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
Acknowledgment is made of applicant’s claim for foreign priority (EP19193114.6, filed on 22 August 2019) under 35 U.S.C. 119 (a)-(d). Receipt is acknowledged of certified copies of papers required by 37 CFR 1.55.
Claim Rejections - 35 USC § 103
In the event the determination of the status of the application as subject to AIA 35 U.S.C. 102 and 103 (or as subject to pre-AIA 35 U.S.C. 102 and 103) is incorrect, any correction of the statutory basis (i.e., changing from AIA to pre-AIA ) for the rejection will not be considered a new ground of rejection if the prior art relied upon, and the rationale supporting the rejection, would be the same under either status.
The following is a quotation of 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.
Claims 13-19, 22, 25, 27, 33 and 34 are rejected under 35 U.S.C. 103 as being unpatentable over LOCKWOOD et al (US20060000780A1, hereinafter LOCKWOOD) in view of RODRÍGUEZ-IZNAGA et al. (Ammonium modified natural clinoptilolite to remove manganese, cobalt and nickel ions from wastewater, 2017, hereinafter RODRÍGUEZ-IZNAGA) and SELVAM et al. (Histamine-binding capacities of different natural zeolites: a comparative study, 2018, hereinafter SELVAM).
Regarding Claim 13, LOCKWOOD discloses solid and liquid ion-exchange materials for removing heavy metals or radionuclides from aqueous or gaseous solutions (¶[0002]). Industrial wastewater is identified as a typical medium containing heavy metal cations, such as mercury, lead, zinc, copper, antimony, chromium, and nickel, which may originate from smelting, electroplating, and chemical manufacturing processes (¶[0003], ¶[0011]). In Example 1, a slurry comprising NaOH solution and naturally occurring clinoptilolite was treated under heat and agitation, then filtered to produce a modified clinoptilolite solid (S200) (¶[0036]). Examples 2, 3, and 5 demonstrate the use of S200 or S200L in removing lead, zinc, and copper from aqueous solutions, each achieving 99.9% reduction of heavy metals in the treated liquid (¶¶[0037]–[0038], [0040]).
However, LOCKWOOD does not disclose a modified clinoptilolite zeolite (1) having an Si/Al ratio greater than 4:1, (2) at least 70% of the exchangeable cations replaced by ammonium, and (3) a D50 from 0.1 µm to 20 µm and a D98 from 0.15 µm to 1500 µm.
RODRÍGUEZ-IZNAGA discloses the removal of manganese, cobalt, and nickel from industrial wastewaters using natural clinoptilolite modified to its ammonium form (Abstract, Pg. 200). The zeolite sample contains 85% clinoptilolite with impurities including mordenite, quartz, montmorillonite, and feldspar, and is referred to as CLI. The particle size of the material is reported as +0.25 mm to 0.5 mm (§2 Experimental, Pg. 201), which corresponds to 250 µm to 500 µm and falls within the claimed “weight top cut particle size D98 from 0.15 µm to 1500 µm.”
The elemental oxide composition of the purified sample is reported as 63.2 wt.% SiO₂ and 10.13 wt.% Al₂O₃ (§2, Pg. 201). Based on molecular weights of 60.08 g/mol for SiO₂ and 101.96 g/mol for Al₂O₃, this corresponds to approximately 1.052 mol of Si and 0.1987 mol of Al per 100 g of material, resulting in a molar Si/Al ratio of approximately 5.29:1 which is greater than the claimed “Si/Al ratio of greater than 4:1.”
In the preparation of ammonium-modified clinoptilolite (NH₄-CLI), CLI samples were treated with 0.15 mol/L NH₄Cl solution under agitation at 25 °C, 80 °C, and 100 °C, using a ratio of 1 g of CLI to 20 mL of solution. The liquid and solid phases were separated over time, and the concentrations of Na⁺, Ca²⁺, K⁺, and Mg²⁺ were measured in the supernatant using atomic absorption spectrometry, while NH₄⁺ was determined using the Nessler reagent (§2.1 Preparation of ammonium-clinoptilolite form, Pg. 201).
