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 .
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.
Claims 3-5, 9-13, 16 and 17 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.
Claim 3 recites “the first raw material includes a residue after nickel is selectively leached from a nickel-containing mixed hydroxide precipitate (MHP)”. However, claims 1 and 2 recite that the first raw material contains an oxidized transition metal, wherein the oxidized transition metal includes at least one of an oxidized nickel, oxidized cobalt, and an oxidized manganese. It is unclear whether there is actually any oxidized nickel in the first raw material that includes a residue after selectively leaching nickel from the nickel-containing MHP. For the purpose of examination and in view of the specifications ([0039], [0099], and Table 1), the limitation in claim 3 will be interpreted to mean that there will be some oxidized nickel leftover in the residue after selectively leaching nickel from the nickel-containing MHP.
Claims 3-5 and 9 are rejected under 35 USC § 112 by virtue of its dependence on claim 3.
Claim 10 recites the limitation "the sulfuric acid solution". There is insufficient antecedent basis for this limitation in the claim. However, claim 8 recites leaching a metal salt to obtain a leached liquid from a raw material mixture in a sulfuric acid solution. For the purpose of examination and in view of [0056] of the specifications, claim 10 will be interpreted to depend on claim 8 instead of claim 6. Therefore, it is respectfully suggested to amend claim 10 by changing “The method of claim 6” to “The method of claim 8”. Claim 10 also recites that the “weight ratio of the sulfuric acid solution relative to a total weight of the raw material mixture is in a range from 3 to 7”. It is unclear what the weight ratio is because the ratio is recited incorrectly. For the purpose of examination and in view of the calculated weight ratio of example 2 in the specifications (Table 3, [00123]), the weight ratio of the sulfuric acid solution relative to a total weight of the raw material mixture will be interpreted to be in a range between 3:1 and 7:1.
Claim 11 recites the limitation "the sulfuric acid solution". There is insufficient antecedent basis for this limitation in the claim. However, claim 8 recites leaching a metal salt to obtain a leached liquid from a raw material mixture in a sulfuric acid solution. For the purpose of examination and in view of [0057] of the specifications, claim 11 will be interpreted to depend on claim 8 instead of claim 7. Therefore, it is respectfully suggested to amend claim 11 by changing “The method of claim 7” to “The method of claim 8”. Claim 11 also recites that the “weight ratio of the sulfuric acid solution relative to a total weight of the raw material mixture is in a range from 5.95 to 6.5”. It is unclear what the weight ratio is because the ratio is recited incorrectly. For the purpose of examination and in view of the calculated weight ratio of example 2 in the specifications (Table 3, [00123]), the weight ratio of the sulfuric acid solution relative to a total weight of the raw material mixture will be interpreted to be in a range between 5.95:1 and 6.5:1.
Claim 12 recites the limitation "the sulfuric acid solution" that is used to obtain the leached liquid. There is insufficient antecedent basis for this limitation in the claim. However, claim 8 recites leaching a metal salt to obtain a leached liquid from a raw material mixture in a sulfuric acid solution. For the purpose of examination and in view of [0058] of the specifications, claim 12 will be interpreted to depend on claim 8 instead of claim 5. Therefore, it is respectfully suggested to amend claim 12 by changing “The method of claim 5” to “The method of claim 8”.
Claim 13 recites “an oxidizing agent other than a sulfuric acid solution or a reducing agent is not used in obtaining the leached liquid”. It is unclear whether a reducing agent can be used to obtain the leach liquid or not. For the purpose of examination and in view of [0059] in the specifications, the limitation will be interpreted to mean that no additional oxidizing agent or additional reducing agent, other than the sulfuric acid solution, will be used in obtaining the leached liquid.
Claim 16 recites the limitation "wherein nickel, cobalt and manganese are extracted". There is insufficient antecedent basis for this limitation in the claim. However, claim 15 recites “wherein obtaining at least one of nickel, cobalt and manganese from the leached liquid comprises extracting”. For the purpose of examination and in view of [0067]-[0068] of the specifications, claim 16 will be interpreted to depend on claim 15 instead of claim 12. Therefore, it is respectfully suggested to amend claim 16 by changing “The method of claim 12” to “The method of claim 15”.
