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 .
Continued Examination Under 37 CFR 1.114
A request for continued examination under 37 CFR 1.114, including the fee set forth in 37 CFR 1.17(e), was filed in this application after final rejection. Since this application is eligible for continued examination under 37 CFR 1.114, and the fee set forth in 37 CFR 1.17(e) has been timely paid, the finality of the previous Office action has been withdrawn pursuant to 37 CFR 1.114. Applicant's submission filed on 4/20/2026 has been entered.
Response to Arguments
With respect to the rejection of Claims 1-5, 7, and 17-20 under 35 U.S.C. 112(b)/2nd par. as being indefinite for containing the phrase “a binderless adsorbent”, as understood the traversal relies on amendments. Claims 1-5, 7, 17-18 and 20 have been amended to remove the phrase “binderless” and Claim 19 has been canceled. The rejections are WITHDRAWN.
With respect to the rejection of Claim 2 under 35 U.S.C. 112(b)/2nd par. as being indefinite for containing the phrase “a pore diffusivity (Dp), based on nitrogen pore diffusivity”, as understood the traversal relies on amendments. Claim 2 has been amended to remove the phrase “a pore diffusivity (Dp), based on nitrogen pore diffusivity”. The rejection has been WITHDRAWN.
With respect to the rejection of Claims 1-5, 7, and 17-19 are rejected under 35 U.S.C. 102(a)(1) as anticipated by or, in the alternative, under 35 U.S.C. 103 as obvious over US 2019 0388871 A1 Ortiz et al., as understood the traversal relies on amendments. Claim 1 has been amended to recite “Li13X comprises … with a ratio of silica to alumina greater than 2.3 to about 2.6” and “LiLSX comprises … with a ratio of silica to alumina less than 2.3”. Applicant argues “Applicant asserts that the disclosure of Ortiz, et al. actually teaches away from the presence of 13X zeolite in their disclosed and claimed adsorbent particle.” [Remarks, Page 10, Paragraph 6] and concludes “Accordingly, Ortiz, et al. only discloses a single zeolitic component in the claimed adsorbent: LSX zeolite crystals with an Si/Al atomic ratio in a range from 1.00 to 1.15. Thus, throughout the Application, the composition of the claimed adsorbent material in Ortiz, et al. is only LSX zeolite crystals with the stated Si/Al atomic ratio.” [Remarks, Page 11, Paragraph 7]. This is unpersuasive. First, assertions of the prior art teaching away from the claimed invention are inapplicable to anticipation rejections. MPEP 2131.05. Second, it is understood that the applicant argues that Ortiz et al. teaches away from zeolite 13X by merely being silent towards its inclusion. This is not the test for teaching away. MPEP 2123.II states “Furthermore, "[t]he prior art’s mere disclosure of more than one alternative does not constitute a teaching away from any of these alternatives because such disclosure does not criticize, discredit, or otherwise discourage the solution claimed…." In re Fulton, 391 F.3d 1195, 1201, 73 USPQ2d 1141, 1146 (Fed. Cir. 2004).” Applicant does not argue that Ortiz et al. criticizes, discredits, or otherwise discourages one of ordinary skill in the art from including 13X zeolites. Furthermore as pointed out in the previous Office Action the rejection is based on the inherent formation of zeolite 13X and not its intentional inclusion (“How is one expected to claim a feature they are unaware exists within their disclosure?”) [Office Action dated 9/30/25, Page 6, Paragraph 2].
Applicant further argues that the disclosure that the absorbent material of Ortiz et al. is “based on LSX zeolites” would convey that the material of Ortiz et al. contains exclusively LSX zeolites [Remarks, Page 11]. This is unpersuasive. Ortiz et al. explicitly discloses “The amount by weight of LXS zeolite crystals is generally comprised in a range from 75% to 90% by weight” [0040], i.e. other materials are present, such as the disclosed binder which is converted into zeolites (“the amount of zeolitisable clay is generally comprised in a range from 5% to 25% by weight relative to the total weight of said product obtained” [0040] and “it is easy to obtain zeolitisation of at least 50%, and preferably at least 70%, more preferably at least 80% and even more preferably at least 85%, by weight of the zeolitisable clay or clays present in the binder.” [0050]). Therefore one of ordinary skill in the art would only assume that Ortiz et al. contains exclusively LSX zeolites if the process of zeolitisation formed exclusively LSX zeolites which is not taught by Ortiz et al. Also, asserting that Ortiz et al. exclusively contains LSX zeolites by stating that the reference’s absorbent material is “based on LSX zeolites” is not reasonable; “based on” does not reasonably connote exclusivity.