Based on the reported oxide composition (§2) and cation concentrations (§2.1), the total exchangeable cation content is estimated to be approximately 322 meq per 100 g of material. Displacement of Na⁺, K⁺, Ca²⁺, and Mg²⁺ under the disclosed exchange conditions results in an estimated 264.5 meq per 100 g replaced by ammonium. Based on the total cation content inferred from the reported oxide composition, this corresponds to an exchange level of approximately 82% if Fe³⁺ is included, and 93% if Fe³⁺ is excluded, both of which exceed the claimed threshold that “at least 70% of the exchangeable cations in the modified heulandite group zeolite are replaced by ammonium cations.”
Advantageously, the NH₄-CLI disclosed by RODRÍGUEZ-IZNAGA can be efficiently produced under mild ion-exchange conditions due to the low activation energy for NH₄⁺ intracrystalline exchange, while preserving the clinoptilolite framework as shown by XRD and IR analysis (§3.1, Pg. 203, Table 1; Pg. 205). NH₄-CLI also removes Mn²⁺ and Co²⁺ at room temperature and provides enhanced Ni²⁺ removal at elevated temperature in column studies (§3.2, Pgs. 206–207). In view of LOCKWOOD’s modified clinoptilolite material for heavy-metal removal, a person skilled in the art would have incorporated the ammonium-modified clinoptilolite to provide an ion-exchange material having ammonium cations in the exchange sites and predictable heavy-metal cation removal.
Regarding the claimed “weight median particle size D50 from 0.1 µm to 20 µm,” this limitation is considered a result-effective variable for particulate adsorption and ion-exchange materials, as the median particle size affects contact between the particulate material and the liquid medium. RODRÍGUEZ-IZNAGA discloses a raw material particle size, and grinding or classifying zeolite material to obtain a desired particle-size distribution is a well-known practice in the field. It would have been obvious to a person skilled in the art to optimize the clinoptilolite particle-size distribution to a smaller D50, including the claimed range, because the adjusted median particle size would predictably provide a greater fraction of finer zeolite particles for ion-exchange contact.
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 apply the ammonium-modified clinoptilolite material and process disclosed by RODRÍGUEZ-IZNAGA, in the heavy metal removal method for a liquid medium by LOCKWOOD.
However, modified LOCKWOOD does not explicitly disclose that the “particulate mineral material of step b) has a specific surface area of from 5 m²/g to 200 m²/g, measured using nitrogen sorption and the BET method.”
SELVAM discloses a comparative study of Cuban and Mexican zeolites, focusing on how particle size and mineral composition affect adsorption. The Cuban zeolite contains clinoptilolite and mordenite, while the Mexican sample contains only clinoptilolite. The Cuban zeolite’s higher adsorption capacity was attributed to higher BET surface area and pore volume influenced by large-pore mordenite (Abstract).
The Cuban zeolite samples had particle-size classes of about 3 µm and 40 µm and were processed by conventional mechanical grinding and used as received, without additional micronization or chemical treatment (§ Materials, Pgs. 2658–2659). BET surface area and total pore volume were measured using nitrogen adsorption at 77 K after pre-treatment at 250 °C for 12 hours (§ Characterization, Pg. 2659). Table 3 reports BET surface areas of 98 and 119 m²/g for the Cuban zeolite samples, with total pore volumes of 0.199 to 0.220 cc/g (§ N₂-sorption, Pg. 2661), and the reported BET surface areas fall within the claimed “specific surface area of from 5 m²/g to 200 m²/g.”