Claim 17 recites the limitation " nickel sulfate, cobalt sulfate and manganese sulfate". There is insufficient antecedent basis for this limitation in the claim. However, claim 16 recites “nickel, cobalt and manganese are extracted in the form of nickel sulfate, cobalt sulfate and manganese sulfate, respectively”. For the purpose of examination, claim 17 will be interpreted to depend on claim 16 instead of claim 13. Therefore, it is respectfully suggested to amend claim 17 by changing “The method of claim 13” to “The method of claim 16”.
Claim Rejections - 35 USC § 102
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)(2) the claimed invention was described in a patent issued under section 151, or in an application for patent published or deemed published under section 122(b), in which the patent or application, as the case may be, names another inventor and was effectively filed before the effective filing date of the claimed invention.
Claims 1-5, 8, 9, 12, and 14 are rejected under 35 U.S.C. 102(a)(1) as being anticipated by Hawker et al. (WO-2022183243-A1, hereinafter “Hawker”).
Regarding claim 1 and 2, Hawker is directed to producing a co-precipitate comprising nickel, manganese, and cobalt ([0002]) (i.e., transition metals). Hawker discloses an embodiment of a method of a co-precipitate comprising at least two metals selected from nickel, cobalt, and manganese, the method comprising (lines 1-3 of [00103]):
An oxidized feed having more of at least two metals (lines 6-7 of [00103]) (i.e., a first raw material containing an oxidized transition metal, which also meets the recited oxidized transition metals in claim 2) and a reduced feed having more of the at least two metals (lines 8-9 of [00103]) (i.e., a second raw material containing a reduced transition metal, which also meets the recited reduced transition metals in claim 2);
Treating the feed mixture with an aqueous solution to form a leachate, wherein the feed mixture that may be produced by combining separate feeds, each of which is an oxidized feed and a reduced feed (lines 15 of [00103] and lines 6-8 of [00113]) (i.e., obtaining a leached liquid containing at least one of nickel, cobalt and manganese from a raw material mixture of the first raw material and the second raw material); and
At least two metals (of nickel, cobalt, or manganese) in the co-precipitate that is derived from the feed solution or leachate (tenth and eleventh paragraph of [00103]) (i.e., obtaining at least one of nickel, cobalt and manganese from the leached liquid).
Regarding claim 3-5 and 9, Hawker discloses that mixed hydroxide precipitate (MHP) may provide an oxidized feed (i.e., first raw material), wherein the MHP can be contacted with an acidic solution comprising an oxidant to cause the cobalt to be stabilized in the solid phase (i.e., residue) and the nickel dissolved in the acidic solution. The solid phase is then separated from the acidic solution, wherein the solid phase forms at least part of the feed mixture (line 6 of [0036] and [0041]). The acid in the weak acid leach solution may be sulfuric acid (last line of [0048]) (i.e., a sulfuric acid solution is supplied to the nickel-containing MHP together with the oxidizing agent to selectively leach nickel, and wherein the residue after selectively leaching nickel from the nickel-containing MHP is used as the first raw material in claim 5, and meets claim 3). The oxidant may be sodium or potassium persulfate (lines 1-3 of [0044]) (i.e., the oxidizing agent is a metal persulfate in claim 5 and meets claim 4). The sulfuric acid solution is in a concentration of 0.5M (line 8 of [0048]) (which meets the sulfuric acid concentration range of 0.5M to 1.5M in claim 9).
Claim 12 is treated as dependent on claim 8, as set forth above.
Regarding claim 8 and 12, Hawker discloses treating the feed mixture with an aqueous solution to form a leachate comprising at least two metals from nickel, cobalt, or manganese (lines 2 and 15-16 of [00103]). The aqueous solution comprises a leaching agent that may be sulfuric acid and the pH of the aqueous solution may be less than 2.5 ([0062] and lines 1-3 of [0063]) (i.e., obtaining the leached liquid comprises leaching a metal salt that contains at least one of nickel, cobalt and manganese in a sulfuric acid solution in claim 8 and the recited pH range in claim 12).
Regarding claim 14, Hawker discloses separating impurities from the leachate. The impurities may include iron, aluminum, copper, and zinc ([00104]-[00105]) (i.e., separating a residual metal from the leached liquid).
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.