Applicant further argues “The Examiner acknowledged that zeolite crystals with the stated Si/Al atomic ratio [1.00-1.15] cannot be 13X zeolites.” [Remarks, Page 11, Paragraph 2]. Applicant does not provide a citation and the Examiner is unsure to what passage they are referring to. The presented rejection under 35 U.S.C. 102(a)(1) and/or 35 U.S.C. 103 did not assert that 13X zeolites cannot have any particular Si/Al ratio.
Applicant further argues “For a claim limitation to be "inherent", it must necessarily be present in the disclosure of the cited art, and an ordinary skilled artisan must be able to recognize it. (MPEP 2112(ii)).” [Remarks, Page 12, Paragraph 3]. This is unpersuasive. MPEP 2112.II actually states “There is no requirement that a person of ordinary skill in the art would have recognized the inherent disclosure at the relevant time, but only that the subject matter is in fact inherent in the prior art reference.” (underlining added, citations omitted for brevity).
Applicant further argues “What a person skilled in the art would understand from reviewing Ortiz, et al. is that the only zeolitic material that should be present in the adsorbent material is "LSX zeolite crystals with a Si/Al atomic ratio of 1.00 to 1.15."” [Remarks, Page 13, Paragraph 2]. This is unpersuasive as Ortiz et al. explicitly discloses less than 100% LSX zeolite and material which zeolitized without teaching that the result of said zeolitisation process is LSX zeolite (see above).
Applicant further argues “The claims of the Application are product claims, not process claims. Applicant asserts that the process utilized by Applicant to create its adsorbent material is not necessarily the same as that of Ortiz, et al., as the Applicant is not required to include each and every process step in its Application … It is common, in fact generally utilized, for applicants not to disclose each and every step in a process and maintain those undisclosed process steps as trade secrets.” [Remarks, Page 13, Paragraph 4; italics added]. This is unpersuasive. First it is noted that Applicant is unable to point to any specific process step which is different between the instant invention as disclosed and Ortiz et al. It is therefore assumed that there is none. As such, note that it has been held that where claimed and prior art products are produced by identical or substantially similar methods, a prima facie case of anticipation or obviousness has been established. MPEP 2112.01, citing In re Best, 562 F.2d 1252, 1255 (CCPA 1977). In other words, if the prior art teaches or at least suggests a claim’s positive method steps, it matters not whether the prior art also teaches or suggests the features of the intended result of performing said steps- it would not be reasonable to expect different results when performing identical or at least substantially similar steps. Accord, MPEP 2145 II, citing, e.g., In re Baxter Travenol Labs., 952 F.2d 388, 392 (Fed. Cir. 1991) (stating that “Mere recognition of latent properties in the prior art does not render nonobvious an otherwise known invention”). See also In re Woodruff, 919 F.2d 1575, 1578 (Fed. Cir. 1990) (stating the “general rule that merely discovering and claiming a new benefit of an old process cannot render the [old] process again patentable”) (emphasis in original).
Dovetailing with the foregoing analysis, the instant application contains withdrawn process claims (see Claim 6 and 9-10) for forming zeolite 13X from the clay binder. Ortiz et al. discloses the same procedure for zeolitisation of the clay binder as claimed in the instant invention. To assert that there remains unclaimed features which are necessary to the formation of zeolite 13X is akin to asserting that Claim 6 fails to enable one of ordinary skill in the art to make and use the claimed invention and therefore all withdrawn process steps would be rejectable under 35 U.S.C. 112(a)/1st par. Applicant’s own above-detailed admission that certain steps were withheld from the specification is taken as an admission that the affected claims are not enabled thereby and thus fail the enablement requirement of 35 U.S.C. 112(a)/1st par.
Applicant further argues “Even if the presence of a 13X zeolite is "inherent", which Applicant strongly contests, Ortiz et al. do not provide any information as to the percentage of 13X zeolite that should be present in the adsorbent material” [Remarks, Page 14, Paragraph 2]. This is unpersuasive. In the previous Office Action the Examiner asserted Ortiz et al. discloses that between 2.5-21.25% of the composition is zeolites which were converted to zeolites from clay binder which overlapped with the claimed range of 5-20% of zeolite 13X. Applicant does not point out any deficiencies in this argument (other than what has been discussed above regarding inherency) and therefore the analysis is presumed correct.
Applicant further argues “In addition, the adsorbent material that is claimed in Claim 1 of the Application is required to have a particular bulk density. Note from the examples attached that the bulk density that is claimed is not disclosed by any of the other examples, including the one that is similar to that of Ortiz, et al.” [Remarks, Page 14, Paragraph 4 – Page 15, Paragraph 1]. This is unsupported by the facts. The comparative example C-6 (which the Examiner has previously pointed out deficiencies of) has a bulk density of 677, while Claim 1 requires a bulk density of ≥640.
