Notice of Pre-AIA or AIA Status
The present application, filed on or after March 16, 2013, is being examined under the first inventor to file provisions of the AIA .
Priority
Applicant’s claim for the benefit of a prior-filed application (has PRO 62/930,133, filed on 04 November 2019, is 371 of PCT/US2020/058513, filed on 02 November 2020) under 35 U.S.C. 119(e) or under 35 U.S.C. 120, 121, 365(c), or 386(c) is acknowledged.
Claim Rejections - 35 USC § 112
The following is a quotation of 35 U.S.C. 112(b):
(b) CONCLUSION. —The specification shall conclude with one or more claims particularly pointing out and distinctly claiming the subject matter which the inventor or a joint inventor regards as the invention.
Claim 29 and 30 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 29 recites the limitation “percent increase in lead exchange capacity in water of about 15% to about 150% compared to titanosilicate-based adsorbent materials.” This defines the invention by reference to an undefined comparison standard. The Specification does not identify what constitutes the baseline “titanosilicate-based adsorbent material,” and its performance can vary based on composition, porosity, and testing conditions. Without a defined benchmark, a person of ordinary skill in the art cannot determine the scope of the claim with reasonable certainty.
Claim 30 recites the limitation “percent increase in cadmium exchange capacity in water of about 50% to about 500% compared to titanosilicate-based adsorbent materials.” This also relies on an undefined external standard. The Specification fails to provide a specific baseline for comparison, and the cadmium exchange performance of titanosilicate materials can differ widely depending on formulation and conditions. As a result, the scope of the claim cannot be determined with reasonable certainty.
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 text of those sections of Title 35, U.S. Code not included in this action can be found in a prior Office action.
The factual inquiries for establishing a background for determining obviousness under 35 U.S.C. 103 are summarized as follows:
Determining the scope and contents of the prior art.
Ascertaining the differences between the prior art and the claims at issue.
Resolving the level of ordinary skill in the pertinent art.
Considering objective evidence present in the application indicating obviousness or nonobviousness.
This application currently names joint inventors. In considering patentability of the claims the examiner presumes that the subject matter of the various claims was commonly owned as of the effective filing date of the claimed invention(s) absent any evidence to the contrary. Applicant is advised of the obligation under 37 CFR 1.56 to point out the inventor and effective filing dates of each claim that was not commonly owned as of the effective filing date of the later invention in order for the examiner to consider the applicability of 35 U.S.C. 102(b)(2)(C) for any potential 35 U.S.C. 102(a)(2) prior art against the later invention.
Claims 1, 5, 9-10, 12, 14, 17, 19, and 29-30 are rejected under 35 U.S.C. 103 as being unpatentable over KAWASAKI et al. (US20060163151A1, hereinafter KAWASKAI) in view of BROWN et al. (US4493902, hereinafter BROWN) and SHIMADA et al (“Determination of external surface composition of zeolite particles by synchrotron radiation XPS” 1996, hereinafter SHIMADA).
Regarding Claim 1, KAWASAKI discloses a composite adsorbent for water purification (¶[0001]). Desirable particulate compounds for the composite adsorbent include titanosilicate-based and aluminosilicate-based inorganic compounds, such as zeolite, selected for their high ion-exchange capacity and selectivity toward heavy metals (¶¶[0028]–[0029]).
In Example 1, a titanosilicate-based particulate (ATS) is mixed with polyethylene powder to form a particulate compound, which is then heated, crushed, and sieved to a 30/150 mesh size to produce a composite powder. The composite powder is then blended with particulate activated carbon (i.e., granular adsorbent material) to make a composite adsorbent, which is packed into a column and tested for removal of soluble lead from water (¶¶[0050]–[0054]).
However, KAWASAKI does not explicitly disclose (1) about 20% to about 60% by weight of a crystalline phase comprising Y-zeolite, (2) about 5% to about 95% by weight of a non-zeolitic matrix phase based on the total weight of the silicate composition, (3) an interconnected porous scaffold having a total mercury pore volume of about 0.005 to about 0.25 cc/g for pores of about 20 to 10,000 Å and about 0.10 to about 0.25 cc/g for pores of about 200 to 10,000 Å, (4) a total nitrogen pore volume of about 0.02 to about 0.10 cc/g for pores of about 20 to 600 Å, and (5) a surface area of about 200 to about 500 m²/g.