A person skilled in the art would recognize that specific surface area is a key structural parameter for adsorption materials. SELVAM reports BET surface areas for Cuban clinoptilolite-containing zeolite, attributable to its microstructure and mordenite content. This fills the structural data gap left by RODRÍGUEZ-IZNAGA and supports use of Cuban clinoptilolite-containing zeolite having the reported BET surface area in the method of LOCKWOOD.
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 rely on the BET surface area data for Cuban clinoptilolite-containing zeolite, as disclosed by SELVAM, when characterizing the ammonium-modified clinoptilolite material in the heavy metal removal process for a liquid medium by modified LOCKWOOD.
Regarding Claim 14, modified LOCKWOOD makes obvious the method for removing heavy metal cations from a liquid medium of Claim 13. RODRÍGUEZ-IZNAGA discloses preparing NH₄-CLI by treating natural Cuban clinoptilolite with aqueous ammonium chloride solution to exchange the native cations with NH₄⁺ (§§2.1–2.3, Pg. 201). The calculated oxide composition corresponds to an estimated Si/Al molar ratio of approximately 5.29:1, and the disclosed ion-exchange conditions correspond to an estimated NH₄⁺ replacement level of approximately 82% to 93%.
Regarding Claims 15–17, modified LOCKWOOD makes obvious the method for removing heavy metal cations from a liquid medium of Claim 14. RODRÍGUEZ-IZNAGA discloses preparation of NH₄-CLI by treating CLI samples with a 0.15 mol/L NH₄Cl solution at a ratio of 1 g CLI per 20 mL solution (§2.1, Pg. 201). This treatment involves the use of ammonium chloride (Claim 15), corresponds to approximately 4.67 wt% ammonium cations based on the weight of the particulate mineral material (see previous Office Action), which falls within the claimed range of 0.05 wt% to 20 wt% (Claim 16), and provides an ammonium cation concentration within the claimed range of 0.001 mol/L to 20 mol/L (Claim 17).
Regarding Claim 18, modified LOCKWOOD makes obvious the method for removing heavy metal cations from a liquid medium of Claim 13. RODRÍGUEZ-IZNAGA discloses preparing Ni-CLI, Mn-CLI, and Co-CLI by treating CLI with corresponding heavy-metal chloride solutions, followed by separating the heavy metal-loaded solid by filtration and washing with distilled water (§2.3, Pg. 202).
Regarding Claim 19, modified LOCKWOOD makes obvious the method for removing heavy metal cations from a liquid medium of Claim 13. RODRÍGUEZ-IZNAGA discloses that experiments were conducted in a tubular column containing NH₄-CLI for the removal of Mn²⁺, Co²⁺, and Ni²⁺ from aqueous solutions. Mixed solutions of NiCl₂, MnCl₂, and CoCl₂ were passed through the column at a controlled flow rate, with eluate samples collected over time for analysis (§2.2, Pg. 201).
Regarding Claim 22, modified LOCKWOOD makes obvious the method for removing heavy metal cations from a liquid medium of Claim 14. Based on the reported oxide composition (§2) and cation concentrations (§2.1) from RODRÍGUEZ-IZNAGA, the total exchangeable cation replacement level is approximately 93% when Fe³⁺ is excluded. RODRÍGUEZ-IZNAGA studies NH₄⁺ exchange conditions including temperature and exchange behavior, and higher NH₄⁺ replacement would provide more ammonium exchange sites for subsequent heavy-metal cation exchange. It would have been obvious to a person having ordinary skill in the art to adjust process variables such as temperature, concentration, or duration to further increase the degree of cation exchange and achieve at least 95% replacement with predictable results (In re Aller, 220 F.2d 454, 456–57 (CCPA 1955)).
Regarding Claim 25, modified LOCKWOOD makes obvious a method for removing heavy metal cations from a liquid medium of Claim 13. RODRÍGUEZ-IZNAGA discloses that the clinoptilolite samples treated with metal chloride solutions were thoroughly washed with distilled water until Cl⁻ anions were completely removed, then oven-dried and stored in a desiccator (§2.3, Pgs. 201–202). These steps reasonably indicate removal of chloride residues from the clinoptilolite surface.
