DETAILED ACTION
Citation to the Specification will be in the following format: (S. # : ¶/L) where # denotes the page number and ¶/L denotes the paragraph number or line number. Citation to patent literature will be in the form (Inventor # : LL) where # is the column number and LL is the line number. Citation to the pre-grant publication literature will be in the following format (Inventor # : ¶) where # denotes the page number and ¶ denotes the paragraph number.
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 .
Status of Application; Continued Examination
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and the fee set forth in 37 CFR 1.17(e) has been timely paid, the finality of the previous Office action has been withdrawn pursuant to 37 CFR 1.114.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 8/26/2025 has been entered.
Claim(s) 1 and 3-25 is/are pending.
Claim(s) 1 is/are currently amended.
Claim(s) 2 is/are acknowledged as cancelled.
Response to Arguments
Claim Rejections – 35 U.S.C. §§ 102-103
I. With respect to the rejection of Claim(s) 1, 3, 7, 8, 9, 10, 11, 14, 15, 16, 17, 19, 20, 24, and 25 under 35 U.S.C. 102(a)(1) as being anticipated by CN 112723343A to Liu, et al. (cited by Applicants, 04-30-2021; C01B32/184) in view of: (i) Chen, et al., Isolation and Characteristics of Cellulose and Nanocelluslose from Lotus Leafe Stalk Agro-wastes, BioResources 2015; 10(1): 684-696 (hereinafter “Chen at __”) to show a state of fact, and (ii) US 2008/0048152 to Jang, et al. to show a state of fact, as understood, the remarks rely on deletion of “cellulose” from the Markush group in Claim 1, limitation A) and Claim 24, limitation A). This is persuasive for this species. New rejections appear below. The rejection is WITHDRAWN.
II. With respect to the rejection of Claim(s) 1, 3, 7, 8, 9, 10, 11, 14, 15, 16, 17, 19, 20, 24, and 25 under 35 U.S.C. 103 as being unpatentable over CN 112723343A to Liu, et al. (cited by Applicants, 04-30-2021; C01B32/184) in view of: (i) Chen, et al., Isolation and Characteristics of Cellulose and Nanocelluslo9se from Lotus Leafe Stalk Agro-wastes, BioResources 2015; 10(1): 684-696 (hereinafter “Chen at __”) to show a state of fact, (ii) US 2008/0048152 to Jang, et al. to show a state of fact, and further in view of: (iii) US 2013/0087446 to Zhamu, et al., and (iv) Chen, et al., Insight into KOH activation mechanism during biomass pyrolysis: Chemical reactions between O-containing groups and KOH, Applied Energy 2020; 278: 115730, pp. 1-12, the rejection is WITHDRAWN in view of the discussion accompanying “Rejection I” above.
III. With respect to the rejection of Claim(s) 4-6 under 35 U.S.C. 103 as being unpatentable over CN 112723343A to Liu, et al. (cited by Applicants, 04-30-2021; C01B32/184) in view of: (i) Chen, et al., Isolation and Characteristics of Cellulose and Nanocelluslo9se from Lotus Leafe Stalk Agro-wastes, BioResources 2015; 10(1): 684-696 (hereinafter “Chen at __”) to show a state of fact, (ii) US 2008/0048152 to Jang, et al. to show a state of fact, and further in view of: (iii) US 2013/0087446 to Zhamu, et al., and (iv) Safian, et al., A Review on Bio-based Graphene Derived from Biomass Wastes, BioResourses 2020; 15(4): 9756-9785 (hereinafter “Safian at __”), the rejection is WITHDRAWN in view of the discussion accompanying “Rejection I” above.
