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 .
Compliance with 37 C.F.R. § 1.121
The amendments to the claims filed on 12/03/2025 is considered non-compliant , because the status identifiers of the claims 165, 168, and 170 are incorrect. These claims are withdrawn as indicated in the previous office action, and should be labeled "(Withdrawn)". In the interest of compact prosecution, the amendments have been entered. Applicant is required to comply with 37 C.F.R. § 1.121 for any future amendments.
Remarks
The amendments and remarks filed on 12/03/2025 have been entered and considered. The text of those sections of Title 35, U.S. Code not included in this action can be found in a prior office action. The rejections and/or objections presented herein are the only rejections and/or objections currently outstanding. Any previously presented objections or rejections that are not presented in this Office Action are withdrawn. Claims 143-149 and 151-172 are pending; Claims 1-142 and 150 are cancelled; Claims 143, 146-149, 151, 157-159, 161, and 169 are amended; Claim 172 is new; Claims 165, 168, and 170 are withdrawn; and Claims 143-149, 151-164, 166-167, 169, and 171-172 are under examination.
3. The species election requirement set forth in the prior office action dated 09/03/2025 is still maintained since the elected species is not allowable.
Withdrawal of Objections
The objection to Claims 151 and 158 in the previous office action is withdrawn due to the amendment to the claims filed on 12/03/2025.
Withdrawal of Rejections
The rejection of Claims 147 and 150 under 35 U.S.C. 112(a) as failing to comply with the written description requirement is withdrawn due to the amendment to or cancellation of the claims filed on 12/03/2025.
The rejection of claims 146, 150, 157, 159, 161, and 169 under 35 U.S.C. 112(b) is withdrawn due to the amendment or cancellation of the claims as well as Applicant’s clarification in the 12/03/2025 response (pages 10-11).
The rejection of Claims 143, 145, 147, and 150-160 under 35 U.S.C. 102(a)(1) as being anticipated by Hallberg et al. is withdrawn due to the amendment or cancellation of the claims.
The rejection of Claims 143-145, 147, and 150-161 under 35 U.S.C. 103 over Hallberg et al. is withdrawn due to the amendment or cancellation of the claims.
The rejection of Claims 143-147, 149-156, and 158-160 under 35 U.S.C. 103 as being unpatentable over Gunasekara et al. is withdrawn due to the amendment or cancellation of the claims.
The rejections of Claims 143-156, 158-164, 166-167, 169, and/or 171 under 35 U.S.C. 103 over Gunasekara et al. in view of Hallberg et al., Michelson et al., Duyvesteyn et al., Bertuol et al., Hay et al., Hyeung et al., Byrd et al. and/or Pandey et al. are withdrawn due to the amendment or cancellation of the claims.
Claim Objections
Claim 146 is objected to due to the recitation of abbreviations for enzyme names, such as CymA, DFE, DmkA, DmkB, EetA, EetB, FmnA, FmnB, GACE, MtrA, MtrC, Ndh2, OmcF, OmcS, OmcZ, PplA, and T4ap. Abbreviations should be spelled out at least once in the claims. Appropriate correction is required. This objection is maintained.
Claim Interpretation
Claim 146 recites the limitations comprising a slash “/’ symbol, such as “MtrA/MtrC” and “OmcF/OmcS/OmcZ”. According to Applicant’s arguments in the response filed on 12/03/2025 (the para spanning pages 10 and 11), the recited slash “/’ symbol is interpreted as “and”.
Claim 169 recites the symbol “
PNG
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36
30
media_image1.png
Greyscale
” in the structure of the peptide (connected to the NH- group of His) in the claim. According to Applicant’s arguments in the response filed on 12/03/2025 (page 11, para 3), the recited symbol is interpreted as any unspecified part (molecule or atom).
Claim Rejections - 35 USC § 112(a) or 112, First Paragraph
Claims 143-149, 151-164, 166-167, 169, and 171-172 are rejected under 35 U.S.C. 112(a) or 35 U.S.C. 112 (pre-AIA ), first paragraph, because the specification, while being enabling for a method of recovering metals/nickel from an oxide ore by using a microorganism(s) of Shewanella species along with tricarboxylic acid (e.g. citric acid) or dicarboxylic acid (e.g. oxalic acid), does not reasonably provide enablement for a method of recovering metals from an oxide ore by using any microorganism(s) (e.g. acidophilic bacteria) along with any organic acid. The specification does not enable any person skilled in the art to which it pertains, or with which it is most nearly connected, to make and/or use the invention commensurate in the entire scope with these claims.
In making a determination as to whether an application has met the requirements for enablement under 35 U.S.C. 112 ¶ 1, the following factors enumerated In re Wands, 8 USPQ2d 1400, at 1404 (CAFC 1988) are considered: (1) the breadth of the claims, (2) the amount of direction or guidance presented, (3) the presence or absence of working examples, (4) the nature of the invention, (5) the state of the prior art, (6) the relative skill of those in the art, (7) the predictability or unpredictability of the art, and (8) the quantity of experimentation necessary. While it is not essential that every factor be examined in detail, those factors deemed most relevant should be considered.
The breadth of the claims. The instant claims are directed in part to a method of recovering nickel, manganese, and/or cobalt from an oxide ore, comprising: (a) combining at a pH ranging from about 5 to 9 a microorganism(s), a substrate mixture, oxide ore, an organic acid in an aqueous phases; (b) maintaining the mixture for a period of time to reduce an amount of ferric iron in the ore to ferrous iron, and solubilize ferrous iron, nickel, cobalt, and manganese in the aqueous phase; and (c) isolating the aqueous phase as a leach solution, wherein the aqueous phase in the step (b) is maintained at the pH of 5-9. The microorganism(s) recited in the base claim 143 can be any microorganism(s) which encompasses any fugus, Archaea and bacteria (including acidophilic bacteria such as Acidithiobacillus ferrooxidans, Sulfobacillus benefaciens, Acidicaldus organivorans, and Acidiphilium SJH); and the organic acid recited in the claim can be any organic compound which acts as a weak proton donor. The dependent claim 147 limits the microorganism(s) to be Shewanella bacteria or a laundry list of other bacteria or archaea belonging to a wide range of different species or genius such as Candidatus, Telmatospirillum, Nitrosococcus, Magnetospirillum, Geoglobus, Sideroxydans, Archaeoglobus, Clostridium, Listeria, Thermincola and Bacillus. The dependent claim 157 limits the organic acid to be various dicarboxylic acid, tricarboxylic acid, monocarboxylic acid, hydroxamic acid, and mugineic acid.