Regarding Claim 27, modified LOCKWOOD makes obvious the method for removing heavy metal cations from a liquid medium of Claim 13. LOCKWOOD discloses the treatment of industrial wastewater containing mercury, lead, zinc, and copper, which are included in the claimed group of cadmium, copper, lead, mercury, zinc, and mixtures thereof (¶[0003], ¶[0011]).
Regarding Claim 33, LOCKWOOD discloses solid and liquid ion-exchange materials for removing heavy metals or radionuclides from aqueous or gaseous solutions (¶[0002]). Industrial wastewater is identified as a typical medium containing heavy metal cations, such as mercury, lead, zinc, copper, antimony, chromium, and nickel, which may originate from smelting, electroplating, and chemical manufacturing processes (¶[0003], ¶[0011]). In Example 1, a slurry comprising NaOH solution and naturally occurring clinoptilolite was treated under heat and agitation, then filtered to produce a modified clinoptilolite solid (S200) (¶[0036]). Examples 2, 3, and 5 demonstrate the use of S200 or S200L in removing lead, zinc, and copper from aqueous solutions, each achieving 99.9% reduction of heavy metals in the treated liquid (¶¶[0037]–[0038], [0040]).
However, LOCKWOOD does not disclose a modified clinoptilolite zeolite (1) having an Si/Al ratio greater than 4:1, (2) at least 70% of the exchangeable cations replaced by ammonium, (3) a D50 from 0.05 µm to 500 µm and a D98 from 0.15 µm to 1500 µm, and (4) prepared using a water-soluble ammonium salt in an amount so that the ammonium cations are from 0.5 wt% to 4 wt% based on the total weight of the particulate mineral material.
RODRÍGUEZ-IZNAGA discloses the removal of manganese, cobalt, and nickel from industrial wastewaters using natural clinoptilolite modified to its ammonium form (Abstract, Pg. 200). The zeolite sample contains 85% clinoptilolite with impurities including mordenite, quartz, montmorillonite, and feldspar, and is referred to as CLI. The particle size of the material is reported as +0.25 mm to 0.5 mm (§2 Experimental, Pg. 201), which corresponds to 250 µm to 500 µm, overlaps the claimed “weight median particle size D50 from 0.05 µm to 500 µm,” and falls within the claimed “weight top cut particle size D98 from 0.15 µm to 1500 µm.”
The elemental oxide composition of the purified sample is reported as 63.2 wt.% SiO₂ and 10.13 wt.% Al₂O₃ (§2, Pg. 201). Based on molecular weights of 60.08 g/mol for SiO₂ and 101.96 g/mol for Al₂O₃, this corresponds to approximately 1.052 mol of Si and 0.1987 mol of Al per 100 g of material, resulting in a molar Si/Al ratio of approximately 5.29:1 which is greater than the claimed “Si/Al ratio of greater than 4:1.”
In the preparation of ammonium-modified clinoptilolite (NH₄-CLI), CLI samples were treated with 0.15 mol/L NH₄Cl solution under agitation at 25 °C, 80 °C, and 100 °C, using a ratio of 1 g of CLI to 20 mL of solution. The liquid and solid phases were separated over time, and the concentrations of Na⁺, Ca²⁺, K⁺, and Mg²⁺ were measured in the supernatant using atomic absorption spectrometry, while NH₄⁺ was determined using the Nessler reagent (§2.1 Preparation of ammonium-clinoptilolite form, Pg. 201).
Based on the reported oxide composition (§2) and cation concentrations (§2.1), the total exchangeable cation content is estimated to be approximately 322 meq per 100 g of material. Displacement of Na⁺, K⁺, Ca²⁺, and Mg²⁺ under the disclosed exchange conditions results in an estimated 264.5 meq per 100 g replaced by ammonium. Based on the total cation content inferred from the reported oxide composition, this corresponds to an exchange level of approximately 82% if Fe³⁺ is included, and 93% if Fe³⁺ is excluded, both of which exceed the claimed threshold that “at least 70% of the exchangeable cations in the modified heulandite group zeolite are replaced by ammonium cations.”