IV. With respect to the rejection of Claim(s) 12-14 under 35 U.S.C. 103 as being unpatentable over CN 112723343A to Liu, et al. (cited by Applicants, 04-30-2021; C01B32/184) in view of: (i) Chen, et al., Isolation and Characteristics of Cellulose and Nanocelluslo9se from Lotus Leafe Stalk Agro-wastes, BioResources 2015; 10(1): 684-696 (hereinafter “Chen at __”) to show a state of fact, (ii) US 2008/0048152 to Jang, et al. to show a state of fact, and further in view of: (iii) US 2013/0087446 to Zhamu, et al., and (iv) Sasikala, et al., Prospects of Supercritical Fluids in Realizing Graphene-Based Functional Materials, Adv. Mater. 2016; 28: 2663-2691 (hereinafter “Sasikala at __”), the rejection is WITHDRAWN in view of the discussion accompanying “Rejection I” above.
V. With respect to the rejection of Claim(s) 16-20 under 35 U.S.C. 103 as being unpatentable over CN 112723343A to Liu, et al. (cited by Applicants, 04-30-2021; C01B32/184) in view of: (i) Chen, et al., Isolation and Characteristics of Cellulose and Nanocelluslo9se from Lotus Leafe Stalk Agro-wastes, BioResources 2015; 10(1): 684-696 (hereinafter “Chen at __”) to show a state of fact, (ii) US 2008/0048152 to Jang, et al. to show a state of fact, and further in view of: (iii) US 2013/0087446 to Zhamu, et al., and (iv) US 2011/0017587 to Zhamu, et al., the rejection is WITHDRAWN in view of the discussion accompanying “Rejection I” above.
VI. With respect to the rejection of Claim(s) 21 and 23 under 35 U.S.C. 103 as being unpatentable over CN 112723343A to Liu, et al. (cited by Applicants, 04-30-2021; C01B32/184) in view of: (i) Chen, et al., Isolation and Characteristics of Cellulose and Nanocelluslo9se from Lotus Leafe Stalk Agro-wastes, BioResources 2015; 10(1): 684-696 (hereinafter “Chen at __”) to show a state of fact, (ii) US 2008/0048152 to Jang, et al. to show a state of fact, and further in view of: (iii) US 2013/0087446 to Zhamu, et al., and (iv) US 2011/0017955 to Zhamu, et al., the rejection is WITHDRAWN in view of the discussion accompanying “Rejection I” above.
VII. With respect to the rejection of Claim(s) 22 under 35 U.S.C. 103 as being unpatentable over CN 112723343A to Liu, et al. (cited by Applicants, 04-30-2021; C01B32/184) in view of: (i) Chen, et al., Isolation and Characteristics of Cellulose and Nanocelluslo9se from Lotus Leafe Stalk Agro-wastes, BioResources 2015; 10(1): 684-696 (hereinafter “Chen at __”) to show a state of fact, (ii) US 2008/0048152 to Jang, et al. to show a state of fact, and further in view of: (iii) US 2013/0087446 to Zhamu, et al., and (iv) US 2017/0158513 to Zhamu, et al., the rejection is WITHDRAWN in view of the discussion accompanying “Rejection I” above.
Claim Rejections - 35 USC §§ 102-103
The text of those sections of Title 35, U.S. Code not included in this action can be found in a prior Office action.
I. Claim(s) 1, 3, 7, 8, 9, 10, 11, 14, 15, 16, 17, 19, 20, 24, and 25 – or as stated below - is/are rejected under 35 U.S.C. 102(a)(1) as being anticipated by CN 112723343A to Liu, et al. (cited by Applicants, 04-30-2021; C01B32/184) in view of:
(i) Zhang, et al., Impact of Hot Water Treated Lotus Leaves on Interfacial and PhysicoMechanical of Gelatin/Lotus Leaf Composites, Journal of Polymers and the Environment 2020; 28: 3270-3278 (hereinafter “Zhang at __”) to show a state of fact,
(ii) US 2008/0048152 to Jang, et al. to show a state of fact.
Citation to Liu is to the machine translation.1
With respect to Claim 1, this claim requires “A) providing a biomass in a liquid state, solution state, solid state, or semi-solid state wherein said biomass is selected from a lignocellulosic biomass or non-lignocellulosic biomass, wherein the lignocellulosic biomass comprises See (Zhang at 3277, Conclusions: “FTIR analyses of the hot water treated lotus leaf revealed the removal of hemicellulose, lignin and hydroxyl groups from the leaf resulting in the enhancement of the interfacial bonding.” Stated differently, lotus leaves have hemicellulose and lignin in them. The process described by Zhang results in their removal. Zhang is only offered to show the presence of hemicellulose and lignin in lotus leaves, and is not “combined” with Liu.