The amount of direction or guidance presented and the existence of working examples. In the specification there are working examples (Examples 1-20), which demonstrate that S. putrefaciens (a bacterium of Shewanella species) and citric acid (an organic acid in group of tricarboxylic acids) can effectively solubilize and leach ferrous, nickel, manganese, and cobalt from an oxide ore under claimed conditions. However, these examples failed to show a bacterium of Shewanella species can be combined with any organic acid for effectively solubilizing and leaching the metals from an oxide ore under claimed conditions. In addition, there is no data or examples in the specification to support any other microorganisms including any fungus, Archaea, and any other bacteria (including acidophilic bacteria and those recited in the claim 147) can be used in the claimed method to combine with any organic acid and form a mixture at pH of 5-9, and effectively solubilize/leach the metals from an oxide ore. There is no evidence in the specification to support any organic acid (including those recited in the claim 157) can be used to combine with acidophilic bacteria such as A. ferrooxidans, S. benefaciens, A. organivorans, and Acidiphilium SJH at the pH of 5-9 for effectively solubilizing and leaching the metals from an oxide ore. The specification fails to provide any information and guidance regarding how to use the claimed method to reach a goal of effectively solubilizing and leaching ferrous, nickel, manganese, and cobalt from an oxide ore by applying a combination of any microorganisms and any organic acid to the oxide ore while pH is maintained in a range of 5-9.
The state of prior art, and the predictability or unpredictability of the art. The art as evidenced by Tzeferis et al. (of record, described below in the 103 rejection) teaches that organic acids including tricarboxylic acid/citric acid and dicarboxylic acid/oxalic acid are very effective at solubilizing/extracting metals (nickel and iron) from laterite ores, and monocarboxylic acids including lactic, formic, acetic and salicylic acids are relatively ineffective (see abstract). The teachings of the prior art demonstrate that tricarboxylic acid and dicarboxylic acid are effective organic acids for solubilizing metals from ores. There is no teaching or suggestions in the art to support that any organic acids (including hydroxamic acid and mugineic acid recited in claim 157) can effectively solubilize/leaches metals from the ore. Furthermore, the art as evidenced by Hallberg et al. (cited in IDS, described below in the 103 rejection) teaches a leaching process for recovering nickel from a laterite ore (title and abstract), comprising steps: (a) combining at a low pH of about 1.8 an iron-reducing acidophilic bacterium, a substrate mixture, an inorganic acid H2SO4, and an oxide ore in an aqueous phase to form a mixture; (b) maintaining the mixture for a period of time to reduce an amount of ferric iron and solubilizing/leaching ferrous iron, nickel, cobalt, and manganese from the ore; and (c) isolating the aqueous phase as a leach solution (page 621: methodology sections 2.1 – 2.4, and left col/para 1/line 7- para 2/last line; page 622: section 3.2/lines 1-3; Fig. 2); wherein the acidophilic bacterium is Acidithiobacillus ferrooxidans, Sulfobacillus benefaciens, Acidicaldus organivorans, or Acidiphilium SJH. The teachings of the prior art demonstrate it is essential to use a strong inorganic acid H2SO4 to generate a mixture at a low pH of about 1.8 such that the acidophilic bacterium can effectively solubilizes/leaches the metals from the ore. There is no teaching or suggestions in the art to support that at a pH of 5-9 the acidophilic bacterium can effectively solubilize/leaches the metals from the ore when an organic acid is used.
The quantity of experimentation necessary. It is not routine in the art to use a combination of any microorganism and any organic acid at the pH of 5-9 to reduce an amount of ferric iron in an ore to ferrous iron, and solubilize/leach ferrous iron, nickel, cobalt, and manganese in an aqueous phase to generate a leaching solution, especially for using acidophilic bacteria which require a low pH of about 1.8 as well as using fungus and Archaea for reductive dissolution of ferric iron minerals. Neither the prior art nor disclosure of the specification shows that a combination of any microorganism and any organic acid can be effectively used at the pH of 5-9 for reductive dissolution of ferric iron minerals and generating a leaching solution comprising solubilized ferrous iron, nickel, cobalt, and manganese. Therefore, in absence of some guidance as to how to use a combination of any microorganism and any organic acid at the pH of 5-9 for generating a leaching solution from ores, one of skill in the art would have to carry out a large amount of experimentation to find which additional steps or additional compounds need to be included in the disclosed method, or how to modify the disclosed method, to reach the goal of reductive dissolution of ferric iron minerals and recovery of nickel, cobalt, and manganese in a leaching solution.
Therefore, Claims 143-149, 151-164, 166-167, 169, and 171-172 are not enabled due to the lack of information and guidance with regard to how to use a combination of any microorganism and any organic acid at the pH of 5-9 for recovery of nickel, cobalt, and manganese from ores. Neither the specification nor the prior art enable the entire scope of the claimed invention.
Claim Rejections - 35 USC § 112(b), or 112, Second Paragraph
Claims 147 and 151 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 pre-AIA the applicant regards as the invention.
Claim 147 is indefinite due to the recitation of microorganisms followed by a limitation placed in a parenthetical phrase, i.e. “Telmatospirillum (Alphaproteobacterial Genus)”. A parenthetical phrase is akin to “for example”, which render the claim indefinite because it does not clearly indicate if the limitation in the parentheses is required. Furthermore, the claim is indefinite due to the recitation of “Frateuria-like isolate WJ2”. This term is not defined in the specification. It is unclear based on what specific standard (e.g. color, shape, GC content, or a metabolic pathway), a bacterium can be considered as a Frateuria-like isolate WJ2. This rejection is maintained.