Advantageously, the NH₄-CLI disclosed by RODRÍGUEZ-IZNAGA can be efficiently produced under mild ion-exchange conditions due to the low activation energy for NH₄⁺ intracrystalline exchange, while preserving the clinoptilolite framework as shown by XRD and IR analysis (§3.1, Pg. 203, Table 1; Pg. 205). NH₄-CLI also removes Mn²⁺ and Co²⁺ at room temperature and provides enhanced Ni²⁺ removal at elevated temperature in column studies (§3.2, Pgs. 206–207). In view of LOCKWOOD’s modified clinoptilolite material for heavy-metal removal, a person skilled in the art would have incorporated the ammonium-modified clinoptilolite to provide an ion-exchange material having ammonium cations in the exchange sites and predictable heavy-metal cation removal.
Regarding the claimed ammonium cation amount of 0.5 wt.-% to 4 wt.-%, this limitation is considered a result-effective variable for ammonium ion-exchange treatment, as the ammonium cation amount controls the NH₄⁺ available for exchange with native clinoptilolite cations. RODRÍGUEZ-IZNAGA studies NH₄⁺ ion-exchange under different treatment conditions, including treatment at 25 °C, 80 °C, and 100 °C, using 0.15 mol/L NH₄Cl solution and 1 g CLI per 20 mL solution (§2.1, Pg. 201). Based on those treatment conditions, the NH₄Cl treatment provides approximately 4.67 wt% ammonium cations based on the weight of the particulate mineral material. It would have been obvious to a person skilled in the art to optimize the ammonium cation amount within the claimed 0.5 wt.-% to 4 wt.-% range based on the ion-exchange treatment conditions, since the adjusted amount would predictably maintain NH₄⁺ availability for exchange with native clinoptilolite cations.
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 apply the ammonium-modified clinoptilolite material and process disclosed by RODRÍGUEZ-IZNAGA, in the heavy metal removal method for a liquid medium by LOCKWOOD.
However, modified LOCKWOOD does not explicitly disclose that the “particulate mineral material of step b) has a specific surface area of from 5 m²/g to 200 m²/g, measured using nitrogen sorption and the BET method.”
SELVAM discloses a comparative study of Cuban and Mexican zeolites, focusing on how particle size and mineral composition affect adsorption. The Cuban zeolite contains clinoptilolite and mordenite, while the Mexican sample contains only clinoptilolite. The Cuban zeolite’s higher adsorption capacity was attributed to higher BET surface area and pore volume influenced by large-pore mordenite (Abstract).
The Cuban zeolite samples had particle-size classes of about 3 µm and 40 µm and were processed by conventional mechanical grinding and used as received, without additional micronization or chemical treatment (§ Materials, Pgs. 2658–2659). BET surface area and total pore volume were measured using nitrogen adsorption at 77 K after pre-treatment at 250 °C for 12 hours (§ Characterization, Pg. 2659). Table 3 reports BET surface areas of 98 and 119 m²/g for the Cuban zeolite samples, with total pore volumes of 0.199 to 0.220 cc/g (§ N₂-sorption, Pg. 2661), and the reported BET surface areas fall within the claimed “specific surface area of from 5 m²/g to 200 m²/g.”
A person skilled in the art would recognize that specific surface area is a key structural parameter for adsorption materials. SELVAM reports BET surface areas for Cuban clinoptilolite-containing zeolite, attributable to its microstructure and mordenite content. This fills the structural data gap left by RODRÍGUEZ-IZNAGA and supports use of Cuban clinoptilolite-containing zeolite having the reported BET surface area in the method of LOCKWOOD.
