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 .
Response to Arguments
With respect to the objection of Claim 6 due to minor informalities, Claim 6 has been canceled. The rejection is WITHDRAWN.
With respect to the rejection of Claims 1-16 under 35 U.S.C. 112(b), as understood traversal relies on amendments. Applicant has amended Claims 1-16 to remove all instances of the phrase “Fenton-like” and “electron-poor Cu center”. Furthermore Claim 8 has been amended to remove the phrase “a structural formula of (Bi, Cu)Al2O3”. The rejections have been WITHDRAWN.
With respect to the rejection of Claims 1-16 under 35 U.S.C. 103 as being unpatentable over Xie et al., as understood the traversal relies on amendments. Claim 1 has been amended to recite “the catalyst material is γ-Cu-Al2O3 doped with Bi12O15Cl6, wherein a mass fraction of Cu is 3.0% to 9.0%, and a mass fraction of Bi12O15Cl6 is 10.3% to 29.6%”, “a temperature of 100 °C and a rotational speed of 100 r/min to 200 r/min” (previously presented as Claim 15), and “the calcination in the muffle furnace is conducted at 400 °C to 600 °C for 3 h to 7 h with a heating rate of 5 °C/min to 10 °C/min.” (Previously Claim 16). Applicant argues “While the Xie reference teaches "the mixture was calcined in a muffle furnace at 600 °C for 6h to obtain the product (γ-Cu-Al2O3-Bi12O15Cl6)." (Xie at page 7, Experimental, section 2.2), Xie does not teach the specific limitation of a heating rate of 5°C/min to 10°C/min during the calcination step. In the Applicant's invention, the controlled heating rate of 5°C/min to 10°C/min is critical for retaining the mesoporous structure and a pore size distribution of about 7.1 nm, which directly results in superior catalytic performance is disclosed. ... A stable and low heating rate is required to ensure integrity of the final catalyst structure. If the heating rate exceeds 10°C/min, the template agent will be rapidly ablated, leading to the collapse of the internal structure. However, if the heating rate is below 5°C/min, the exterior of the template agent will be gradually carbonized, forming a dense and hard protective layer, preventing the interior from being ablated and making it difficult to form the desired catalytic material structure. See, Wang Declaration at 7-9. Thus, one ordinarily skilled in the art would not have motivation to select and control the heating rate within the claimed window because the criticality of the heating rate for achieving the desired catalyst structure and performance is not mentioned in the prior art.” [Remarks, Page 8, Paragraph 4]. It is noted that the present submission was accompanied by an Affidavit by a present inventor which can be summarized by the figure presented below [Affidavit, Page 2]:
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While Xie et al. does not disclose the heating rate during calcination they do similarly disclose a SEM image of the final product, reproduced below [Page 31, Figure 1A]:
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The SEM image presented by Xie et al. closely matches the middle image which was calcined at a heating rate of between 5-10 °C/min. No evidence of a hard outer layer nor cracking of the structure can be found which strongly suggests that the heating rate employed by Xie et al. was between 5-10 °C/min.
Further, Xie et al. explicitly discloses (In a Supplemental Data Appendix) that for at least the 0.64CAB sample the surface area is high (indicating no hard layer), the pore volume is good (indicating no collapse of structure) and the pore size is 7.1 nm, the same as in the instant application, see Figure S3 (below).
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Therefore it is understood that although Xie et al. does not explicitly disclose a heating rate between 5-10 °C/min that must have been the heating rate used because “A stable and low heating rate is required to ensure integrity of the final catalyst structure” and the final catalyst structure of Xie et al. has the integrity still intact. Furthermore it is considered within the abilities of one of ordinary skill in the art to use routine optimization when dealing with unknown variables, such as the heating rate. In other words, even absent an explicit disclosure it would have been obvious for one of ordinary skill in the art to have experimented with different heating rates, including between 5-10 °C/min until a suitable heating rate leading to desirable properties (e.g. pore size, surface area, pore volume, etc.) was found.