Claim 151 is indefinite due to the recitation of “… fermentation products derived from carbonaceous waste products, molasses, sugar, beet sugar, cane sugar, glucose derived from palm oil, dextrose hydrolyzed from corn, dextrose hydrolyzed from cornstarch, or sucrose-containing materials, acetate, lactate, or mixtures thereof”. It is unclear whether the “molasses, sugar, beet sugar, cane sugar, glucose … acetate, lactate” is recited for defining the fermentation products or as standing-alone reducing agent. For the purpose of examination, the recited phrase is interpreted as “… fermentation products, acetate, lactate, or mixtures thereof; wherein the fermentation products are derived from the carbonaceous waste products, molasses, sugar, beet sugar, cane sugar, glucose derived from palm oil, dextrose hydrolyzed from corn, dextrose hydrolyzed from cornstarch, or sucrose-containing materials”.
Claim Rejections - 35 USC § 103
Claims 143-147, 149, 151-160 and 172 are rejected under 35 U.S.C. 103 as being unpatentable over Gunasekara et al. (US 2024/0254591, 2024, effective filing date: May 12, 2021, of record) in view of Tzeferis et al. (Hydrometallurgy, 1994, 36(3): 345-360, the abstract is of record), as evidenced by Lin et al. (SSRN electronical journal, 4082769, pages 1-21, published on April 13, 2022, cited in IDS).
Gunasekara et al. teach a process for recovering trace metal from a metal oxide-containing starting material, i.e. a metallic ore (reading on the “oxide ore” in claim 143) by utilizing metal-oxide reducing bacteria to reduce metal oxides in the ore (abstract). The process of Gunasekara et al. comprises the steps: (a) contacting/combining the metallic ore with the metal-oxide reducing bacteria and an aqueous medium/phase comprising substrate mixture (to form a mixture); (b) maintaining the mixture for a period of time under suitable condition to reduce the metal oxide and convert at least a portion of the metal oxide to a water-soluble metal salt, and releasing (solubilizing) at least a portion of trace metal in the ore into the aqueous medium; and (c) separating/isolating the aqueous medium, and recovering the trace metal from the aqueous medium (abstract, paras 0006, 0012-14, 0022-0026, examples 1-2, Claim 1, Fig. 2); wherein the metal oxide comprises iron oxide (e.g. FeOOH, Fe(OH)3 or Fe2O3) and/or manganese oxide, and the metal-oxide reducing bacteria are preferably from Shewanellaceae and/or Geobacteraceae, which reduce the iron oxide (i.e. ferric iron) and manganese oxide into a soluble-form iron [i.e. ferrous iron Fe(II)], or a soluble-form manganese Mn(II), which are then combined with chloride ion Cl⁻ (i.e. a ligand that binds the metal) to form an water-soluble iron chloride (FeCl2) or manganese chloride (MnCl2) (abstract, Claims 3-6 and 8-9, paras 0020/lines 6-10, 0025, 0027/lines 7-8, 0030, 0032, 0076-78, 0081, 0113); wherein the mixture (the aqueous medium) comprises a substrate mixture comprising a lactate substrate, a combination of lactate and glucose, or an acetate substrate (reading on the reducing agent in claims 143 and 151) (paras 0113/lines 10-12, 0115/page 8/last 6 lines, and 0039); wherein the trace metal preferably is nickel and cobalt (para 0042/last 2 lines); wherein the metal-oxide starting material (metallic ore) is an laterite ore (para 0045) (reading the laterite ore in claim 152); and wherein the metal-oxide reducing bacteria from Shewanellaceae are preferably Shewanella oneidensis MR-1, S. putrefaciens CN-32, or S. loihica PV-4 (reading on the Shewanella species and specific Shewanella strains recited in the claims 147 and 149) (Table 1, paras 0029 and 0030), and the metal-oxide reducing bacteria from Geobacteraceae are preferably Geobacter sulfurreducens PCA or G. metalliresucens GS-15 (Table 2, paras 0031-32). Overall, Gunasekara et al. teach a mixture formed in the step (a), comprising: at least one metal-oxide reducing bacterium, an oxide ore, a substrate mixture (including a reducing agent of lactate, glucose and/or acetate substrate contained in the aqueous medium), a ligand (a compound having a chloride ion Cl⁻ contained in the aqueous medium, see page 8, last 6 lines), and an aqueous phase, which either meet the limitations or are comparable to the mixture components in the step (a) of claim 143. Regarding the limitation about reducing ferric iron in the ore to ferrous iron, and solubilizing iron, nickel, cobalt, and manganese in an aqueous phase recited in the step (b) of the claim 143, Gunasekara et al. teach reducing ferric iron in the ore to ferrous iron and solubilizing iron, manganese, and trace metal in an aqueous phase, and specifically teach nickel and cobalt are preferred trace metal in their method. Thus, it would have been obvious to solubilize iron, manganese, nickel, and cobalt in the aqueous phase in the method of Gunasekara et al. for recovering nickel, cobalt, and/or manganese.
Gunasekara et al. do not expressively teach that the ligand comprises an organic acid, specifically citric acid, as required by the claims 143, 157, and/or 172. However, it would have been obvious to one of ordinary skill in the art to further include an organic acid(s), such as citric acid or citric acid plus oxalic acid, as a ligand in the mixture/aqueous medium of step (a) in the method of Gunasekara et al. for increasing solubilization of metal ions from the ore, thus enhancing production of the soluble trace metals (e.g. nickel ions), because it is well known in the art that citric acid and oxalic acid improve solubility of metals from oxide ore. In support, Tzeferis et al. investigate ability of organic acids to solubilize nickel and iron from Greek laterite, and they reveal that citric acid is the most effective organic acid for nickel extraction, achieving recoveries to 60%; and that oxalic acid remarkably improves iron extraction, releasing more than 60% of iron (see abstract).