BROWN discloses a zeolite-based matrix in the form of microspheres containing more than 40% by weight of a crystalline phase comprising Y-faujasite zeolite dispersed within a non-zeolitic phase (Col. 1, Lns. 8–15). The microspheres are formed as single, integrated particles in which both the crystalline zeolite and non-zeolitic phases are co-located (Col. 1, Lns. 40–49). The disclosed weight percentage of Y-zeolite falls within the claimed range of about 20% to about 60%, and the remainder corresponds to a non-zeolitic matrix within the claimed range of about 5% to about 95%.
The pore volumes of 20–100 Å pores were measured by nitrogen adsorption using a multi-gas analyzer (Col. 7, Lns. 15–24). Mercury intrusion porosimetry was used to measure the pore volumes of 100–600 Å and 600–20,000 Å pores. Pore diameters were calculated using the Washburn equation, assuming a contact angle of 140° and a surface tension of 484 ergs/cm² (Col. 7, Lns. 25–41). The microspheres had 0.02 cc/g of pores having diameters in the range of 20–100 Å, 0.07 cc/g of pores in the range of 100–600 Å, and 0.12 cc/g of pores in the range of 600–20,000 Å, yielding a total porosity of 0.20 cc/g. The measured surface area was 430 m²/g, and the bulk density of the 200/270 mesh fraction was 1.16 g/cc (Col. 32, Lns. 8–14). This surface area falls within the claimed range of about 200 to about 500 m²/g. The measured surface area is within the claimed range, the disclosed nitrogen pore volume also falls within the claimed range, and the mercury pore volumes are within and partially overlap the corresponding claimed ranges.
The microspheres contain Y-faujasite in the sodium form and are subjected to ion exchange with ammonium or rare earth cations to replace sodium, yielding microspheres with reduced bulk Na₂O and increased REO, followed by a drying step (Col. 11, Lns. 49–61).
A person having ordinary skill in the art would recognize the significance of BROWN’s Y-zeolite matrix as a highly active microspherical composition suitable for blending with other functional components to tailor selectivity, activity, and other material characteristics depending on system needs (Col. 15, Lns. 49–57). In doing so, a person having ordinary skill in the art would understand that BROWN provides structural details missing from KAWASAKI, particularly with respect to the composition and form of the zeolite-containing matrix. Therefore, it would have been obvious to a person having ordinary skill in the art, prior to the effective filing date of the claimed invention, to incorporate the Y-zeolite-containing microsphere matrix, disclosed by BROWN, into the water-purification composite sorbent by KAWASAKI.
While modified KAWASAKI reports sodium content in terms of bulk Na₂O weight percentage, a person having ordinary skill in the art would understand that sodium cations can remain present in the microspheres after ion exchange and drying. However, modified KAWASAKI does not disclose the distribution of sodium within the microspheres or quantify the sodium content at the external surface.
SHIMADA discloses that non-destructive depth profiling analysis with high surface sensitivity was performed by XPS with synchrotron radiation excitation, revealing a thin Al- and Na-rich overlayer at the external surface of NaY particles (abstract). In §2 Experimental, XPS spectra were measured using synchrotron radiation at BL-13C of the Photon Factory, employing a spherical grating monochromator coupled to a hemispherical electrostatic analyzer operated at 25 eV pass energy. The zeolites analyzed were NaY and HY fine powders, with the HY sample prepared by triple ion exchange followed by calcination at 400 °C. Sodium was measured using Na 2s spectral lines, and surface charging was minimized by sonicating the powders onto stainless steel sample plates (pg. 125, Col. 2).
A person having ordinary skill in the art would have recognized that the ability to measure external surface composition by X-ray photoelectron spectroscopy (XPS), as demonstrated in SHIMADA, provides a practical analytical method for characterizing the distribution of sodium at the external surface of ion-exchanged zeolite particles. While modified KAWASAKI reduces bulk sodium content through ion exchange, it does not disclose any surface composition. Based on SHIMADA, a skilled artisan would have understood that the surface sodium content of the ion-exchanged product could be evaluated using XPS, and subsequently optimized through adjustment of ion exchange and calcination conditions (KSR Int’l Co. v. Teleflex Inc., 550 U.S. 398).
Therefore, it would have been obvious to a person having ordinary skill in the art, prior to the effective filing date of the claimed invention, to combine SHIMADA’s surface-composition measurement method with the ion exchange and calcination process applied to the water-purification sorbent by modified KAWASAKI.
Based on the combined disclosures, selecting ion exchange and calcination conditions to achieve a surface sodium level between about 5 and 20 atomic percent would have constituted routine experimentation (In re Aller, 220 F.2d 454, 456–57; 1955).
Regarding Claim 2, modified KAWASAKI makes obvious a composite adsorbent of Claim 1. KAWASAKI discloses the use of an aluminosilicate-based inorganic compound such as X-type zeolite ([¶0029]).