Applicant further argues that Claim 1 has been amended to recite “a mass fraction of Cu is 3.0% to 9.0%, and a mass fraction of Bi12O15Cl6 is 10.3% to 29.6%” and the embodiment of Xie et al. previously relied upon in the first Office Action falls outside of this range (41.2% of Bi12O15Cl6) and argues “Applicant respectfully submits that these synergistic and unexpectedly superior catalytic results are not predicted or suggested by Xie, which focuses on higher Bi content.” [Remarks, Page 10, Paragraph 6 – Page 11 Paragraph 1]. It is acknowledged that the previous embodiment is outside of the newly claimed range, however Xie et al. discloses other embodiments within the range (see, for example, “In addition, the XPS curve fittings indicate that atomic ratio of Cu (II) to Cu (I) is significantly increased from 1:1 to 1.2:1 and 1.43:1 as the Bi content increases from 0 wt% (γ-Cu-Al2O3) to 12.5 wt% (0.64CAB) and 41.2 wt% (2.64CAB), respectively.” [Xie et al., Page 30, Col. 2, Paragraph 4]). Given the embodiment (0.64CAB) that includes 12.5 wt% Bi12O15Cl6 it cannot be said that Xie et al. does not predict or suggest a mass fraction of Bi12O15Cl6 between 10.3-29.6%. Applicant further cites In re Omeprazole and argues “Applicant respectfully submits that the two-prong test of In re Omeprazole is met by (1) the inventor identifying the problem of overlooked compositional synergy and suboptimal catalytic performance and (2) adding the specific compositional range for Bi12O15Cl6 at an increased cost to solve the problem not known by a person having ordinary skill.” [Remarks, Page 12, Paragraph 1], however this is unpersuasive in light of an explicit teaching from Xie et al. of the claimed range. It cannot be said that the prior art overlooked an embodiment that was explicitly disclosed and therefore the two prong test fails prong (1).
Applicant further argues for the patentability of newly amended Claim 8 which requires “a mesoporous structure with a pore size distribution of 7.1 nm and a pore volume of 0.454 cm3/g”. Applicant argues “Xie does not teach the specific limitation of a pore size distribution of about 7.1 nm or pore volume of 0.454 cm3/g.” [Remarks, Page 9, Paragraph 5]. However, this is unpersuasive in light of Figure S3 (above) which discloses a pore size distribution of 7.117 nm and pore volume of 0.454 cm3/g for an embodiment with the required Bi12O15Cl6 wt% of Claim 1. The rejections are MAINTAINED.
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 1-5 and 8-14 are rejected under 35 U.S.C. 103 as being unpatentable over Xie et al., “Novel Fenton-like catalyst γ-Cu-Al2O3-Bi12O15Cl6 with electron-poor Cu centre and electron-rich Bi centre for enhancement of phenolic compounds degradation and H2O2 utilization: The synergistic effects of σ-Cu-ligand, dual-reaction centres and oxygen vacancies”. Claim 1 requires “A preparation method of a catalyst material, wherein the catalyst material is γ-Cu-Al2O3 doped with Bi12O15Cl6, wherein a mass fraction of Cu is 3.0% to 9.0%, and a mass fraction of Bi12O15Cl6 is 10.3% to 29.6%”. Xie et al. discloses an embodiment (0.64CAB) with 12.5 wt.% Bi12O15Cl6 “In addition, the XPS curve fittings indicate that atomic ratio of Cu (II) to Cu (I) is significantly increased from 1:1 to 1.2:1 and 1.43:1 as the Bi content increases from 0 wt% (γ-Cu-Al2O3) to 12.5 wt% (0.64CAB) and 41.2 wt% (2.64CAB), respectively.” [Xie et al., Page 30, Col. 2, Paragraph 4]). Xie et al. further discloses a copper content of 4.7% in the same sample “the decrease of Cu content from 0.64CAB (4.7%) to 2.64CAB (3.6%) is much lower than that from γ-Cu-Al2O3 (6.7%) to 0.64CAB (4.7%).” [Page 31, Paragraph 1].
Claim 1 further requires “the method comprising the following steps: step 1: dissolving bismuth nitrate pentahydrate in a nitric acid solution, and diluting a first resulting solution with deionized water to obtain a solution A”. Xie et al. discloses “Typically, 0.64 g Bismuth nitrate pentahydrate was dissolved in 5 mL nitric acid solution (2 M), and the solution was diluted to 100 mL using deionized water.” [Page 29, Section 2.2]. Claim 1 further requires “step 2: adding citric acid to solution A, and adjusting a pH of a second resulting solution with ammonia water to obtain a solution B”. Xie et al. discloses “Then 0.3 g
citric acid was dissolved in this solution with adjustment of pH to 6.5 by using ammonia.” [Page 29, Section 2.2]. Although Xie et al. does not explicitly state that the ammonia is added in an aqueous solution, one of ordinary skill in the art would know that ammonia is a gas at STP and is more conveniently added to solutions as an ammonium hydroxide solution (also referred to as ammonia water). MPEP 2144.01 (implicit and inferred teachings may be used in 35 U.S.C. 103 rejections). It would thus have been obvious to one of ordinary skill in the art before the effective filing date of the claimed invention to employ/supply Xie et al.’s ammonia as an aq. NH4OH/ammonia water solution for increased convenience and ease/safety of handling compared to gaseous NH3. MPEP 2143 I.(G).