Regarding the pH range recited in Claims 143 and 158, Gunasekara et al. teach that bio-extraction is carried out in the aqueous medium at a neutral pH ranged from not less than about 5 to not greater than about 9 or 7.5 (para 0087). In view of the teachings of Gunasekara et al., it would have been obvious to maintain the pH of the mixture and the aqueous phase in the steps (a) and (b) to be in a range from about 5 to 9 in the method suggested by Gunasekara et al. and Tzeferis et al. for recovering metal from ores.
Regarding Claim 144, Gunasekara et al. teach an order of adding the microorganism cells to a suspension of the iron oxide ore (para 0113/lines 8-12), and Gunasekara et al. also teach the iron oxide ore is comprised in M1 aqueous medium, the medium comprising a ligand; a substrate mixture (such as lactate or lactase plus glucose); and an aqueous phase (para 0115: page 8/last 6 lines, page 9/lines 3-4). Thus, it would have been obvious to add the microorganism cells to a suspension/slurry comprising the iron oxide ore, ligand, substrate mixture, and aqueous phase in the method suggested by Gunasekara et al. and Tzeferis et al.
Regarding the claim 145, Gunasekara et al. are silent about whether the bacterial microorganisms are derived from the ore. However, how the microorganisms are obtained (derived from) is directed to a process of producing the microorganisms. The claimed microorganisms are not limited to the manipulation process of obtaining (deriving) them from ores, only to the structure implied by the manipulation process. Gunasekara et al. teach the metal-oxide reducing bacteria having all the claimed structures (including specific bacteria recited in the dependent claims 147 and 149). In addition, the bacteria of Gunasekara et al. have the same function as those microorganisms in the claimed method with regard to reducing ferric iron and solubilizing ferrous iron, nickel, cobalt, and manganese. Thus, the teachings of Gunasekara et al. meet the additional limitation in the claim 145, in the absence of evidence to the contrary. See MPEP 2113.
Regarding Claim 146, the Shewanella oneidensis and Geobacter sulfurreducens taught by Gunasekara et al. respectively produce a combination of MtrA and MtrC as well as a combination of OmcF, OmcS and OmcZ, as evidenced by Lin et al., who teach that Shewanella oneidensis expresses MtrA, MtrB, and MtrC, and that Geobacter sulfurreducens expresses OmcF, OmcS and OmcZ (page 3: para 2/lines 2-5, para 3/lines 6-8). Regarding Applicant’s elected species of a combination of Omc and Mtr enzymes, Gunasekara et al. teach using a combination of Shewanellaceae bacterium (e.g. S. oneidensis) and Geobacteraceae bacterium (e.g. G. sulfurreducens) in their method for reducing iron oxide in the ore (Claims 7, 4, and 6; paras 0035, 0030, 0032; Tables 1 and 2). Thus, the microorganisms used in method of Gunasekara et al. produce a combination of Omc and Mtr enzymes, meeting the elected species in the claim.
Regarding Claim 153, Gunasekara et al. teach that iron in the ore can be 20% by weight or higher (para 0048, last 3 lines), thus rendering the claim to be obvious.
Regarding Claim 154, Gunasekara et al. teach that the ore comprises nickel at an amount of about 1% to about 2%, or about 1-1.5% (paras 0045/lines 2-4, 0047/last 2 lines), thus rendering the claim to be obvious.
Regarding Claim 156, Gunasekara et al. teach that the ore comprises cobalt at an amount of about 0.2-0.25% (para 0047/line 6), thus rendering the claim to be obvious.
Regarding Claim 155, Gunasekara et al. teach that the ore is associated with manganese, as indicated above. Gunasekara et al. further teach that the ore comprises the metal oxide comprising iron oxide, e.g. FeOOH, Fe(OH)3 or Fe2O3 (paras 0027/lines 7-8, 0076/lines 6-8). Thus, the ore of Gunasekara et al. is associated with ferric iron minerals, and ferric iron (oxy)hydroxide.
Regarding Claim 159, Gunasekara et al. teach that the reduction of the iron oxide is carried out under anaerobic (i.e. anoxic) or microaerobic condition (paras 0115/page 9/lines 8-10, 0029/last 5 lines).
Regarding Claim 160, the limitations about releasing specific amounts of trace metals (nickel and cobalt) recited in the claim are directed to the outcome, rather than steps of the claimed method, i.e. the claim is directed to what the method does, not to what the method is. The method suggested by Gunasekara et al. and Tzeferis et al. comprises all the steps recited in the claim. In the absence of evidence to the contrary, it is presumed that methods having substantially the same steps are capable of generating the same outcome. Furthermore, Gunasekara et al. teach an amount from at least about 10% to at least about 95% by weight of the trace metal in the ore is released into the aqueous medium (para 0083); and Tzeferis et al. teach recovering up to 60% nickel from the ore. Thus, combined teachings of Gunasekara et al. and Tzeferis et al. render the claim to be obvious.
Therefore, the invention as a whole would have been prima facie obvious to a person of ordinary skill in the art before the effective filing date of the claimed invention.
Claims 143-147, 149, 151-161 and 172 are rejected under 35 U.S.C. 103 as being unpatentable over Gunasekara et al. (US 2024/0254591, 2024, effective filing date: May 12, 2021, of record) over Tzeferis et al. (Hydrometallurgy, 1994, 36(3): 345-360, the abstract is of record), as applied to Claims 143-147, 149, 151-160 and 172, further in view of Hallberg et al. (Minerals Engineering, 2011, 24: 620–624, cited in IDS), as evidenced by Lin et al. (SSRN electronical journal, 4082769, pages 1-21, published on April 13, 2022, cited in IDS).
The teachings of Gunasekara et al. and Tzeferis et al. are described above.
Regarding Claim 161, Gunasekara et al. and Tzeferis et al. do not expressively teach that the aqueous phase of step (c) is isolated from the mixture by sedimentation of solids.