Claim 1 further requires “B) heat treating said biomass at a temperature selected from a range of 100° C to 3,200° C and, concurrently, operating a chemical or mechanical means to form graphene domains dispersed in a disordered matrix of carbon or hydrocarbon molecules, wherein said graphene domains are each composed of from 1 to 30 planes of hexagonal carbon atoms or fused aromatic rings having a length or width from 5 nm to 20 μm and, in the situations wherein there are 2-30 planes in a graphene domain, having an inter-graphene space between two planes of hexagonal carbon atoms or fused aromatic rings no less than 0.34 nm.” The biomass is heat treated at the claimed temperatures. (Liu at 3: “the activation temperature is 700-1800°C”). A chemical means is “operated.” Id. (step S3 / activator mixing). Liu teaches single plane/layer graphene. See (Liu at 2: “Graphene is a new material in which carbon atoms connected by sp2 hybridization are closely packed into a single-layer two-dimensional structure.”). Domains with 3-5 planes are reasonably taught. (Liu “Figs.”). The dimensions are taught. Id. Liu refers throughout to “high-quality graphene material.” (Liu at 4: “It can be seen from Figure 1 that the obtained carbon material is a high-quality graphene material.”). This more than reasonably suggest a crystalline material and the claimed spacing, which is that of graphite. This spacing is well known and taught in any number of places, for example, any number of Jang patents/publications. See (Jang 2: [0031] – “For graphite flakes, the resulting graphene platelets typically contain one to five layers of graphite planes or graphene sheets with each layer of approximately 0.34 nm (3.4Å) thick.”).
Claim 1 further requires “C) separating and isolating said planes of hexagonal carbon atoms or fused aromatic rings to recover graphene sheets from said disordered matrix.” Separating/isolating is broad and generic. At least the washing step is interpreted as separating and isolating. (Liu at 3: “stir and wash, and rinse with distilled water to filter … to obtain absolutely dry biomass-based graphene.”)
Claim 1 further requires “said biomass includes an additive dispersed in said biomass during said heat treating step, wherein said additive is selected from a template, an activator, a chemical functionalization agent, or a combination thereof wherein the additive regulates a thermal transformation process of the biomass during the heat treating step.” Liu teaches an activator (KOH) dispersed in the biomass during heat treatment. See e.g. (Liu at 2-3: steps S3-S4). ).
As to Claim 3, the dimensions are taught. (Liu “Figs.”).
As to Claim 7, KOH would give rise to -OH functional groups. (Liu at 3, passim).
As to Claim 8, single plane/layer graphene is taught. See (Liu at 2: “Graphene is a new material in which carbon atoms connected by sp2 hybridization are closely packed into asingle-layer two-dimensional structure.”). Double/triple layer graphene is reasonably depicted. (Liu “Fig.”).
As to Claim 9, the temperature is taught. (Liu at 4: “the activation temperature is 900°C”).
As to Claim 10, the temperature is taught. (Liu at 4: “the activation temperature is 900°C”).
As to Claim 11, exposure to any number of gasses is taught. (Liu at 3: “one or more of N2, Ar or He”). Mechanical shearing is taught. (Liu at 2: “pulverizer for pulverization”).
As to Claim 14, the water wash is interpreted as dissolving. (Liu at 3-4; passim).
As to Claim 15, “high-quality graphene material” is interpreted as pristine graphene. (Liu at 4). Alternatively or additionally, the functionalization discussed elsewhere is relied on to address the broad “chemically modified graphene” language.
As to Claim 16, KOH would give rise to -OH functional groups. (Liu at 3, passim).
As to Claim 17, KOH would give rise to -OH functional groups. (Liu at 3, passim).
As to Claim 19, KOH contains a hydroxyl group. (Liu at 3, passim).
As to Claim 20, KOH would give rise to -OH functional groups. (Liu at 3, passim).
