Detailed Notice
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 .
Election/Restrictions
Claim 13-15 are withdrawn from further consideration pursuant to 37 CFR 1.142(b) as being drawn to a nonelected species, there being no allowable generic or linking claim. Election was made without traverse in the reply filed on 10/28/2025.
Claims 1-12 and 16-41 are pending examination.
Specification
The disclosure is objected to because of the following informalities: Applicant has mistakenly reversed the meaning of the cathode and anode half-reactions, as per [0093]. Accordingly, all mentions of anode or anolyte instead are intended to relate to cathode or catholyte, and vice-versa. All instances of this mistaken inversion need correction by restatement of the correct half-reaction to the correct electrode/electrolyte.
Appropriate correction is required.
Drawings
Drawings 1-8 are objected to because they each refer to a cathode, anode, anolyte, or catholyte, which is reversed from the intended. Corrected drawing sheets in compliance with 37 CFR 1.121(d) are required in reply to the Office action to avoid abandonment of the application. Any amended replacement drawing sheet should include all of the figures appearing on the immediate prior version of the sheet, even if only one figure is being amended. The figure or figure number of an amended drawing should not be labeled as “amended.” If a drawing figure is to be canceled, the appropriate figure must be removed from the replacement sheet, and where necessary, the remaining figures must be renumbered and appropriate changes made to the brief description of the several views of the drawings for consistency. Additional replacement sheets may be necessary to show the renumbering of the remaining figures. Each drawing sheet submitted after the filing date of an application must be labeled in the top margin as either “Replacement Sheet” or “New Sheet” pursuant to 37 CFR 1.121(d). If the changes are not accepted by the examiner, the applicant will be notified and informed of any required corrective action in the next Office action. The objection to the drawings will not be held in abeyance.
Claim Interpretation
As noted in the restriction/election requirement, applicant has a plurality of species contained within the instant patent application which causes confusion as regards the claim language and the structure of the intended method being performed by an apparatus. For the purpose of creating unanimous understanding as to what precisely is being prosecuted, the examiner understands that the pertinent sections of the specification pertaining to the elected species to examined are best represented by a top-spray plasma jet system [0127-0130] wherein the plasma jet is sprayed into the anode compartment of an H-type electrolytic cell [0090-0094] wherein the compartments are separated by a proton exchange membrane [0038 and 0041 and 0137-0143] and there exists a degasifier and crystallizer in connection with the “anode” (which is understood to be a cathode), and a makeup liquid injection connected to the “cathode” (which is understood to be an anode) [see Fig. 1]. Simply, anywhere applicant states anode or anolyte, examiner understands these structures instead to be the cathode or catholyte, and vice-versa.
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.
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.
Claim 1 is 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. Specifically applicant requires that following the vibrational excitement of nitrogen atom or nitrogen containing molecule, there are multiple ‘optional” steps. It is unclear whether these steps are actually optional, or whether the applicant does indeed intend to limit that the instant Claim 1 only requires a plasma source generating a vibrationally excited nitrogen containing molecule or atom. For the purposes of compact prosecution, it will be assumed that these limitations are not optional, and there wherever the word optionally appears, what is intended is a require step. Further, applicant states that the “method comprising plasma, such as a microjet plasma” is unclear in the metes and bounds of the clause. Specifically, it is not understood whether the instant claim requires a microjet plasma, or whether for mere demonstration “microjet plasma” is stated. Clarification is required.
Claims 2-12 and 16-36 are rejected as depending from Claim 1.