Regarding Claim 5, modified KAWASAKI makes obvious a composite adsorbent of Claim 1. BROWN discloses pore measurements in the 20–100 Å range by nitrogen and in the 35–20,000 Å range by mercury (Col. 7, Lns. 15–41). Accordingly, the nitrogen-measured pores fall within the microporous range, while the mercury-measured pores span mesoporous to macroporous sizes.
Regarding Claim 9, modified KAWASAKI makes obvious a composite adsorbent of Claim 1. BROWN discloses that the silicate composition has a particle size in the 200/270 mesh fraction (Col. 32, Lns. 3–7), corresponding to about 53 to 74 microns, and this falls within the claimed range of about 40 to about 150 microns.
Regarding Claim 10, modified KAWASAKI makes obvious a composite adsorbent of Claim 1. BROWN discloses that the crystalline Y-faujasite zeolite phase is formed in situ within microspheres derived from a mixture of metakaolin and kaolin clay that has been calcined at least substantially through its characteristic exotherm (Col. 3, Lns. 3–10).
Regarding Claim 12, modified KAWASAKI makes obvious a composite adsorbent of Claim 10. BROWN discloses that the crystalline Y-faujasite zeolite phase is formed in situ within microspheres derived from a mixture of metakaolin and kaolin clay that has been calcined at least substantially through its characteristic exotherm (Col. 3, Lns. 3–10). Given that modified KAWASAKI incorporates the same Y-zeolite-containing composite formed from both metakaolin and kaolin clay, it would have been obvious to a person having ordinary skill in the art to adjust the metakaolin content to about 30% to about 60% by weight and the kaolin content to about 40% to about 70% by weight through routine optimization (In re Aller, 220 F.2d 454, 456–57; 1955).
Regarding Claim 14, modified KAWASAKI makes obvious a composite adsorbent of Claim 1. KAWASAKI discloses that a titanosilicate-based adsorbent material (ATS) is blended with polyethylene powder and particulate activated carbon to form a composite adsorbent structure ([¶0065]).
Regarding Claim 17, modified KAWASAKI makes obvious a composite adsorbent of Claim 1. BROWN discloses adding sodium silicate to the aqueous slurry before spray drying, where it functions as a binder between the clay particles (Col. 8, Lns. 26–39).
Regarding Claims 29 and 30, modified KAWASAKI makes obvious a composite sorbent material of Claim 1. KAWASAKI discloses that titanosilicate- and aluminosilicate-based inorganic compounds are desirable particulate materials for sorbent applications due to their large ion-exchange capacity and high selectivity toward heavy metals (¶[0028]).
The claimed exchange capacities for lead (Claim 29) and cadmium (Claim 30) are result-effective variables that carry no patentable weight in the absence of structural distinction. Modified KAWASAKI discloses a zeolite-containing silicate composition formed into a porous sorbent. Without evidence of structural differences, the claimed performance is presumed to be an inherent property of the prior-art material (In re Best, 562 F.2d 1252, 1255 (CCPA 1977); MPEP §2112).
Claim 19 is rejected under 35 U.S.C. 103 as being unpatentable over KAWASAKI in view of BROWN and SHIMADA as applied to claim 17 above, and further in view of BOUVIER et al. (US20180214848A1, hereinafter BOUVIER).
Regarding Claim 19, modified KAWASAKI makes obvious a composite adsorbent of Claim 17. However, modified KAWASAKI does not disclose a pore-forming agent comprising starch, lignosulfonates, cellulose-based materials, synthetic polymers, or combinations thereof.
BOUVIER discloses a mesoporous zeolite adsorbent (¶[0001]). Agglomeration and shaping is carried out using zeolite and binder by methods such as extrusion, compacting, or granulation. During this process, organic additives such as lignin, starch, carboxymethylcellulose, methylcellulose and its derivatives, lignosulfonates, and polycarboxylic acid-based compounds may be included to modify the pulp properties and enhance macroporosity in the final agglomerates (¶¶[0088]–[0089]).
A person having ordinary skill in the art would recognize the significance of BOUVIER’s disclosure that organic additives such as starch, methylcellulose, and lignosulfonates are added during agglomeration to modify rheology and enhance pore development during thermal processing (¶¶[0089], [0092]). The additives are included to improve handling during shaping and to give the final agglomerates desirable properties, particularly macroporosity.
Therefore, it would have been obvious to a person having ordinary skill in the art, prior to the effective filing date of the claimed invention, to incorporate a pore-forming agent, as disclosed by BOUVIER, into the agglomeration and shaping process that produces the composite adsorbent by modified KAWASAKI.