Claim Rejections - 35 USC § 112
The following is a quotation of the first paragraph of 35 U.S.C. 112(a):
(a) IN GENERAL.—The specification shall contain a written description of the invention, and of the manner and process of making and using it, in such full, clear, concise, and exact terms as to enable any person skilled in the art to which it pertains, or with which it is most nearly connected, to make and use the same, and shall set forth the best mode contemplated by the inventor or joint inventor of carrying out the invention.
The following is a quotation of the first paragraph of pre-AIA 35 U.S.C. 112:
The specification shall contain a written description of the invention, and of the manner and process of making and using it, in such full, clear, concise, and exact terms as to enable any person skilled in the art to which it pertains, or with which it is most nearly connected, to make and use the same, and shall set forth the best mode contemplated by the inventor of carrying out his invention.
Claims 1-5, 7, 17-18, and 20 rejected under 35 U.S.C. 112(a) or 35 U.S.C. 112 (pre-AIA ), first paragraph, because the best mode contemplated by the inventor or a joint inventor, or for applications subject to pre-AIA 35 U.S.C. 112, the inventor(s) has not been disclosed. Evidence of concealment of the best mode is based upon Remarks filled on 4/20/2026 Applicant argues that one of ordinary skill in art following the synthesis as described in the specification would be unable to make the zeolite 13X required by Claim 1 and 17 (and dependent Claims 2-5, 7, 18, and 20) without the knowledge of additional undisclosed “trade secrets” [Remarks dated 4/20/2026, Page 13, Paragraph 4 – Page 14, Paragraph 1]. Therefore it is understood that the disclosure omits process steps which lead to the formation of zeolite 13X, as required by Claims 1-5, 7, 17-18, and 20, and as such does disclose the best mode for practicing the invention. MPEP 2165 states “Determining compliance with the best mode requirement requires a two-prong inquiry. First, it must be determined whether, at the time the application was filed, the inventor possessed a best mode for practicing the invention. This is a subjective inquiry which focuses on the inventor’s state of mind at the time of filing. Second, if the inventor did possess a best mode, it must be determined whether the written description disclosed the best mode such that a person skilled in the art could practice it.”. Regarding Prong 1 Applicant admittance that trade secrets were know to the inventors which synthesized the necessary product satisfies Prong 1. Regarding Prong 2 Applicants own admittance that these steps were intentionally withheld satisfies Prong 2.
Claims 1-5, 7, 17-18, and 20 are rejected under 35 U.S.C. 112(a) or 35 U.S.C. 112 (pre-AIA ), first paragraph, as failing to comply with the enablement requirement. The claim(s) contains subject matter which was not described in the specification in such a way as to enable one skilled in the art to which it pertains, or with which it is most nearly connected, to make and/or use the invention. In the response filled on 4/20/2026 Applicant argues that one of ordinary skill in art following the synthesis as described in the specification would be unable to make the zeolite 13X required by Claim 1 and 17 (and dependent Claims 2-5, 7, 18, and 20) without the knowledge of additional undisclosed “trade secrets” [Remarks dated 4/20/2026, Page 13, Paragraph 4 – Page 14, Paragraph 1].
In order to determine compliance with the enablement requirement of 35 U.S.C. 112(a), the Federal Circuit developed a framework of factors in In re Wands, 858 F.2d 731, 737, 8 USPQ2d 1400, 1404 (Fed. Cir. 1988), referred to as the Wands factors to assess whether any necessary experimentation required by the specification is "reasonable" or is "undue.". Wands factors appear below:
(A) The breadth of the claims;
(B) The nature of the invention;
(C) The state of the prior art;
(D) The level of one of ordinary skill;
(E) The level of predictability in the art;
(F) The amount of direction provided by the inventor;
(G) The existence of working examples; and
(H) The quantity of experimentation needed to make or use the invention based on the content of the disclosure.
Regarding factor (A) the claims are drawn to a composition of matter comprising three different specific components (“a blend of a lithium exchanged zeolite 13X (Li13X), a lithium exchanged low silica X zeolite (LiLSX), and halloysite clay”) all components must be within a range of wt.% of the total mixture (ranges are between 5-15 wt.% wide). However Claim 1 and 17 use the open ended claim language “comprising” rather than the closed ended language “consisting of” which allows other components to be present, which broadens the claims.