Claims 7-13, 16-41 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. Where applicant acts as his or her own lexicographer to specifically define a term of a claim contrary to its ordinary meaning, the written description must clearly redefine the claim term and set forth the uncommon definition so as to put one reasonably skilled in the art on notice that the applicant intended to so redefine that claim term. Specifically applicant requires in each of these claims, either by dependence or explicit statement, some structural relationship of an apparatus to an anolyte, catholyte, cathode, or anode (e.g., such as claim 11 requiring that the anolyte solution is recirculated). As per [0093] of the instant specification, it is clear that the applicant has mistaken the convention of sign ascribed to the anode and cathode. However, at a plain face reading, this does create confusion as to the applicant’s intended final apparatus for doing the method depending from Claim 1. For the purposes of compact prosecution, the examiner understands that applicant’s principal intent is that anywhere the applicant has written anolyte or anode, it would appear by invocation of the water splitting half reaction, such as [0138-0139], they intended to say the catholyte or cathode, respectively, instead and vice-versa. The cathode and catholyte are understood to be instead the anode and anolyte; the anode and anolyte are understood to be the cathode and catholyte. Under MPEP section 2163.07 II, correction of these mistakes in the claims and specification does not introduce new matter, as given the half-reactions described in [0093] and the corresponding depiction of oxygen evolving from the “cathode”, one of ordinary skill would immediately and obviously understand the error which had occurred in the drafting of this application. Electrochemistry is notoriously fickle in its sign convention, where the voltaic/battery cell signage is the opposite of the electrolytic cell signage, which would appear to be the error made for. Correction of the errors for all elements relating to anode, cathode, catholyte, and anolyte is required.
Claims 10 is 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. Specifically, applicant requires that the gas flow rate is sufficient for the gas to reach the anode within 1 second. This is unclear as the metes and bounds of the claim limitation are not obvious as written. If the region through which the gas travelled were at a length reaching one astronomical unit, the claim would require thereby that the gas flow rate exceed the speed of light, which presently defies known laws of physics. Accordingly, for compact prosecution, it is understood that the claim merely requires that the gas flow rate is sufficient to reach the anode. Attention is required.
Claim 5 is 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. Specifically claim 5 requires that the length of the RF electrode is optional. It is not clear whether the claim requires this limitation or not. For the purposes of compact prosecution it is understood the claim merely requires gas to flow through an annulus determined by an outer surface of a ground electrode and an inner surface of an RF electrode.
Claims 12 is 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. Specifically claim 12 requires that the degasification chamber may be optionally be an ultrasonic. It is not clear whether the claim requires this limitation or not. For the purposes of compact prosecution it is understood the claim merely requires that the recirculated solution passes through a degasification chamber.
Claims 19 is 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. Specifically claim 19 requires that precipitated ammonium nitrate is optionally separated from the recycled liquor. It is not clear whether the claim requires this limitation or not. For the purposes of compact prosecution it is understood the claim merely requires that requires temperature and concentrations are maintained to precipitate solid ammonium nitrate.
Claims 24 is 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. Specifically claim 24 requires that the recirculation paths return to the anolyte cell. It is not clear whether the claim requires this limitation or not. For the purposes of compact prosecution it is understood the claim merely requires that the recirculation paths must return to the anolyte cell.
Claims 29 is 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. Specifically claim 29 requires that condensate liquid is optionally removed as a product, and wherein the condenser is optionally a fractional distillation column to remove ammonia from other condensed gases. It is not clear whether the claim requires this limitation or not. For the purposes of compact prosecution it is understood the claim merely requires that the recycled anolyte gas passes through a condenser at a temperature lower than the anolyte cell and where the condensate comprises primarily liquid ammonia and water.
Claims 34 is 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. Specifically, applicant states that a proton membrane allows conduction of hydroxyl ions. This is indefinite as it is unclear how a proton membrane, which conducts protons, those being positively charged ions, could also conduct negatively charged ions as well, yet preclude the neutral, negative, and positively charged ammonia derivates of nitrate ammonia and ammonium. For the sake of compact prosecution it is understood that the instant claim merely requires that a proton membrane separate the anolyte cell and catholyte cell.
Claims 37 is 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. Specifically claim 37 requires that the metallic hydroxide is optionally potassium hydroxide. It is not clear whether the claim requires this limitation or not. For the purposes of compact prosecution it is understood the claim merely requires that no specific metallic hydroxide is required.
Claim Rejections - 35 USC § 102
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.
Claims 1-3, 5, 7-8, 10 are rejected under 35 U.S.C. 102(a)(1) as being anticipated by Kumari et. al “Synergistic plasma-assisted electrochemical reduction of nitrogen to ammonia” Chem. Commun, 2018, 54, 13347 with the corresponding Supporting Information as supplementary evidence.