Claims 6 and 7 are rejected under 35 U.S.C. 103 as being unpatentable over Hawker as applied to claim 1 above, and further in view of Ha et al. (KR-20210112727-A, hereinafter “Ha”).
Regarding claims 6 and 7, Hawker discloses that the feed mixture can be obtained from a cathode material from a lithium ion battery (lines 1-2 of [0051]) (i.e., secondary battery) but does not disclose that the cathode active material is reduced in claim 6, or that the cathode is pulverized and the pulverized material is then reduced to prepare the reduced transition metal containing nickel, cobalt, and manganese as the second raw material in claim 7.
Ha is directed to a method for recovering an active metal of a lithium secondary battery ([0001]) and discloses that a preliminary positive electrode active material mixture may be prepared from recovered cathodes by pulverization. The cathode active material is then reduced to form a lithium precursor and transition metal precursor via a reductive reaction with hydrogen ([0047] and [0083]-[0084]). The cathode active material includes nickel, cobalt, and manganese ([0041]) (i.e., pulverizing a cathode of a secondary battery, and reducing a pulverized material to prepare the reduced transition metal containing nickel, cobalt and manganese in claim 7, and meets claim 6).
It is noted that both the Hawker and Ha references are directed to a recovery of transition metals from a mixture.
Therefore, before the effective filing date of the claimed invention, it would have been obvious to one of ordinary skill in the art to modify the method of Hawker by pulverizing and reducing the cathode active materials containing nickel, cobalt, and manganese as the second raw material as taught by Ha because (1) cathode active materials that are pulverized and reduced are easier to recover in a slurry state and the recovery efficiency of the active metal recovery process is improved (Ha, [0026] and [0047]); and (2) the reduced transition metals from the reduced cathode active materials can be used as the reduced feed or second raw material, as taught by Hawker.
Claims 10 and 11 are rejected under 35 U.S.C. 103 as being unpatentable over Hawker as applied to claim 8 above.
Claims 10 and 11 are treated as dependent on claim 8, as set forth above.
Regarding claims 10 and 11, Hawker does not disclose that the weight ratio of sulfuric acid solution to a total weight of the raw material mixture is between 3:1 and 7:1 in claim 10 or that the weight ratio of sulfuric acid solution to a total weight of the raw material mixture is between 5.95:1 and 6.5:1 in claim 11.
Hawker does disclose that the feed mixture is treated with an aqueous solution comprising a sulfuric acid leaching agent to achieve a targeted pH to leach out the desired transition metals (lines 2 and 15-17 of [00103] and [0062]). Therefore, it would have been obvious to one of ordinary skill in the art to realize that the amount and weight of the sulfuric acid relative to the total weight of the raw material mixture is an important variable to achieve the targeted pH for leaching the desired transition metals, i.e., a result-effective variable. It would have been obvious to conduct routine experimentation to determine the optimal weight ratio of sulfuric acid to raw material mixture and eventually come to the recited weight ratios in claims 10 and 11 without undue experimentation.
Claim 13 is rejected under 35 U.S.C. 103 as being unpatentable over Hawker, as applied to claim 1 above, and further in view of Ha, Krupka et al. (Geochemical Factors Affecting the Behavior of Antimony, Cobalt, Europium, Technetium, and Uranium in Vadose Sediments, 2002, hereinafter “Krupka”), and Bysar (US-1671004-A).
Regarding claim 13, Hawker does not disclose that no additional oxidizing agent or reducing agent, other than the sulfuric acid, is used in obtaining the leach liquid.
Hawker does disclose that the solid oxidized feed, after treating MHP with a metal persulfate and sulfuric acid, contains cobalt stabilized in the solid phase in the form of Co(III) (Hawker, [0042]). Ha also discloses that the reduced cathode active material feed contains a preliminary transition metal precursor which includes Ni (Ha, [0092]). Krupka is directed to exploring different properties, such as oxidation/reduction, of different elements, including cobalt, in vadose zone sediments, which is pertinent to the instant application’s problem of recovering transition metals such as cobalt (Krupka, Abstract) and discloses that cobalt(III) can be used as a strong oxidizing agent (pg. 29, section 3.1). Bysar is directed to a process for extracting nickel (Bysar, pg. 1, first column, lines 1-2) and discloses using metallic nickel as a reducing agent to reduce nickel present in a solution to the nickelous form, Ni(II), in a process for recovering nickel (pg. 2, first column, lines 34-40).