Regarding factor (B) the nature of the invention is a zeolitic material for absorbing particular gasses. Zeolite materials in general are known in the art as high surface area materials that are capable of adsorbing gasses and lithium exchanged zeolites (similar to those required by Claims 1 and 17) are known to be applicable to the separation of O2 from atmospheric air, see at least US 3,140,933 Mckee et al. at Col. 3, Table 1 (Lithium exchanged zeolite X has the highest separation factor for an O2/N2 mixture).
Regarding factor (C) and (D), the prior art recognizes the utility of zeolites, in particular lithium exchanged zeolites, for the intended use of the invention. Regarding the zeolitization of clay binders this is also known. Cited prior art US 2019 0388871 A1 Ortiz et al. serves as an example (see Claim 1 and 17 below). However, as noted in the rejection, while Ortiz et al. recognizes that clay binder can be converted into zeolites by treatment with sodium hydroxide they do not disclose the type of zeolite formed.
Similarly DE 102018109701 A1 Reitmeier et al. discloses zeolitization of metakaolin (“subsequent zeolitization of the metakaolin, according to steps a) to c)” [0117]) into the faujasite type zeolite (“The zeoliation in step b) is carried out in such a way that at least 50 wt%, preferably at least 80 wt% of the binder used is converted into a faujasite type zeolite.” [0024]). Additionally, US 20200055019 A1 Reitmeier discloses “These other zeolite particles are obtained by transformation of suitable clay minerals such as kaolin, kaolinite or metakaolin by means of zeolitization in a hydrothermal reaction. Here, the support material containing zeolite and clay mineral and optionally additives such as a silicon source is thermally treated in an alkaline solution, with the aqueous alkaline solution optionally also containing one or more silicon sources and/or aluminium sources which are required for converting the clay mineral into a faujasite structure having an atomic Si/Al ratio in the required range” [0030], which further teaches alkaline zeolitization of kaolin type clays to faujasite type zeolites. Additionally Reitmeier teaches that optional additives such as a Si and/or Al source will change the Si/Al ratio of the zeolitized binder. However listed examples do not include any experiments that included any optional additional silica/alumina sources and therefore one of ordinary skill in the art would not be able to determine the specific additive and the amount required to achieve any particular Si/Al ratio without doing their own experimentation.
Similarly US 20100196213 A1 Lutz et al. discloses “The agglomerates derived from step 3/ are then optionally subjected to a treatment in an alkaline basic aqueous solution (step 4/): this treatment may be performed for example by hot maceration in a solution of an alkali metal or alkaline-earth metal hydroxide, preferably in a sodium hydroxide solution or in a mixture of sodium hydroxide or potassium hydroxide, whose concentration is preferably greater than 0.5 M, as described in international application WO 1999/05063. Following such a treatment, and in particular when the binder is based on kaolin(s), kaolinite(s), nacrite(s), dickite(s), halloysite(s), and/or metakaolin(s), there is obtained the at least partial conversion of the inert binder in terms of adsorption to an active material in terms of adsorption.” [0081-0082]. Lutz et al. characterizes the formed zeolites by particle size, density, and crush strength (see Example 1-11) but does not disclose how varying the clay binder and other process conditions affects the type of zeolite formed. Regarding the level of one of ordinary skill in the art it is understood that one skilled in the art of zeolite synthesis would be able to perform any and all of the synthesizes listed above, even in the absence of a specific example (such as prophetic examples).
Regarding factor (E), the prior art provides a few examples of specific clays being converted into specific types of zeolites (see Reitmeier et al. above) but generally does not provide examples wherein the alkalinity, temperature, time, and inclusion of optional additives repeatably generate specific zeolites which differ by crystal structure and/or Si:Al ratios.
In conclusion it is well known in the art that clay binders can be converted to zeolites under the conditions disclosed by the instant application (sodium hydroxide and elevated temperature), however the art lacks specific teaching of what types of zeolites are formed by what reaction conditions and the prior art lacks a specific example of zeolite 13X being formed by the zeolitization process.
Regarding factor (F), the amount of direction provided by the inventor, the specification discloses a synthesis “A low silica zeolite X (2.0 silica/alumina ratio) is mixed with a halloysite clay in a ratio of about 85/15 zeolite to clay. This mixture is then formed into spheres and calcined. These calcined particles are then introduced to a hot (~90C) sodium hydroxide solution for several hours to convert the clay into 13X zeolite. The particles are then washed with water to remove excess caustic, and then the particles undergo a lithium ion exchange to at least about 95%.” [0040]. It is noted that the concentration of sodium hydroxide is not disclosed and the temperature and time are approximate. In the first Office Action (dated 5/23/2025) this was considered adequate for disclosing a method of forming 13X zeolite.