Regarding Claim 1, 7-8, 10 Fig. 1 of Kumari is shown below. Kumari teaches a method for forming ammonia via the use of non-thermal plasma generated from a mixture of helium and nitrogen gas, to produce vibrationally excited N2 species which then electrochemically reacted at with a solution in a cathode compartment containing protons which crossed over (via a proton exchange membrane) from the water oxidation reaction occurring at the anode compartment [Pg. 13350, Col. 1, bottom paragraph].
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Regarding Claims 2 and 3, Kumari teaches that the plasma jet reactor consists of an inner steel rod electrode and an outer copper tube electrode with a spacing of approximately 5 mm [Pg. 1, Col. 1, 1st paragraph]. Kumari teaches that a N2 and He gas were flowed through the glass at 2.5 std L min-1, which is understood to be on the order of 1 Barg [Pg. 1, Col. 1, 1st paragraph]. Kumari teaches that the plasma was driven by an AC power supply, such that the copper tube is connected to ground, which means that the steel electrode functions as an RF electrode [Pg. 1, Col. 1, 1st paragraph].
Regarding Claim 5, Kumari teaches that an inner 3.2 mm steel diameter electrode and an outer 13 mm copper tube electrode comprise the RF and ground electrodes. Each rod has a diameter. In a volume of space between the two electrode rods flows gas, which is understood to teach to the instant claim [Pg. 1, Col. 1, 1st paragraph].
Claim 1 and 34 are rejected under 35 U.S.C. 102(a)(1) as being anticipated by Lovell (US20240052502A1).
Regarding Claim 1, Lovell teaches a method for forming ammonia from nitrogen and hydrogen by subjecting a nitrogen gas to plasma forming conditions; contacting the nitrogen-containing plasma with water/electrolyte; electrocatalytically reducing the dissolved species formed by the nitrogen-containing plasma to provide ammonia [0031].
Regarding Claim 34, Lovell teaches the use of a H-cell electrolytic cell wherein the catholyte and anolyte chambers are separated by a proton exchange membrane, which understood to conduct protons generated at the anode to the catholyte solution [0124].
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.
Claim 4 is rejected under 35 U.S.C. 103 as being unpatentable Kumari et. al “Synergistic plasma-assisted electrochemical reduction of nitrogen to ammonia” Chem. Commun, 2018, 54, 13347 with the corresponding Supporting Information as supplementary evidence, as applied to claim 1 above, and further in view of Papadopoulos (US 11153960 B1).
Regarding Claim 4, Kumari teaches to Claim 1 as shown above.
However, Kumari does not teach that the microplasma device has both electrodes being made of an alloy of at least 90% weight tungsten.
Papadopoulos teaches a system for generating plasma [abstract].
Papadopoulos teaches that the nature of the material of the electrodes has very little effect on the characteristics of discharge for plasma generation, although tungsten in particular is commonly used for high temperature applications [0035; 0050; 0056].
Prior to the filing of the present invention it would have been obvious to one of ordinary skill that the use of tungsten for the electrode materials in a plasma device, as per Papadopoulos, could be substituted for the Cu and stainless steel electrodes in the microplasma generation device, as per Kumari, to obtain the predictable result of a microplasma device with electrodes better thermal resistance characteristics.
Claim 9 is rejected under 35 U.S.C. 103 as being unpatentable Kumari et. al “Synergistic plasma-assisted electrochemical reduction of nitrogen to ammonia” Chem. Commun, 2018, 54, 13347 with the corresponding Supporting Information as supplementary evidence, as applied to claim 1 above, further in view of Zheng et al. “Self-Activated Ni Cathode for Electrocatalytic Nitrate Reduction to Ammonia From Fundamentals to Scale-Up for Treatment of Industrial Wastewater.” Environ. Sci. Technol. 2021, 55, 13231−13243.
Regarding Claim 9, Kumari teaches to Claim 1, as shown above. Kumari teaches that the cathode catalyst was Pt, which is highly active towards the hydrogen evolution reaction, and suggests that a more reactive catalyst for the nitrogen reduction reaction is desirable.
