH which is less than approximately 3 but greater than 1.), which overlaps with the claimed range of from 1.5 to 2.5.
It would have been obvious to one of ordinary skill in the art before the
effective filing date of the invention to have selected the overlapping portion of the pH values after ion exchange because selection of overlapping portions of ranges has been held to be a prima facie case of obviousness. See MPEP § 2144.05.I.
Claim 21 is rejected under 35 U.S.C. 103 as being unpatentable over Fraser (U.S. Patent No. 10,995,014, 2021) in view of Lu (CN 116190844 A) (the attached machine translation is referenced below).
Regarding claim 21, Fraser teaches a method for producing a cathode material precursor (Fraser, Fig. 2, Col. 14, line 65 - Col. 20, line 6) comprising:
leaching a black mass from a recycled lithium-ion battery stream with a leaching agent (Fraser, Fig. 2, H2SO4 and H2O2; Col. 15, lines 7-16) to obtain an aqueous acidic leach solution of metal salts comprising a nickel salt, a cobalt salt, a manganese salt, a lithium salt, and a plurality of impurity salts (Fraser, Table 2.0),
filtering the aqueous acidic leach solution to remove insoluble materials (Fraser, Col. 15, lines 7-16),
treating the filtered aqueous acidic leach solution with an aqueous base (Fraser, Col. 16, line 66 - Col. 17, line 3, “NMC hydroxides produced downstream were used as the neutralization agent”) and an oxygen-containing gas and removing insoluble materials (Fraser, Col. 17, lines 3-5, “The reactors were air sparged to ensure all iron was oxidized to the ferric form. Iron and aluminum precipitated as hydroxides.”),
reducing amounts of the plurality of impurity salts in the treated aqueous acidic leach solution by ion exchange (Fraser, Col. 17, lines 25-30), wherein the pH of the treated aqueous acidic leach solution is reduced to greater than 1 and less than approximately 3 after ion exchange (Fraser, Col. 17, lines 28-30, pH is approximately 3 prior to loading on acidic column; Fraser, Col. 18, lines 1-4, the effluent from ion exchange is further acidified to a pH of 1 prior to NMC crystallization. Together, these observations give a range of ending pH which is less than approximately 3 but greater than 1.), which overlaps with the claimed range of from 2 to 4,
increasing the pH of the treated aqueous acidic leach solution to > 4 (Fraser, Col. 17, lines 16-19, “Within the same reactor train the system was basified to increase the pH to about 4 to 5.5 to facilitate the re-precipitation of iron and aluminum.”), and adjusting amounts of the metal salts in the treated aqueous acidic leach solution to form an adjusted aqueous acidic leach solution (Fraser, Col. 18, lines 9-11, “Water was flashed in the evaporator to concentrate the solution to ~10-15/L Li prior to the subsequent cooling crystallization steps.”), and
coprecipitating the metal salts from the adjusted aqueous acidic leach solution (Fraser, Col. 18, lines 14-17, “As the solution was flash cooled, more water was evaporated which facilitated the crystallization of mainly nickel, manganese and cobalt as hydrated sulfates while leaving the primary impurities predominantly in the mother liquor.”).
Fraser does not explicitly teach that the aqueous acidic leach solution has a pH of < 1. However, Lu teaches that a pH of from 0.5 to 1.5, which overlaps with the claimed range of <1, is effective for leaching Fraser’s battery material (lithium nickel manganese oxide) with sulfuric acid (Lu, [00106]).
The embodiment of Fraser relied upon in the instant rejection (Fraser, Example 1, Col. 14, line 65 - Col. 20, line 6) does not explicitly teach that the treated aqueous acidic leach solution has a pH >5. However, Fraser teaches generally that a pH of 5.5 is appropriate to select in this step (Fraser, Col. 7, lines 42-47). It would therefore be obvious to select a pH of about 5.5 for the pH of the treated aqueous acidic leach solution.