However in the Remarks (dated 4/20/2026) Applicant argues “Applicant asserts that the process utilized by Applicant to create its adsorbent material is not necessarily the same as that of Ortiz, et al., as the Applicant is not required to include each and every process step in its Application.” [Page 13, Paragraph 4]. It is noted that the rejection had pointed out that Ortiz et al. discloses a mixture of zeolite X and halloysite clay at temperatures between 80-100 °C. As the disclosed process steps are either similar or the exact same it is therefore understood that had one of ordinary skill in the art performed the synthesis as disclosed by the present invention zeolite 13X would not have necessarily been formed due to omitted process steps that are required for the formation of zeolite 13X not being performed. Applicant further explicitly admits that they did not disclose the process steps necessary “It is common, in fact generally utilized, for applicants not to disclose each and every step in a process and maintain those undisclosed process steps as trade secrets. … Thus, there can be no assertion that a process, which is not disclosed to the people skilled in the art, is the same as that of Ortiz et al.” [Page 14, Paragraph 1, emphasis added].
Regarding factor (G), the instant invention specification provides a single working example of a successful synthesis of zeolite 13X from halloysite clay, however as the Applicant has argued that a similar process as disclosed would not be sufficient to have formed zeolite 13X without additional trade secrets (see above) it cannot be said that this working example provides enough guidance to one of ordinary skill in the art to have realized the synthesis of zeolite 13X.
Regarding factor (H), there is no difference between the synthesis as described by the prior art and as disclosed by the instant invention. The inclusion of one or more additives (which may take multiple forms), with their own concentration, and including any number of additional process steps in order to discover the trade secrets necessary leads to an infinite number of potential experiments that may be required, as the person of ordinary skill in the art is not constrained to picking from a finite list. This is considered undue burden.
In conclusion the general process of converting clay binders into zeolite with a base such as sodium hydroxide is well known in the art. The art has shown many examples of clays to be used and possible zeolites that are formed, however it is not clear that one of ordinary skill in the art could make any zeolite from any clay without some degree of experimentation. The instant application synthesis was assumed to be enabling before the Applicant attested that they did not fully disclose every step required to have formed zeolite 13X from halloysite clay. The prior art does not explicitly teach a process which results in halloysite clay being transformed into zeolite 13X and therefore one of ordinary skill in the art would not have necessarily been able to practice the invention as claimed without undue experimentation to discover the concealed trade secrets.
The following is a quotation of 35 U.S.C. 112(b):
(b) CONCLUSION.—The specification shall conclude with one or more claims particularly pointing out and distinctly claiming the subject matter which the inventor or a joint inventor regards as the invention.
The following is a quotation of 35 U.S.C. 112 (pre-AIA ), second paragraph:
The specification shall conclude with one or more claims particularly pointing out and distinctly claiming the subject matter which the applicant regards as his invention.
Claims 1-5, 7, 17-18, and 20 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 1 and 17 recites “a ratio of silica to alumina greater than 2.3 to about 2.6” and “a ratio of silica to alumina less than 2.3”. This is indefinite because it is not clear if the ratios recited are based on a molar ratio or a mass ratio (or another less common ratio). The specification fails to cure this deficiency. For the purpose of this Office Action Claim 1 is interpreted as requiring a molar ratio of silica to alumina to be within the claimed ranges.
Additionally the phrase “a ratio of silica to alumina greater than 2.3 to about 2.6” presents multiple ranges (greater than 2.3 and greater than about 2.6) making it unclear which range actually limits the claim. For the purpose of this Office Action Claim 1 is given the broadest reasonable interpretation of a ratio of silica to alumina greater than 2.3.
Claims 2-5, 7, 18, and 20 are dependent on either Claim 1 or 17 and fail to cure the deficiencies noted above and are therefore similarly rejected.
Claim Rejections - 35 USC § 102/103
The following is a quotation of the appropriate paragraphs of 35 U.S.C. 102 that form the basis for the rejections under this section made in this Office action:
A person shall be entitled to a patent unless –
(a)(1) the claimed invention was patented, described in a printed publication, or in public use, on sale, or otherwise available to the public before the effective filing date of the claimed invention.
(a)(2) the claimed invention was described in a patent issued under section 151, or in an application for patent published or deemed published under section 122(b), in which the patent or application, as the case may be, names another inventor and was effectively filed before the effective filing date of the claimed invention.
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.