However, Kumari does not teach that the cathode comprises an alloy comprising Nickel.
Zheng teaches a method of electrocatalytic reduction of nitrates to form ammonia [abstract]. Zheng teaches the use of Ni foam cathode [Pg. 13232, Experimental Section, Laboratory Tests on Ni Cathode]. Zheng teaches that Ni is a self-activated catalyst, meaning that the surface sites of the Ni catalyst become converted into Ni(OH)2 [Pg. 13236, Col. 2, middle paragraph last sentence]. Zheng teaches that the use of a Ni(OH)2 catalyst is advantageous to the production of ammonia in aqueous solutions, as the nitrate reduction reaction (where it is understood that as per [0094] nitrates are a known intermediate in the system and) has thermodynamic and kinetic favorability over the hydrogen evolution reaction [see Fig. 5c; Pg. 13239, Col. 1, Para. 3]. Zheng teaches that Ni(OH)2 is an effective electrocatalyst for producing ammonia owing to its high selectivity over HER and its long-term stability [Pg. 13240, Col. 1, 2nd paragraph].
Prior to the filing of the present invention it would have been obvious to one of ordinary skill that the Ni cathode of Zheng could have been substituted for the Pt particle cathode of Kumari in order that one would arrive at a plasma-assisted electrochemical system for ammonia production that has improved stability and selectivity for ammonia production over HER.
Claims 11-12, 17, 28, 30-31, 35-36 are rejected under 35 U.S.C. 103 as being unpatentable over Lovell (US20240052502A1) in view of MacFarlane (US20210079534A1).
Regarding Claim 11-12 and 17, Lovell teaches to Claim 1 as shown above. Lovell teaches the use of a H-cell electrolytic cell wherein the catholyte and anolyte chambers are separated by a membrane [0124].
However, Lovell does not teach that the catholyte solution is recirculated.
MacFarlane teaches a method for the electrochemical reduction of dinitrogen to ammonia [abstract]. Below is Fig. 10 of MacFarlane.
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As seen in Fig. 10, MacFarlane teaches an method of dinitrogen reduction wherein N2 is saturated into electrolyte via (54), which supplies N2 saturated electrolyte to the cathode (40) via inlet (56); the solution is reduced to form ammonia via protons supplied from the anode (42) by migration across the proton membrane (44); the catholyte solution being laden with ammonia, hydrogen, and nitrogen gases leaves via outlet (58) such that ammonia and hydrogen gases are removed in a product separation vessel (60) before the electrolyte is returned to (54) wherein the electrolyte is resupplied N2 gas and is resupplied to the catholyte chamber via inlet (56) [0116; and 0452 to 0455].
Prior to the filing of the present invention it would have been obvious to one of ordinary skill that the known method of recirculating the electrolyte and remove gaseous electroredox product from a catholyte solution, as per MacFarlane, could be applied to the base device of the electrochemical H-cell with a plasma nitrogen forming element, as per Lovell, with a reasonable expectation of success.
Regarding Claim 19, Lovell teaches that the product balance may be maintained in order to directly produce ammonium nitrate [0117].
Regarding Claim 28 and 35, Lovell teaches the use of a H-cell electrolytic cell wherein the catholyte and anolyte chambers are separated by a membrane [0124]. Lovell teaches that teaches that a plasma bubbler is introduced to the catholyte cell as per Fig. 6b [0117]. Lovell further teaches in Fig. 6b that oxygen gas leaves the anolyte solution, understood to be removed [0117]. Below is Fig. 6b of Lovell.
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However, Lovell does not teach that the anolyte gas is recycled.
As seen in Fig. 10, MacFarlane teaches an method of dinitrogen reduction wherein N2 is saturated into electrolyte via (54), which supplies N2 saturated electrolyte to the cathode (40) via inlet (56); the solution is reduced to form ammonia via protons supplied from the anode (42) by migration across the proton membrane (44); the catholyte solution being laden with ammonia, hydrogen, and nitrogen gases leaves via outlet (58) such that ammonia and hydrogen gases are removed in a product separation vessel (60) before the electrolyte containing unreacted N2 gas is returned to the bubbler (54) wherein the electrolyte is supplied with more N2 gas via the bubbler (54) to render the electrolyte and is resupplied to the catholyte chamber via inlet (56) [0116; and 0452 to 0455]. Accordingly, it is understood that MacFarlane teaches that the catholyte gas is recycled, and it is also understood that the makeup flow of electrolyte comprises water and N2 and is equivalent to the molar outflow of N2 as MacFarlane is teaching that the electrolyte supplied to the cathode is always saturated with N2.