However, it would have been obvious to separate or isolate the aqueous solution (aqueous phase) from the mixture by sedimentation of solids and decantation of aqueous liquid phase in the method suggested by Gunasekara et al. and Tzeferis et al. for recovering a leach solution containing nickel and/or cobalt, because it is a common practice in the art to carry out solid-liquid separation through sedimentation of solids, as supported by Hallberg et al., who teach a leaching process for recovering nickel from a laterite ore, (title and abstract), comprising steps of combining an iron-reducing acidophilic bacterium with a substrate mixture comprising sulfur element and citric acid in a aqueous phase/medium; maintaining the mixture to reduce ferric iron in the ore and solubilize ferrous iron, nickel, cobalt, and manganese in the aqueous phase; and separating the aqueous phase of dissolved nickel from the mixture (page 621: methodology sections 2.1 – 2.4, and left col/para 1/line 7- para 2/last line; page 622: section 3.2/lines 1-3; Fig. 2); wherein the remaining undissolved laterite ore is separated by sedimentation (page 621, right col., para 2, line 10).
It is noted that the teachings of Hallberg et al. about contents of iron, nickel, manganese, and cobalt in the ore (see page 621: left col/para 3/lines 1-9; and page 620: right col/lines 1-4) also meet the limitations in the claims 153-156.
Therefore, the invention as a whole would have been prima facie obvious to a person of ordinary skill in the art before the effective filing date of the claimed invention.
Claims 143-149, 151-160 and 172 are rejected under 35 U.S.C. 103 as being unpatentable over Gunasekara et al. (US 2024/0254591, 2024, effective filing date: May 12, 2021, of record) over Tzeferis et al. (Hydrometallurgy, 1994, 36(3): 345-360, the abstract is of record), as applied to Claims 143-147, 149, 151-160 and 172, further in view of Michelson et al. (Environ. Sci. Technol. 2019, 53:3480−3487, of record), as evidenced by Lin et al. (SSRN electronical journal, 4082769, pages 1-21, published on April 13, 2022, cited in IDS).
The teachings of Gunasekara et al. and Tzeferis et al. are described above.
Regarding Claim 148, Gunasekara et al. and Tzeferis et al. do not teach the mixture formed in the step (a) comprises an electron shuttle, specifically a flavin. However, Gunasekara et al. further teach that Shewanella bacteria have the ability, through a process called extracellular electron transport (EET), to reduce insoluble iron oxide and they utilize oxidized iron for cellular respiration (in the absence of oxygen) to convert the insoluble iron oxides to soluble metals (e.g., FeCl2) (first half of para 0020).
It would have been obvious to one of ordinary skill in the art to further include a flavin, as an electron shuttle in the EET process, in the mixture/aqueous medium of step (a) in the method suggested by Gunasekara et al. and Tzeferis et al. for facilitating reduction of insoluble iron oxide by Shewanella bacteria (e.g. S. oneidensis MR-1), thus enhancing production of the soluble trace metals, because it is well known in the art that flavin is an important electron shuttle in the EET process, which delivers electron from Shewanella bacteria to insoluble iron oxide for promoting the reduction of iron oxide to soluble metal and generating ATP. In support, Michelson et al. teach that bacteria have evolved mechanisms for transport of respiratory electrons to the outer membrane in a process defined as extracellular electron transport (EET); Shewanella bacteria use a strategy of electron shuttling via redox mediator flavins to generate ATP through reduction of insoluble electron acceptors such as Fe(III) (i.e. ferric iron) to ferrous iron; and electron shuttling of flavins is a dominant pathway for metal oxide reduction by the species S. oneidensis MR-1; and once being reduced, the reduced flavins may transfer electrons as shuttles to a metal oxide (page 3480: left col/lines 7-13, right col/lines 2 and 5 lines; page 3481: left col/lines 1-4). Michelson et al. demonstrate that flavin electron shuttle allows electrons generated from lactate oxidation in S. oneidensis MR-1 to be shuttled to metal oxides (as a physical distant electron acceptor) without direct physical contact between S. oneidensis MR-1 and the metal oxide (abstract, lines 6-9 and 15-16).
Therefore, the invention as a whole would have been prima facie obvious to a person of ordinary skill in the art before the effective filing date of the claimed invention.
Claims 143-147, 149, 151-160, 162-164, 166-167, 169 and 172 are rejected under 35 U.S.C. 103 as being unpatentable over Gunasekara et al. (US 2024/0254591, 2024, effective filing date: May 12, 2021, of record) over Tzeferis et al. (Hydrometallurgy, 1994, 36(3): 345-360, the abstract is of record), as applied to Claims 143-147, 149, 151-160 and 172, further in view of Duyvesteyn et al. (US Patent No. 5626648, cited in IDS), Bertuol et al. (Chem. Eng. Technol. 2012, 35(12): 2084–2092, of record), Hay et al. (Journal of Inorganic Biochemistry, 1993, 52:17-25, of record), Hyeung et al. (KR 20090097704 A, 2009, machine-translated English version is of record), and Byrd et al. (US 2006/0030007, 2006, of record), as evidenced by Lin et al. (SSRN electronical journal, 4082769, pages 1-21, published on April 13, 2022, cited in IDS), Wołowicz et al. (Chemical Engineering Journal, 2012, 197:493–508, of record), and Luo et al. (US Patent No: 6365147, 2002, of record).
The teachings of Gunasekara et al. and Tzeferis et al. are described above.
Regarding Claims 162-164, 166-167, and 169, Gunasekara et al. and Tzeferis et al. do not teach the steps (d) – (j) recited in the claim 162, specifically comprising: applying a Gly-Gly-His peptide conjugated with a polystyrene bead for selectively binding nickel and/or cobalt from the aqueous phase/leach solution obtained in step (c) to form a conjugate-metal ion complex; isolating the complex and eluting the bound metal(s) from the complex with an acid, subjecting the eluted metal(s) solution to electrowining, and recovering metal(s) from a surface of cathode. However, Gunasekara et al. teach steps for isolating, purifying and recovering trace metals including nickel and/or cobalt, which are comparable to the steps (d) – (j) in the claims. In details, Gunasekara et al. teach processes for selectively separating and recovering the trace metal from the aqueous phase/leach solution and further purifying/recovering the metals, by processes including: absorption of dissolved trace metals, chelating ion exchange, and electrowinning (paras 0099/lines 1-4, and 0103/lines 1-2 and 5-6).