Claim(s) 1-5, 7, and 17-18 is/are rejected under 35 U.S.C. 102(a)(1) as anticipated by or, in the alternative, under 35 U.S.C. 103 as obvious over US 2019 0388871 A1 Ortiz et al. Principles of inherency are applied below. The rejection is made under 102/103 per the practice in MPEP 2112 III. Claim 1 requires “An adsorbent for separation of a gaseous stream”. Ortiz et al. discloses a product containing only zeolites and clay “The amount by weight of LXS zeolite crystals is generally comprised in a range from 75% to 90% by weight relative to the total weight of said product obtained at the end of step a/, and the amount of zeolitisable clay is generally comprised in a range from 5% to 25% by weight relative to the total weight of said product obtained at the end of step a/.” [0040].
Claim 1 further requires “comprising a blend of a lithium exchanged zeolite 13X (Li13X), a lithium exchanged low silica X zeolite (LiLSX), and halloysite clay”. Regarding the lithium exchange Ortiz et al. discloses “In the present application, “exchangeable sites” refers to all of the exchangeable sites in the LSX zeolite crystals and also the exchangeable sides formed during zeolitisation of the binder. In a preferred embodiment of the invention, the lithium exchange is carried out” [0052]. Regarding zeolite 13X Ortiz et al. does not explicitly disclose 13X zeolites, however this is believed to be inherently formed due to the zeolitization of the binder. The rationale to support the inherency is that the steps performed on the halloysite clay to transform it into 13X zeolite taken in the instant application are the same as the steps taken by Ortiz et al. to transform halloysite clay into zeolites, and therefore the expected zeolite formed is zeolite 13X. Specifically, in the instant application “The process of caustically digesting the halloysite clay material occurs at a temperature of about 80°C utilizing a caustic solution. In one embodiment the caustic solution contains primarily sodium hydroxide and potassium hydroxide. In a further embodiment the caustic solution is substantially sodium hydroxide.” [0031] and “There is no limitation on the exact method of contact of the blended product with the caustic solution.” [0032]. In Ortiz et al. “Zeolitisation can be carried out by immersing the agglomerate in an alkaline basic solution, generally an aqueous solution, for example an aqueous solution of sodium hydroxide and/or potassium hydroxide, … , typically at temperatures on the order of 80° C. to 100° C.” [0049]. Regarding low silica X zeolite Ortiz et al. discloses “It has now been found that it is possible to produce high-capacity zeolitic adsorbent materials, from LSX zeolite crystals, containing lithium” [0013]. Regarding halloysite clay Ortiz et al. discloses “The zeolitisable clays which can be used in the context of the present invention typically belong to the class of the kaolinites, halloysites, nacrites, dickites, kaolins and/or metakaolins” [0045].
Claim 1 further requires “wherein the Li13X comprises from about 5 to about 20% of the adsorbent”. Ortiz et al. discloses “the amount of zeolitisable clay is generally comprised in a range from 5% to 25% by weight relative to the total weight of said product obtained” [0040] and “it is easy to obtain zeolitisation of at least 50%, and preferably at least 70%, more preferably at least 80% and even more preferably at least 85%, by weight of the zeolitisable clay or clays present in the binder.” [0050]. This means that the amount of 13X zeolite would be between 2.5% (5% clay with 50% conversion to zeolite) and 21.25% (25% clay with 85% conversion to zeolite) which overlaps the claimed range.
Claim 1 further requires “a ratio of silica to alumina [in Li13X] greater than 2.3 to about 2.6”. 112b issues notwithstanding it is understood that Claim 1 requires a molar ratio of silica to alumina greater than 2.3 (see 112b rejection above). As discussed above, Ortiz et al. does not explicitly disclose Li13X and therefore similarly does not explicitly disclose a ratio of silica to alumina. However if the same caustic digestion was performed on the same halloysite clay the same ratio of silica to alumina would have resulted.
Claim 1 further requires “wherein the LiLSX comprises from an 80 to about 90% of the adsorbent”. Ortiz et al. discloses “The amount by weight of LXS zeolite crystals is generally comprised in a range from 75% to 90% by weight” [0040], which overlaps with the claimed range.
Claim 1 further requires “a ratio of silica to alumina [in LiLSX] less than 2.3”. 112b issues notwithstanding it is understood that Claim 1 requires a molar ratio of silica to alumina less than 2.3 (see 112b rejection above). Ortiz et al. discloses “The LSX zeolite crystals which form the basis of the zeolitic adsorbent material of the present invention have an Si/Al atomic ratio of 1.00+0.05, limits included” [0019]. An atomic ratio of 0.95-1.05 of Si/Al converts to a molar ratio of 1.9-2.1 of silica (SiO2) to alumina (Al2O3) which is within the range claimed.