Claims 23 and 24 are rejected under 35 U.S.C. 103 as being unpatentable over KAWASAKI in view of BROWN.
Regarding Claims 23 and 24, KAWASAKI discloses a composite adsorbent for water purification (¶[0001]). Desirable particulate compounds for the composite adsorbent include titanosilicate-based and aluminosilicate-based inorganic compounds, such as zeolite, selected for their high ion-exchange capacity and selectivity toward heavy metals (¶¶[0028]–[0029]).
In Example 1, a titanosilicate-based particulate (ATS) is mixed with polyethylene powder to form a particulate compound, which is then heated, crushed, and sieved to a 30/150 mesh size to produce a composite powder. The composite powder is then blended with particulate activated carbon (i.e., granular adsorbent material) to make a composite adsorbent, which is packed into a column and tested for removal of soluble lead from water (¶¶[0050]–[0054]).
However, KAWASAKI does not explicitly disclose (1) about 20% to about 60% by weight of a crystalline phase comprising Y-zeolite, (2) about 5% to about 95% by weight of a non-zeolitic matrix phase based on the total weight of the silicate composition, (3) an interconnected porous scaffold having a total mercury pore volume of about 0.005 to about 0.25 cc/g for pores of about 20 to 10,000 Å and about 0.10 to about 0.25 cc/g for pores of about 200 to 10,000 Å, (4) a total nitrogen pore volume of about 0.02 to about 0.10 cc/g for pores of about 20 to 600 Å, and (5) a surface area of about 200 to about 500 m²/g.
BROWN discloses a zeolite-based matrix in the form of microspheres containing more than 40% by weight of a crystalline phase comprising Y-faujasite zeolite dispersed within a non-zeolitic phase (Col. 1, Lns. 8–15). The microspheres are formed as single, integrated particles in which both the crystalline zeolite and non-zeolitic phases are co-located (Col. 1, Lns. 40–49). The disclosed weight percentage of Y-zeolite falls within the claimed range of about 20% to about 60%, and the remainder corresponds to a non-zeolitic matrix within the claimed range of about 5% to about 95%.
The pore volumes of 20–100 Å pores were measured by nitrogen adsorption using a multi-gas analyzer (Col. 7, Lns. 15–24). Mercury intrusion porosimetry was used to measure the pore volumes of 100–600 Å and 600–20,000 Å pores. Pore diameters were calculated using the Washburn equation, assuming a contact angle of 140° and a surface tension of 484 ergs/cm² (Col. 7, Lns. 25–41). The microspheres had 0.02 cc/g of pores having diameters in the range of 20–100 Å, 0.07 cc/g of pores in the range of 100–600 Å, and 0.12 cc/g of pores in the range of 600–20,000 Å, yielding a total porosity of 0.20 cc/g. The measured surface area was 430 m²/g, and the bulk density of the 200/270 mesh fraction was 1.16 g/cc (Col. 32, Lns. 8–14). The disclosed nitrogen pore volume reads upon the claimed range, while the mercury pore volumes are within and overlap with the corresponding claimed ranges.
A person having ordinary skill in the art would recognize the significance of BROWN’s Y-zeolite matrix as a highly active microspherical composition suitable for blending with other functional components to tailor selectivity, activity, and other material characteristics depending on system needs (Col. 15, Lns. 49–57). In doing so, a person having ordinary skill in the art would understand that BROWN provides structural details missing from KAWASAKI, particularly with respect to the composition and form of the zeolite-containing matrix.
Therefore, it would have been obvious to a person having ordinary skill in the art, prior to the effective filing date of the claimed invention, to incorporate the Y-zeolite-containing microsphere matrix, disclosed by BROWN, into the water-purification composite sorbent by KAWASAKI.
Response to Arguments
Applicant’s arguments, see Remarks filed July 16, 2025, with respect to the rejections of claims 1–5, 7–10, 12, 14, 17, 19, 23–24, and 29–30 under 35 U.S.C. §§ 102/103 have been fully considered and are persuasive. Therefore, the rejection has been withdrawn. However, upon further consideration, new grounds of rejection are made under 35 U.S.C. § 103 in view of KAWASAKI et al., BROWN et al., SHIMADA et al., and BOUVIER et al.
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.
Any inquiry concerning this communication or earlier communications from the examiner should be directed to TAK L. CHIU whose telephone number is (703)756-1059. The examiner can normally be reached M-F: 9:00am - 6:00pm (CST).
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/TAK L CHIU/Examiner, Art Unit 1777
/KRISHNAN S MENON/Primary Examiner, Art Unit 1777