Duyvesteyn et al. teach a similar bioleaching process for recovering nickel from a nickel-containing laterite ore or sulfide oxide ore (abstract), comprising steps: (a) providing at least one microorganism selective to leach the ore in an aqueous solution; (b) combining the microorganism, a substrate mixture (containing sugar, a carbonaceous nutrient), the ore, a ligand (sulfuric acid H2SO4 or citric acid), and an aqueous phase to form a mixture/slurry; (c) maintaining the mixture for a period of time under conditions to dissolute/solubilize the nickel in the aqueous phase; and (d) separating (i.e. isolating) a nickel-containing aqueous solution from a solid leach residue (abstract; Examples 1 and 2: col 5/line 66 – col 6/line18, and col 6/lines 45-66). Duyvesteyn et al. further teach selectively separating and recovering nickel from the nickel-containing aqueous solution (i.e. bioleach solution), which preferably comprises: (I) extracting nickel from the bioleaching solution by a process of absorbing the nickel to a resin specifically selective to nickel absorption, which simultaneously increases nickel concentration, providing sufficient nickel for recovery by downstream electrolysis; (II) eluting the absorbed nickel from the resin by applying a mineral acid; and (III) further applying the eluted nickel solution to electrolysis (i.e. electrowinning) for recovering substantially pure nickel from the eluted nickel (col 5: lines 26-30, 56-61, and 11-12). Duyvesteyn et al. further teach, as an example, using the resin of Dow XFS 4195 and Dow XFS 43084 (col 5: lines 32-34 and 43-48). Wołowicz et al., cited as evidence, teach multiple chelating ion exchange resins and list them in table 1, which shows that Dow XFS 4195 and Dow XFS 43084 have their functional groups conjugated to polystyrene matrix, wherein the polystyrene matrix is in a form of beads (table 1; page 495, right col. Section 3.1, lines 3-4). As such, the absorption resin taught by Duyvesteyn et al. is a conjugate comprising polystyrene beads and Ni-binding functional components, as evidenced by Wołowicz et al.
Bertuol et al. teach an electrowinning process for recovering and purifying nickel and/or cobalt from an aqueous solution or a leaching solution, which contain ions of nickel and/or cobalt, wherein an assembly/circuit comprising a platinum anode and a stainless steel cathode is used for electrowinning of the aqueous/leaching solutions, and after applying electric current to the aqueous or leaching solution in the assembly, metals of nickel and/or cobalt are deposited on the cathode; wherein the deposited metals (Ni and/or Co) are recovered from the cathode for obtaining metals in good purity (abstract; Figs. 1 and 9; Section 2.2 spanning pages 2085 and 2086; page 2091/right col/lines 3-9).
Hay et al. teach that the tripeptide glycylglycyl-L-histine (i.e. Gly-Gly-His peptide, or NH2-GGH peptide) acts as a ligand, and specifically binds a nickel(II) ion or a copper(II) ion and forms a complex between the peptide and the metal ion (nickel or copper ion) (title, abstract), wherein the Gly-Gly-His peptide is commercially available (page 19, lines 3-4).
Byrd et al. teach affinity peptides having specific binding activity for metal ions (e.g. Ni2+, nickel ions) as well as a process of purifying the affinity peptides or proteins thereof through their reversible binding to metal ions on a metal chelate affinity chromatography resin/medium (abstract, paras 0033, 0029, and 0051), wherein the process comprises: contacting the peptides/proteins with the metal chelate affinity chromatography resin to allow them to bind metal ions immobilized on the resin to form a complex between the resin/metal ions and peptides/proteins, washing the complex, and eluting the bound peptides/proteins from the washed complex (para 0033, Example 2), wherein the metal chelate affinity chromatography resin is a nickel ion-bound affinity chromatography resin, and the peptides bound to the nickel ion resin comprise GGH, i.e. Gly-Gly-His (Example 2: para 0210/last 3 lines, and Table 22, see SEQ ID NOs: 97, 88, 268, 323-324, and 326-327); wherein the peptides bound to the resin are eluted from the complex by applying an eluting solution with decreased/low pH (e.g. a low pH or acidic solution) (para 0029, lines 1-2 and 5-6 from bottom). Byrd et al. further teach that the resin/matrix used for immobilizing metal ions for contacting peptides is well known in the art, for example, those in US Patent No: 6365147 (Luo et al.) (para 0070, lines 5-9). Luo et al. disclose that various absorbent matrices may be used for preparing an immobilized metal affinity chromatography matrix, such as polystyrene in the form of beads (col 2/lines 39-43, col 6/line 15). As such, Byrd et al. inherently teach a conjugate/complex comprising a polystyrene resin (bead) and a metal ion (which can be a nickel ion) bound to a peptide (which can be a peptide comprising Gly-Gly-His), as evidenced by Luo et al.
Hyeung et al. teach a fluorescence-labeled peptide that is used as a sensor for selectively binding and detecting metal ions (copper or zinc ion) in a biological sample, wherein the peptide (PG1 or PG2) comprises Gly-Gly-His and is immobilized on PEG-polystyrene resin (abstract; Experimental Example 2: page 10/paras 2-6).