Claim 1 further requires “and wherein the halloysite clay comprises from about 0.1% to 5.0% of the adsorbent”. Ortiz et al. discloses “the amount of zeolitisable clay is generally comprised in a range from 5% to 25% by weight relative to the total weight of said product obtained” [0040] and “it is easy to obtain zeolitisation of at least 50%, and preferably at least 70%, more preferably at least 80% and even more preferably at least 85%, by weight of the zeolitisable clay or clays present in the binder.” [0050]. This means that the amount of clay remaining would be between 0.75% (5% clay with 85% conversion to zeolite) and 12.5% (25% clay with 50% conversion to zeolite), which overlaps with the claimed range.
Claim 1 further requires “and wherein the adsorbent has a bulk density of at least about 640 g/L, as measured according to DIN/ISO 787.”. Ortiz et al. discloses “Another preferred feature of the zeolitic adsorbent material of the invention is its apparent density, which is generally comprised in a range from 0.58 kg/m−3 to 0.80 kg/m−3, preferably from 0.60 kg/m−3 to 0.75 kg/m−3, more preferably from 0.62 kg/m−3 to 0.70 kg/m−3.” [0031], however the units are obviously wrong. Firstly unlike either kg/m3 or kg*m-3 the unit kg/m−3 is not a density. Secondly if the interpretation kg/m3 (or the equivalent kg*m-3) was adopted it is noted that the material as disclosed would be lighter than air (at a density of about 1.2 kg/m3) which would be impossible for a solid material containing voids filled with air. One of ordinary skill in the art would have recognized this as an obvious error and therefore the common units of density, g/mL (or identically kg/L), are adopted. 0.58 to 0.80 g/mL (or 0.58 to 0.80 kg/L) converts to 580 to 800 g/L, which is within the claimed range. It is noted that Ortiz et al. uses a different standard, “The apparent density of the zeolitic adsorbent material according to the present invention is measured as described in standard DIN 8948/7.6.” [0080], rather than DIN/ISO 787. It is understood that these two standards generate similar but not identical densities and therefore Ortiz et al. is understood to disclose densities of about 580 to about 800 g/L.
Given the above uncertainties about the density disclosed by Ortiz et al. an alternative rejection based on the inherency rationale is given for the limitation of “the adsorbent has a bulk density of at least about 640 g/L, as measured according to DIN/ISO 787.”. The material of Ortiz et al. would have inherently had a density of at least about 640 g/L as measured according to DIN/ISO 787 because it has an identical composition and method of making as the claimed invention and therefore the physical properties, such as density as measured according to DIN/ISO 787, must also be the same. The identical composition can be seen by the mapping of Claim 1 (above). The method of converting clay into zeolite was already relied upon in an inherency rationale (above). Prior to the step of converting clay into zeolite both the instant application [0027] and Ortiz et al. [0032] disclose agglomerating a mixture of zeolite and clay, drying, and calcining. The calcination temperature of the instant application “calcined at a temperature from about 500 to about 700°C” [0030] and Ortiz et al. “calcining can be performed under a flow of oxidizing and/or inert gas … in a range from 250° C. to 700° C., preferably from 300° C. to 650° C” [0042] is the same. After the conversion of clay into zeolite both the instant application [0027] and Ortiz et al. [0032] disclose ion exchange with Li, drying, and activating. Therefore both inventions have an identical composition and method of making and the physical properties must also be the same.
Or alternatively, whatever differences in the composition of the zeolite formed by Ortiz et al. and zeolite 13X and density (no such concession is given) would have been obvious to one of ordinary skill in the art.
Claim 2 requires “a median pore diameter greater than or equal to 5 microns and a percentage of pores less than 0.1 micron lower than 6.0 percent”. Ortiz et al. does not disclose pore diameter, percentage of pores less than 0.1 micron, or pore diffusivity, however these features are believed to be inherent to the material of Ortiz et al. The rationale to support inherency is that both inventions have an identical composition and method of making and the physical properties must also be the same (see Claim 1).
Or alternatively, whatever differences in the pore diameter, percentage of pores less than 0.1 micron, or pore diffusivity (no such concession is given) would have been obvious to one of ordinary skill in the art.