Prior to the filing of the present invention it would have been obvious to one of ordinary skill that the known method of recirculating the anolyte gas while adding yet more reactant gas, as per MacFarlane, could be applied to the base device of the electrochemical H-cell with a plasma nitrogen forming element, as per Lovell, with a reasonable expectation of success.
Regarding Claims 30-32, Lovell teaches the use of a H-cell electrolytic cell wherein the catholyte and anolyte chambers are separated by a membrane [0124]. Lovell teaches that teaches that a plasma bubbler is introduced to the catholyte cell as per Fig. 6b [0117].
However, Lovell does not teach that the anolyte gas and combined with makeup gas before re-entering the microplasma reactor.
As seen in Fig. 10, MacFarlane teaches an method of dinitrogen reduction wherein N2 is saturated into electrolyte via (54), which supplies N2 saturated electrolyte to the cathode (40) via inlet (56); the solution is reduced to form ammonia via protons supplied from the anode (42) by migration across the proton membrane (44); the catholyte solution being laden with ammonia, hydrogen, and nitrogen gases leaves via outlet (58) such that ammonia and hydrogen gases are removed in a product separation vessel (60) before the electrolyte containing unreacted N2 gas is returned to the bubbler (54) wherein the electrolyte is supplied with more N2 gas via the bubbler (54) to render the electrolyte and is resupplied to the catholyte chamber via inlet (56) [0116; and 0452 to 0455]. Accordingly, it is understood that MacFarlane teaches that the catholyte gas is recycled, and it is also understood that the makeup flow of electrolyte comprises water and N2 and is equivalent to the molar outflow of N2 as MacFarlane is teaching that the electrolyte supplied to the cathode is always saturated with N2.
Prior to the filing of the present invention it would have been obvious to one of ordinary skill that the known method of recirculating the anolyte gas while adding yet more reactant gas, as per MacFarlane, could be applied to the base device of the electrochemical H-cell with a nitrogen plasma generating system, as per Lovell, such that one would arrive at a system which resupplies catholyte gas and solution to the microplasma bubbler before the plasma laden solution returns to the catholyte chamber, with a reasonable expectation of success.
Regarding Claim 35 and 36, as seen in Fig. 6b of Lovell, water is supplied to the system while oxygen is removed [Fig. 6B above]. It is understood that as the volume of the electrolyte in the anolyte is related to the water oxidation reaction to produce the required protons and subsequent oxygen gas, that the molar outflow of oxygen would be substantially similar to the inflow of water, in order that the cell does not become depleted.
Allowable Subject Matter
Claims 16,18, 20-27, 29, 33-34, 37-41 objected to as being dependent upon a rejected base claim, but would be allowable if rewritten in independent form including all of the limitations of the base claim and any intervening claims.
The following is a statement of reasons for the indication of allowable subject matter: The prior art does not teach or suggest the use of a recirculation system for a crystallization process through a condenser system. These elements in specific are related to processes for converting the electrogenerated ammonia, generated via the plasma assisted electrocatalytic conversion of a nitrogen containing plasma, into ammonium nitrate. This additional processing step which exists in this system in tandem with the initial ammonia process is not taught or suggested by the prior art.
Conclusion
Any inquiry concerning this communication or earlier communications from the examiner should be directed to NATHANAEL J DOWNES whose telephone number is (571) 272-1141. The examiner can normally be reached 8am to 5pm.
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NATHANAEL JASON. DOWNES
Examiner
Art Unit 1794
/NATHANAEL JASON DOWNES/
Examiner, Art Unit 1794 /BRIAN W COHEN/Primary Examiner, Art Unit 1759