Claim 1 further requires “step 3: dissolving aluminium isopropoxide (AIP), copper chloride dihydrate, and glucose in the solution B to obtain a suspension C”. Xie et al. discloses “8.4 g of Al(OiPr)3, 0.4 g of CuCl2·2H2O, and 7.2 g of glucose were added in solution” [Page 29, Section 2.2].
Claim 1 further requires “step 4: stirring the suspension C at a temperature of 100°C and a rotational speed of 100 r/min to 200 r/min to allow evaporation until a solid D is completely precipitated”. Xie et al. discloses “For removal of water and other volatiles, the mixture was evaporated at 100 °C with mechanical stirring.” [Page 29, Section 2.2]. While Xie et al. does not explicitly disclose the stirring speed required by Claim 6 they do explicitly disclose stirring. The speed of 100 r/min to 200 r/min is understood to be a low stirring speed which would have been obvious to one of ordinary skill in the art, given that the solution is boiling at 100 °C some speed is required to prevent ‘bumping’ of the solvent. Regarding optimization through routine experimentation MPEP 2144.05.II.A states “Generally, differences in concentration or temperature will not support the patentability of subject matter encompassed by the prior art unless there is evidence indicating such concentration or temperature is critical. "[W]here the general conditions of a claim are disclosed in the prior art, it is not inventive to discover the optimum or workable ranges by routine experimentation." In re Aller, 220 F.2d 454, 456 (CCPA 1955) (Claimed process which was performed at a temperature between 40°C and 80°C and an acid concentration between 25% and 70% was held to be prima facie obvious over a reference process which differed from the claims only in that the reference process was performed at a temperature of 100°C and an acid concentration of 10%.)”. Similarly differences in the stirring speed during a reaction are obvious unless the stirring speed is critical to the invention. Therefore, in the instant application the conclusion of obviousness is further supported by a lack of teaching in the specification or the Affidavit submitted on 12/25/2025 that the stirring speed is critical to the invention, i.e. that speeds below 100 rpm or above 200 rpm would have failed to produce a catalyst with the claimed properties.
Claim 1 further requires “step 5: subjecting the solid D to calcination in a muffle furnace to obtain the catalyst material, wherein the calcination in the muffle furnace is conducted at 400 °C to 600 °C for 3 h to 7 h with a heating rate of 5 °C/min to 10 °C/min.”. Xie et al. discloses “Then the mixture was calcined in a muffle furnace at 600 °C for 6 h to obtain the product” [Page 29, Section 2.2]. The only feature of Claim 7 not explicitly disclosed by Xie et al. is the heating rate of the furnace, however this would have been obvious to one of ordinary skill in the art because a heating ramp of 5-10 °C is typical of calcinations. Furthermore it is understood that the heating rate used by Xie et al. must have been within the range of 5 °C/min to 10 °C/min. In the Remarks submitted 12/25/2025 Applicant attests that “In the Applicant's invention, the controlled heating rate of 5°C/min to 10°C/min is critical for retaining the mesoporous structure and a pore size distribution of about 7.1 nm” [Remarks, Page 8, Paragraph 4]. Given that Xie et al. discloses a catalyst with a mesoporous structure with a pore size of about 7.1 nm (see Claim 8, below) they therefore must have controlled the heating rate to between 5 °C/min to 10 °C/min. Further evidence for the heating rate of Xie et al. falling within the range claimed can be found in the Affidavit submitted on 12/25/2025 which contains SEM images of catalysts of the claimed composition calcined at different rates (see below). The only SEM that matches the SEM images of Xie et al. are those samples which were calcined at a rate of between 5 °C/min to 10 °C/min.
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Claim 2 requires “in step 1, the nitric acid solution has a concentration of 1 mol/L to 2 mol/L, and a ratio of the bismuth nitrate pentahydrate to the nitric acid solution is (0.64-1.28) g: 5 mL.”. Xie et al. discloses 2 mol/ nitric acid and 0.64 g of bismuth nitrate pentahydrate per 5 mL of nitric acid “Typically, 0.64 g Bismuth nitrate pentahydrate was dissolved in 5 mL nitric acid solution (2 M)” [Page 29, Section 2.2].
Claim 3 requires “wherein a ratio of the citric acid to the bismuth nitrate pentahydrate is (0.3-0.9) g : (0.64- 1.28) g.”. Xie et al discloses 0.64 g of bismuth nitrate pentahydrate to 0.3 g of citric acid (see Claim 1) which is within the range claimed.