Claim 3 requires “the adsorbent exhibits a crush strength greater than 8 N/mm.”. Ortiz et al. does not disclose a crush strength measured in N/mm or an equivalent but rather discloses “a bulk crushing strength (BCS), measured according to standard ASTM 7084-04, of greater than 1.5 MPa, preferably greater than 2.0 MPa, preferably greater than 2.5 MPa” [0027] and “a grain crushing strength, measured according to standards ASTM D 4179 (2011) and ASTM D 6175 (2013), comprised in a range from 0.5 daN to 30 daN” [0027]. A crush strength of greater than 8 N/mm is believed to be inherent to the material of Ortiz et al. The rationale to support inherency is that both inventions have an identical composition and method of making and the physical properties must also be the same (see Claim 1).
Or alternatively, whatever differences in the crush strength (no such concession is given) would have been obvious to one of ordinary skill in the art.
Claim 4 requires “the adsorbent has a hysteresis factor of at least about 0.6, as measured by the Hg porosimetry method described in US Patent No. 9,486,732 B2.”. Ortiz et al. does not disclose a hysteresis factor of at least about 0.6, however this feature is believed to be inherent to the material of Ortiz et al. The rationale to support inherency is that both inventions have an identical composition and method of making and the physical properties must also be the same (see Claim 1).
Or alternatively, whatever differences in the hysteresis factor between inventions (no such concession is given) would have been obvious to one of ordinary skill in the art.
Claim 5 requires “the adsorbent has a median pore diameter greater than or equal to 5 microns and a hysteresis factor of at least about 0.6, as measured by the Hg porosimetry method described in US Patent No. 9,486,732 B2.”. Ortiz et al. does not disclose a median pore diameter or hysteresis factor, however these features are believed to be inherent to the material of Ortiz et al. The rationale to support inherency is that both inventions have an identical composition and method of making and the physical properties must also be the same (see Claim 1).
Or alternatively, whatever differences in the hysteresis factor and/or median pore diameter between inventions (no such concession is given) would have been obvious to one of ordinary skill in the art.
Claim 7 requires “the halloysite clay has a tubular shape with a length from about 0.5-2.0 micron and a diameter of about 50- 100 nm.”. Ortiz et al. does not disclose the morphology of the halloysite clay used, however these are understood to be physical properties of the clay which would have been naturally present whether disclosed by Ortiz et al. or not. The instant application contains no mention of modifying the morphology or selecting a particular halloysite clay from a particular location to obtain these features and therefore it is understood that all halloysite clay contains this morphology.
Or alternatively, the selection of halloysite clay with a tubular shape, a length from about 0.5-2.0 micron, and a diameter of about 50- 100 nm would have been obvious to one of ordinary skill in the art because the method of Ortiz et al. requires a clay such as halloysite and is not restricted to any particular morphology.
Regarding Claim 17, Claim 17 recites the same limitations of Claim 1 verbatim, with the exception of having no limitation to the bulk density. Support for the rejection of Claim 17 can therefore be found entirely within the rejection of Claim 1 (above).
Regarding Claim 18, Claim 18 solely recites limitations which are addressed in Claim 2. Support for the rejection of Claim 18 can therefore be found entirely within the rejection of Claim 2 (above).
Claim Rejections - 35 USC § 103
Claim(s) 20 is/are rejected under 35 U.S.C. 103 as being unpatentable over US 2019 0388871 A1 Ortiz et al. in further view of EP 0893157 Plee. Claim 20 requires “the low silica X zeolite and the 13X zeolite are lithium exchanged at least about 95%.”. Ortiz et al. discloses “Step c/ of replacing the cations at the exchangeable sites of the product obtained in step b/ by lithium cations is carried out according to methods which are likewise well known to the person skilled in the art and are described for example in patent EP0893157.” EP 0893157 Plee discloses “Five successive exchanges are then carried out using 1 M lithium chloride solutions, at a rate of 20 ml/g of solid. Each exchange is continued for 4 hours at 100°C, and intermediate washes are carried out to remove excess salt at each stage. … Li exchange rate (%) (expressed as Li2O/(Li2O + K2O + Na2O) 98,4 %” [0029].
It would have been obvious for one of ordinary skill in the art before the effective filing date of the claimed invention to have combined the method of Ortiz et al. with the Li exchange method of Plee because Ortiz et al. specifically uses the Li exchange method of Plee as an example. The motivation to combine the method of Ortiz et al. with the Li exchange method of Plee is to generate zeolites with most of the cations exchanged for Li which are known to be effective in nitrogen/oxygen separation (“and by lithium exchange, adsorbents can be produced which are particularly efficient not only in nitrogen/oxygen separation but also in nitrogen-carbon monoxide/hydrogen separation.” [Plee 0014]).
Conclusion
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/JOSHUA MAXWELL SPEER/
Examiner
Art Unit 1736
/ANTHONY J ZIMMER/Supervisory Patent Examiner, Art Unit 1736
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