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 suggested by Gunasekara et al. and Tzeferis et al. for isolating and recovering trace metals (nickel, manganese, and/or cobalt) from the aqueous phase (leach solution) obtained in step (c), by applying a Gly-Gly-His peptide comprised in a conjugate with a polystyrene bead for selectively binding nickel ions from the leach solution to form a conjugate-metal ion complex; isolating the complex and eluting the bound metal/nickel ions from the complex with an acid solution, subjecting the eluted metal ion solution to electrowinning in a circuit, and recovering nickel metal from a surface of cathode, wherein an electric current is applied through the metal ion solution during electrowinning, as taught by Duyvesteyn et al., Bertuol et al., Hay et al., Hyeung et al., and Byrd et al. A person of ordinary skill in the art would have been motivated to do so, because Gunasekara et al. teach isolating and recovering the trace metal by resin absorption and electrowinning; and Duyvesteyn et al. teach that absorbing nickel to resin increases nickel concentration, which facilitates nickel recovery by downstream electrowinning. In addition, polystyrene resin (bead) is commonly used in the art as a support, specifically for immobilizing peptides/functional components having affinity to bind metal ions (e.g. nickel ions), as supported by Duyvesteyn et al., Byrd et al. and/or Hyeung et al. Furthermore, it is well known in the art that a Gly-Gly-His peptide is an effective ligand that selectively binds nickel(II) ions, as supported by Hay et al. It is known in the art that a conjugate comprising polystyrene and a peptide having Gly-Gly-His is effective at binding metal ions, as supported by Hyeung et al. Moreover, it is well known in the art that a binding between metal ions (e.g. nickel ions) and their ligand (an affinity functional group or a Gly-Gly-His peptide) is reversible, and they are readily eluted by an acid solution (with low pH), thus allowing separation of the metal ions from peptide, and recovery of the metal ions, as supported by Duyvesteyn et al. and Byrd et al. With regard to the limitations about electrowinning in the steps (g) – (j), they are well established in the art, as supported by Bertuol et al.
One of ordinary skill in the art has a reasonable expectation of success at modifying the method suggested by Gunasekara et al. and Tzeferis et al. by applying the teachings of Duyvesteyn et al., Bertuol et al., Hay et al., Hyeung et al., and Byrd et al. for absorbing trace metal ions from leach solution by using a Gly-Gly-His peptide on PS beads and further recovering the metal by electrowinning. This is because techniques for metal ion absorption through affinity with Gly-Gly-His peptide and metal recovery through electrowinning have been well established in the art (as supported by the cited prior art), and applying them to the method suggested by Gunasekara et al. and Tzeferis et al. will allow trace metal ions (e.g. nickel ions) in leach solution effectively extracted and recovered.
Therefore, the invention as a whole would have been prima facie obvious to a person of ordinary skill in the art before the effective filing date of the claimed invention.
Claims 143-147, 149, 151-160, 162-164, 166-167, 169, and 171-172 are rejected under 35 U.S.C. 103 as being unpatentable over Gunasekara et al. (US 2024/0254591, 2024, effective filing date: May 12, 2021, of record) in view of Tzeferis et al. (Hydrometallurgy, 1994, 36(3): 345-360, the abstract is of record), Duyvesteyn et al. (US Patent No. 5626648, cited in IDS), Bertuol et al. (Chem. Eng. Technol. 2012, 35(12): 2084–2092, of record), Hay et al. (Journal of Inorganic Biochemistry, 1993, 52:17-25, of record), Hyeung et al. (KR 20090097704 A, 2009, machine-translated English version is of record), and Byrd et al. (US 2006/0030007, 2006, of record), as applied to Claims 143-147, 149, 151-160, 162-164, 166-167, 169 and 172, further in view of Pandey et al. (US 2021/0132062, published on May 6, 2021, of record), as evidenced by Lin et al. (SSRN electronical journal, 4082769, pages 1-21, published on April 13, 2022, cited in IDS), Wołowicz et al. (Chemical Engineering Journal, 2012, 197:493–508, of record), and Luo et al. (US Patent No: 6365147, 2002, of record).
The teachings of Gunasekara et al. as modified by Tzeferis et al., Duyvesteyn et al., Bertuol et al., Hay et al., Hyeung et al., and Byrd et al. are described above.
Regarding Claim 171, the modified Gunasekara does not teach the polystyrene bead comprises NH2-PEG groups. However, Hyeung et al. specifically teach the polystyrene resin (bead) immobilized with a Gly-Gly-His peptide is a polystyrene conjugated with PEG (PEG-polystyrene resin).
It would have been obvious to one of ordinary skill in the art to apply a polystyrene resin conjugated with PEG-NH2 (i.e. PEG having NH2-PEG groups) as the PEG-polystyrene bead (resin) in the modified method of Gunasekara et al. for immobilizing the Gly-Gly-His peptide, because it is well known in the art that PEG-NH2 (i.e. PEG having NH2-PEG groups) is well suited for conjugating peptides or proteins. In support, Pandey et al. teach that peptides/polypeptides can be chemically conjugated to carrier particles, and one of functional groups suited for such peptide conjugation is PEG-NH2 (para 0077, lines 1-4).
Therefore, the invention as a whole would have been prima facie obvious to a person of ordinary skill in the art before the effective filing date of the claimed invention.
Response to Arguments
Applicant's arguments about the claim objection in the response filed on 12/03/2025 (pages 9-10) have been fully considered but they are persuasive in part. Specifically, Applicant’s arguments based on correction of MtrA/MtrA/MtrC to MtrA/MtrC in claim 146 and the amendment in claim 151 are persuasive, and the objection is withdrawn. However, Applicant's arguments based about abbreviations in the claim 146 are not persuasive, because Applicant failed to provide any factual evidence to support the recited abbreviations are conventional nomenclature in the art. Furthermore, the specification of the instant application does not provide the spelled-out full names for any of the abbreviations recited in in the claim 146, which include: CymA, DFE, DmkA, DmkB, EetA, EetB, FmnA, FmnB, GACE, MtrA, MtrC, Ndh2, OmcF, OmcS, OmcZ, PplA, and T4ap. Thus, this claim objection is maintained.
Applicant's arguments about the claim rejection under 35 U.S.C. 112(b) in the 12/03/2025 response (pages 10-11) have been fully considered. Applicant’s arguments about the rejection of claims 146, 150, 157, 159, 161, and 169 are moot because the rejections have been withdrawn as indicated above. However, Applicant’s arguments about the rejection of claims 147 and 151 are not persuasive, because Applicant failed to remove all the parenthetical phrases, which are akin to “for example”, from the claim 147, and failed to provide any factual evidence to support the recited “Frateuria-like isolate WJ2” is a known bacterium whose features are well characterized in the art. Furthermore, the amendment to Claim 151 raised new issues as indicated above, thus not being sufficient to overcome the rejection.