It would have been obvious to a person having ordinary skill in the art before the effective filing date of the invention to have selected a pH of the aqueous acidic leach solution of from 0.5 to 1.5 in Fraser’s method. The rationale to support a conclusion that the claim would have been obvious is that all 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 yielded nothing more than predictable results to one of ordinary skill in the art (see MPEP 2143.A.). The simple substitution of one known element for another is likely to be obvious when predictable results are achieved. See KSR International Co. v. Teleflex Inc., 550 U.S. 398, 415-421, USPQ2d 1385, 1395 - 97 (2007) (see MPEP § 2143.B.). In the instant case, selecting a pH of the aqueous acidic leach solution of from 0.5 to 1.5 in Fraser’s method would yield the predictable effect of leaching metals from Fraser’s material, as taught by Lu (Lu, [00106]).
Additionally, it would have been obvious to one of ordinary skill in the art before the
effective filing date of the invention to have selected the overlapping portions of the pH values because selection of overlapping portions of ranges has been held to be a prima facie case of obviousness. See MPEP § 2144.05.I.
Allowable Subject Matter
Claim 20 is allowed.
Claims 5 and 11 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: Fraser (U.S. Patent No. 10,995,014, 2021), Lanxess (“Produce information - Lewatit® VP OC 1026”, 2011), Kochhar (U.S. 2020/0078796 A1), Wang (U.S. 2021/0391606 A1), Snydacker (U.S. 2019/0044126 A1), and Rohde (WO 2023/148174 A1) are considered to be the closest prior art to the instant claims.
Regarding claim 5, Fraser teaches the method of claim 1, as discussed above, wherein the leaching agent comprises an oxidizing or reducing agent (Fraser, Fig. 2, Col. 15, lines 7-13, hydrogen peroxide), which differs from the claim limitation that the leaching agent does not comprise an oxidizing agent or a reducing agent.
Fraser further does not explicitly teach the black mass is heat treated prior to leaching with the aqueous acid. However, Rohde teaches that heat treatment of the black mass is a viable option for pyrolyzing organic (e.g. electrolyte) and polymeric (e.g. separator and binder materials) (Rohde, Page 9, line 29 - Page 10, line 2).
It would have been obvious to a person having ordinary skill in the art before the effective filing date of the invention to have modified Fraser’s method by heat treating the black mass prior to leaching, as Rohde teaches that this step removes unwanted battery components (Rohde, Page 9, line 29 - Page 10, line 2).
Regarding the claim limitation that the leaching agent does not comprise an oxidizing agent or a reducing agent, Kochhar teaches that hydrogen peroxide “may increase extraction of copper, cobalt, etc. but decrease nickel extraction” (Kochhar, [0240]). While this may generally motivate a person having ordinary skill in the art to exclude hydrogen peroxide from the leaching solution, this teaching would not be relevant to Fraser’s method specifically, as Fraser teaches that the method “achieve[s] complete dissolution of valuable metals such as nickel, cobalt and lithium” (Fraser, Col. 15, lines 11-13) even while including hydrogen peroxide. A person having ordinary skill in the art would therefore not have been motivated to apply Kochhar’s teaching of excluding hydrogen peroxide (an oxidizing agent or a reducing agent) to Fraser’s method.
Regarding claim 11, Fraser teaches the method of claim 10, as discussed above, but neither Fraser nor the other cited prior art references teach or suggest both that the filtered aqueous acidic leach solution has a starting pH of from 5 to 6 prior to electrodeposition and an ending pH of from 3.5 to 4.5 after electrodeposition. While Wang teaches that a pH range of from 0 to 5 is appropriate for electrodeposition of copper from an acidic battery leach solution (Wang, [0095]), which overlaps with the claimed range of from 5 to 6, there is no teaching that the electrodeposition would decrease the pH to an ending pH of from 3.5 to 4.5.
Regarding claim 20, Fraser teaches its shared features with claim 1 (see rejection of claim 1 under 35 U.S.C. 102(a)(1) above), but for the same reason as discussed above for claim 5, none of the cited prior art references would motivate a person having ordinary skill in the art to exclude an oxidizing agent or a reducing agent from the leaching agent.
Conclusion
The prior art made of record and not relied upon is considered pertinent to applicant's disclosure. Snydacker (U.S. 2019/0044126 A1) acknowledges that passing relevant solutions of metal salts through an acidic ion exchange material can decrease the pH of the solutions (Snydacker, [0186]).
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/ZACHARY JOHN BAUM/Examiner, Art Unit 1736
/ANTHONY J ZIMMER/Supervisory Patent Examiner, Art Unit 1736
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