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 rely on the BET surface area data for Cuban clinoptilolite-containing zeolite, as disclosed by SELVAM, when characterizing the ammonium-modified clinoptilolite material in the heavy metal removal process for a liquid medium by modified LOCKWOOD.
Regarding Claim 34, modified LOCKWOOD makes obvious the method for removing heavy metal cations from a liquid medium of Claim 33.
Regarding the claimed “weight median particle size D50 from 0.1 µm to 20 µm,” this limitation is considered a result-effective variable for particulate adsorption and ion-exchange materials, as the median particle size affects contact between the particulate material and the liquid medium. RODRÍGUEZ-IZNAGA discloses a raw material particle size, and grinding or classifying zeolite material to obtain a desired particle-size distribution is a well-known practice in the field. It would have been obvious to a person skilled in the art to optimize the clinoptilolite particle-size distribution to a smaller D50, including the claimed range, because the adjusted median particle size would predictably provide a greater fraction of finer zeolite particles for ion-exchange contact.
Response to Arguments
Applicant’s arguments, see Remarks filed January 12, 2026, have been fully considered but are not persuasive. The rejection of Claims 13–19, 22, 25, and 27 under 35 U.S.C. § 103 is updated and maintained. New Claims 33 and 34 are rejected under 35 U.S.C. § 103.
Applicant’s argument identifies a numerical difference between RODRÍGUEZ-IZNAGA’s reported particle size and the amended D50 range, but the numerical difference alone does not establish patentability. Particle-size distribution is an optimizable parameter for particulate adsorption and ion-exchange materials because it affects handling, packing, contact between the particulate material and the liquid medium, and access to ion-exchange sites. RODRÍGUEZ-IZNAGA’s reported particle size appears to be the starting clinoptilolite material and already falls within the claimed D98 range. As set forth in the rejection, grinding or classifying zeolite material to obtain a desired particle-size distribution is a well-known practice, and selecting a smaller D50 would predictably provide a greater fraction of finer zeolite particles for ion-exchange contact.
Applicant has not submitted evidence showing that the amended D50 range is critical or produces unexpected heavy-metal removal performance. To the extent removal performance is considered, the instant Specification reports metal-dependent results, with high removal for Hg but substantially lower removal for Cu and Zn. LOCKWOOD already reports high liquid-phase heavy-metal removal using modified clinoptilolite, including 99.9% removal of lead, zinc, and copper. Thus, the present record does not show that selecting the amended D50 range produces a removal result different from, or unexpected over, the known heavy-metal removal performance of modified clinoptilolite materials.
To the extent Applicant relies on mercury-removal performance discussed during prosecution or shown in the Specification, the showing is not commensurate with the full scope of the claims, which recite multiple heavy metal cations and mixtures thereof. LOCKWOOD identifies mercury as a relevant heavy-metal contaminant and provides comparative liquid-phase removal data for modified clinoptilolite against other heavy metals. Where the prior art discloses substantially similar modified clinoptilolite materials for heavy-metal removal, Applicant bears the burden to show that the asserted removal property would not reasonably be expected from the prior art material (In re Best, 562 F.2d 1252 (CCPA 1977)).
Applicant’s argument that SELVAM does not cure the deficiencies of RODRÍGUEZ-IZNAGA is not persuasive. SELVAM is not relied upon for the ammonium-modification chemistry or the heavy-metal removal step. Rather, SELVAM is relied upon for the BET surface-area characterization of Cuban clinoptilolite-containing zeolite, including reported BET surface areas that fall within the claimed 5 m²/g to 200 m²/g range. LOCKWOOD and RODRÍGUEZ-IZNAGA provide the heavy-metal-removal and ammonium-modified clinoptilolite teachings, while SELVAM supplies the specific surface-area data for the zeolite material.
Conclusion
THIS ACTION IS MADE FINAL. 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
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