It is noted that Hawker, Ha, and Bysar are all references directed to a recovery of a transition metal from a mixture and that Krupka is directed to the properties of cobalt, which is pertinent to the instant application’s problem of recovering transition metals.
Therefore, before the effective filing date of the claimed invention, it would have been obvious to one of ordinary skill in the art to modify the method of Hawker by not using any additional oxidizing or reducing agent, other than sulfuric acid, to obtain the leached liquid. Hawker discloses that the solid oxidized feed contains Co(III), which can be used as an oxidizing agent as taught by Krupka. Ha discloses that the reduced feed contains metallic Ni, which can be used as a reducing agent as taught by Bysar. Therefore, it would have been obvious to not add any additional oxidizing or reducing agent to the method of Hawker because Hawker teaches that (1) a reduced feed and an oxidizing feed can be mixed together with a sulfuric acid to generate a leachate; (2) an oxidized feed needs to be additionally treated with a reducing agent and a reduced feed needs to be additionally treated with an oxidizing agent (Hawker, [00103], paragraph 7-8); and (3) the solid oxidized feed can act as the oxidizing agent (as taught by Krupka) to the reduced feed and the reduced feed can act as the reducing agent (as taught by Bysar) to the oxidizing feed when the two feeds are mixed together. Thus, no additional oxidizing or reducing agent is necessary to treat the reduced or oxidized feed to obtain the leachate, thereby reducing the costs for additional reagents and limiting the introduction of impurities from external reagents which is preferable (Hawker, lines 9-11 of [0067]).
Claims 15-17 are rejected under 35 U.S.C. 103 as being unpatentable over Hawker as applied to claim 1 above, and further in view of Van Der Meer et al. (US-20240274912-A1, hereinafter “Van”).
Claim 16 is treated as dependent on claim 15 and claim 17 is treated as dependent on claim 16, as set forth above.
Regarding claims 15-17, Hawker does not disclose extracting from the leached liquid at least one of nickel, cobalt, and manganese in the form of nickel sulfate, cobalt sulfate, or manganese sulfate using at least one of a phosphoric acid-based or carboxylic acid-based extractant.
Van is directed to a method for extracting metals from the black mass of lithium-ion batteries, wherein the black mass comprises lithium, nickel, and cobalt (Abstract). Van discloses adding sulfuric acid to adjust the pH of the leaching solution before adding the extractants ([0046]). Nickel and cobalt are then recovered by using a solvent extraction (i.e., obtaining at least one of nickel, cobalt and manganese from the leached liquid comprises extracting at least one of nickel, cobalt and manganese in claim 15) to produce a nickel sulphate or cobalt sulphate solution (i.e., nickel, cobalt and manganese are extracted in the form of nickel sulfate, cobalt sulfate and manganese sulfate, respectively in claim 16). The solvent extraction is carried out using extraction chemicals having a carboxylic acid functional group (i.e., nickel sulfate, cobalt sulfate and manganese sulfate are extracted using at least one of a phosphoric acid-based extractant and a carboxylic acid-based extractant in claim 17) ([0070] and [0072]).
It is noted that Hawker and Van are references directed to a recovery of a transition metal from a mixture.
Therefore, before the effective filing date of the claimed invention, it would have been obvious to one of ordinary skill in the art to modify the method of Hawker by extracting from the leached liquid at least one of nickel, cobalt, and manganese in the form of nickel sulfate, cobalt sulfate, or manganese sulfate using at least one of a phosphoric acid-based or carboxylic acid-based extractant as taught by Van, because a carboxylic acid-based extractant can be used to extract nickel or cobalt in the form of nickel or cobalt sulfate to produce a rather pure nickel or cobalt sulfate solution and that solvent extraction is the preferred method for separation and recoveries (Van, [0070], [0072], and [0086]).
Conclusion
Any inquiry concerning this communication or earlier communications from the examiner should be directed to NATHAN N HOANG whose telephone number is (571)270-1950. The examiner can normally be reached Mon-Thurs 7am-4pm; Fri 7am-11am.
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/NATHAN NGOC-NGOC HOANG/Examiner, Art Unit 1772
/YOUNGSUL JEONG/Primary Examiner, Art Unit 1772