Applicant's arguments about the rejection of claims 147 and 150 under 35 U.S.C. 112(a) in the 12/03/2025 response (page 11) have been fully considered, but they are moot because the rejections have been withdrawn as indicated above
Applicant's arguments about the rejections of Claims 143-145, 147, and/or 150-161 under 35 U.S.C. 102(a)(1) or 103 as being anticipated by or obvious over Hallberg et al. in the 12/03/2025 response (pages 12-13) have been fully considered but they are moot because the rejections have been withdrawn as indicated above.
Applicant's arguments about the rejections of Claims 143-156, 158-164, 166-167, 169, and/or 171 under 35 U.S.C. 103 over Gunasekara et al. either alone or in combination with Hallberg et al., Michelson et al., Duyvesteyn et al., Bertuol et al., Hay et al., Hyeung et al., Byrd et al. and/or Pandey et al. in the 12/03/2025 response (pages 14-15) have been fully considered but they are moot because the rejections have been withdrawn as indicated above. However, Applicant's arguments about the rejection of Claims 143-147 and 149-160 under 35 U.S.C. 103 over Gunasekara et al. in view of Tzeferis in pages 15-17 of the response are found not persuasive after Examiner’s full consideration for the following reasons.
In response to Applicant’s arguments about the teachings of Tzeferis in pages 15-16 of the response, solubilizing nickel from laterite ores by citric acid taught by Tzeferis is a leaching process, which uses the same starting material/laterite ores and produces the same products/solubilized nickel as those in the leaching process of Gunasekara et al., thus being readily combined with the leaching process of Gunasekara et al. for facilitating and improving the solubilization of nickel. With regard to Applicant’s arguments based on recovery yields of nickel in pages 15-16 of the response, Tzeferis in the abstract expressively teaches that “Citric acid proved to be the most effective organic acid for nickel extraction, achieving recoveries up to 60%” and “citric acid gave as high nickel yields as equimolar sulphuric acid under the same leaching conditions” (emphasis added), which clearly indicates that citric acid as the most effective organic achieves sufficient solubilization of nickel (up to 60%) from laterite ores, and its recovery yield is the same as sulphuric acid when equimolar sulphuric acid and same leaching conditions are used. In view of the teachings of Tzeferis, one of ordinary skill in the art would have recognized that the combination of citric acid with the leaching process of Gunasekara et al. would significantly improve recovery yield of nickel from laterite ores. With regard to Applicant’s further arguments based on choosing inorganic acid/sulphuric acid in a leaching process, Examiner notes that in contrary to Applicant’s arguments one of ordinary skill in the art would choose a safe organic acid/citric acid, rather than sulphuric acid, to improve the leaching process of Gunasekara et al., because it is well known in the art that sulphuric acid is a corrosive and toxic reagent, harmful to the environments and also expensive (which increases production costs), and it has safety issues to handle sulphuric acid during the operation. See the prior art as evidenced by Aghemio Rodriguez (US 2013/0333524, 2013), who teaches: the use of sulphuric acid as leaching agent generates a particularly harmful issue due to its high toxic and contaminating capacity; the use of sulphuric acid requires the implementation of machinery, devices, equipment, and materials particularly resistant to acid attack, thereby highly expensive, considerably increasing the production costs; and the operation risks are high and the consequences in case of accident are particularly serious for operators and workers (paras 0002/lines 5-7, and 0014/lines 1-9). Furthermore, Gunasekara et al. expressively teach performing the leaching process in their method at the neutral pH in a range of 5-9. Adding strong sulphuric acid to the system of Gunasekara et al. would dramatically reduce pH and make the pH significantly lower than the required pH range of 5-9. As such, one of ordinary skill in the art would have recognized the weak citric acid taught by Tzeferis is most suitable for improving the leaching process of Gunasekara et al. Finally in response to Applicant’s arguments based on a slow process over a leaching time of 40 days in last para of page 15, Examiner reminds Applicant that the instant claims do not recite any limitations to define a specific leaching time period or a specific reaction rate in the claimed method. It is the Examiner’s position that the recovery yields (up to 60%) of nickel from ores by using citric acid as taught by Tzeferis are sufficient for improving solubilization of nickel in the method of Gunasekara et al. Thus, it would have been obvious to further include citric acid in the method of Gunasekara et al.
Applicant's arguments about Hallberg teaches away from using an organic acid such as citric acid for extracting nickel in the 12/03/2025 response (pages 16-17) are misleading and not persuasive. Examiner reminds Applicant that the teachings of Hallberg (e.g. Fig. 6) are directed to At. Ferrooxidants, which is an iron-reducing acidophilic bacterium completely different and distinct from the Shewanellaceae bacterium used in the method of Gunasekara. As such, what At. Ferrooxidants does in the method of Hallberg is not applicable to the Shewanellaceae bacterium of Gunasekara. Thus, Hallberg does not teach away from modifying the method of Gunasekara by further including an organic acid such as citric acid in the mixture comprising Shewanellaceae bacterium for facilitating nickel extraction from laterite ores.
Overall, the conclusion of the obviousness of the amended claims 143-149, 151-164, 166-167, 169, and 171-172 has been established for all the reasons indicated above.
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 extension fee 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 date of this final action.
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Any inquiry concerning this communication or earlier communications from the examiner should be directed to Qing Xu, Ph.D., whose telephone number is (571) 272-3076. The examiner can normally be reached on Monday-Friday from 9:30 AM to 5:00 PM. If attempts to reach the examiner by telephone are unsuccessful, the examiner’s supervisor, Manjunath N. Rao, can be reached at (571) 272-0939. Any inquiry of a general nature or relating to the status of this application or proceeding should be directed to the receptionist whose telephone number is (571) 272-1600.
/Qing Xu/
Patent Examiner
Art Unit 1656
/MANJUNATH N RAO/Supervisory Patent Examiner, Art Unit 1656