Claim 4 requires “in step 2, the pH of the second resulting solution is adjusted with the ammonia water to 5 to 9.”. Xie et al. discloses adjusting to pH 6.5 “adjustment of pH to 6.5 by using ammonia.” [Page 29, Section 2.2].
Claim 5 requires “in step 3, the AIP, the copper chloride dihydrate, and the glucose are added in a ratio of (6.0-9.0) g : (0.1-0.8) g : (4.0-8.0) g.”. Xie et al. discloses “8.4 g of Al(OiPr)3, 0.4 g of CuCl2·2H2O, and 7.2 g of glucose were added in solution” [Page 29, Section 2.2], which is a ratio of 8.4:0.4:7.2.
Claim 8 requires “wherein the catalyst material has a mesoporous structure with a pore size distribution of 7.1 nm and a pore volume of 0.454 cm3/g.”. Xie et al. discloses a pore size distribution of 7.1 nm and a pore volume of 0.454 cm3/g for sample 0.64CAB in the supplemental data appendix, see figure S3 below:
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This appendix is considered to intrinsically be part of the disclosure of Xie et al.
Claim 9 requires “the catalyst material is provided in combination with H2O2 in water to degrade an organic pollutant.”. Xie et al. discloses “The catalytic activities of catalysts were evaluated by degradation of phenolic compounds (BPA, 2-Chlorophenol) and non-phenolic compound (Rh B). Typically, 100 mL aqueous solutions with certain organic and catalyst were mixed in 150 mL beaker flasks. After magnetically stirred for 30 min, 8 mM H2O2 was added in” [Page 30, Section 2.4, Paragraph 1]. BPA, 2-Chlorophenol, and Rh B are organic pollutants.
Claim 10 requires “the organic pollutant is any one selected from the group consisting of rhodamine B, bisphenol A (BPA), and dichlorophenol (DCP).”. Xie et al. discloses “The catalytic activities of catalysts were evaluated by degradation of phenolic compounds (BPA, 2-Chlorophenol) and non-phenolic compound (Rh B).” [Page 30, Section 2.4, Paragraph 1].
Claim 11 requires “in step 1, the nitric acid solution has a concentration of 1 mol/L to 2 mol/L, and a ratio of the bismuth nitrate pentahydrate to the nitric acid solution is (0.64-1.28) g: 5 mL.”. Xie et al. discloses 2 mol/ nitric acid and 0.64 g of bismuth nitrate pentahydrate per 5 mL of nitric acid “Typically, 0.64 g Bismuth nitrate pentahydrate was dissolved in 5 mL nitric acid solution (2 M)” [Page 29, Section 2.2].
Claim 12 requires “a ratio of the citric acid to the bismuth nitrate pentahydrate is (0.3-0.9) g : (0.64-1.28) g.”. Xie et al discloses 0.64 g of bismuth nitrate pentahydrate to 0.3 g of citric acid (see Claim 1) which is within the range claimed.
Claim 13 requires “in step 2, the pH of the second resulting solution is adjusted with the ammonia water to 5 to 9.”. Xie et al. discloses adjusting to pH 6.5 “adjustment of pH to 6.5 by using ammonia.” [Page 29, Section 2.2]. For the obviousness of substituting ammonia with ammonia water see Claim 1.
Claim 14 requires “in step 3, the AIP, the copper chloride dihydrate, and the glucose are added in a ratio of (6.0-9.0) g : (0.1-0.8) g : (4.0-8.0) g.”. Xie et al. discloses “8.4 g of Al(OiPr)3, 0.4 g of CuCl2·2H2O, and 7.2 g of glucose were added in solution” [Page 29, Section 2.2], which is a ratio of 8.4:0.4:7.2.
Conclusion
Applicant's amendment necessitated the new ground(s) of rejection presented in this Office action. Accordingly, THIS ACTION IS MADE FINAL. See MPEP § 706.07(a). Applicant is reminded of the extension of time policy as set forth in 37 CFR 1.136(a). A shortened statutory period for reply to this final action is set to expire THREE MONTHS from the mailing date of this action. In the event a first reply is filed within TWO MONTHS of the mailing date of this final action and the advisory action is not mailed until after the end of the THREE-MONTH shortened statutory period, then the shortened statutory period will expire on the date the advisory action is mailed, and any nonprovisional extension fee (37 CFR 1.17(a)) pursuant to 37 CFR 1.136(a) will be calculated from the mailing date of the advisory action. In no event, however, will the statutory period for reply expire later than SIX MONTHS from the mailing date of this final action.
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/JOSHUA MAXWELL SPEER/
Examiner
Art Unit 1736
/DANIEL BERNS/Primary Examiner, Art Unit 1736
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