With respect to Claim 24, this claim requires “A) providing a biomass comprising natural organic molecules in a liquid, solution, solid, or semi-solid state wherein said organic molecules are selected from cellulose, hemicellulose, lignin, carbohydrate, polysaccharide, protein, a chemical derivative thereof, or a combination thereof.” Liu teaches providing biomass in a solid state. (Liu at 2: “S1. Crushed materials: Pour the prepared biomass waste raw materials into a pulverizer for pulverization, pour the pulverized particles into a screen for sieving, and take particles with a uniform pore size for use.”). A number of raw materials are taught, including at least “lotus leaves.” (Liu at 3). Lotus leaves have hemicellulose and lignin in them. Zhang is supplied as evidence. See (Zhang at 3277, Conclusions: “FTIR analyses of the hot water treated lotus leaf revealed the removal of hemicellulose, lignin and hydroxyl groups from the leaf resulting in the enhancement of the interfacial bonding.” Stated differently, lotus leaves have hemicellulose and lignin in them. The process described by Zhang results in their removal. Zhang is only offered to show the presence of hemicellulose and lignin in lotus leaves, and is not “combined” with Liu.
Claim 24 further requires “B) heat treating said biomass to induce decomposition of organic molecules, polymerization, and/or aromatization at a desired temperature and under a desired pressure for a length of time for forming graphene domains dispersed in a disordered matrix of carbon or hydrocarbon molecules, wherein said graphene domains are each composed of one or a plurality of planes of hexagonal carbon atoms or fused aromatic rings having a length or width from 5 nm to 10 μm.” The biomass is heat treated. (Liu at 3: “the activation temperature is 700-1800°C”). Graphene domains are formed. (Liu at 4: “the obtained carbon material is a high-quality graphene material”). The dimensions are taught. (Liu “Figs.”).
Claim 24 further requires “C) separating and isolating said planes of hexagonal carbon atoms or fused aromatic rings to recover graphene sheets from said disordered matrix.” Separating/isolating is broad and generic. The washing at e.g. (Liu at 4) is interpreted as addressing the separating/isolating limitation.
Claim 24 further requires “said biomass includes an additive dispersed in said biomass during said heat treating step, wherein said additive is selected from a template, an activator, a chemical functionalization agent, or a combination thereof wherein the additive regulates a thermal transformation process of the biomass during the heat treating step.” Liu teaches an activator (KOH) dispersed in the biomass during heat treatment. See e.g. (Liu at 2-3: steps S3-S4). ).
As to Claim 25, KOH – a chemical functionalization agent – is added. (Liu at 4; passim).
II. Claim(s) 1, 3, 7, 8, 9, 10, 11, 14, 15, 16, 17, 19, 20, 24, and 25 – or as stated below - is/are rejected under 35 U.S.C. 103 as being unpatentable over CN 112723343A to Liu, et al. (cited by Applicants, 04-30-2021; C01B32/184) in view of:
(i) Zhang, et al., Impact of Hot Water Treated Lotus Leaves on Interfacial and PhysicoMechanical of Gelatin/Lotus Leaf Composites, Journal of Polymers and the Environment 2020; 28: 3270-3278 (hereinafter “Zhang at __”) to show a state of fact,
(ii) US 2008/0048152 to Jang, et al. to show a state of fact, and further in view of:
(iii) US 2013/0087446 to Zhamu, et al., and
(iv) Chen, et al., Insight into KOH activation mechanism during biomass pyrolysis: Chemical reactions between O-containing groups and KOH, Applied Energy 2020; 278: 115730, pp. 1-12 (hereinafter “Chen at __”).
The discussion accompanying “Rejection I” above is incorporated herein by reference.
To the extent the washing step is insufficient to address the broad and generic separating/isolating steps in various claims (no such concession is made), separation and isolation of graphene is an obvious expedient. As Applicants have stated elsewhere, “[i]n 2002, our research team succeeded in isolating single-layer and multi-layer graphene sheets from partially carbonized or graphitized polymeric carbons.” (Zhamu 2: [0018]). Use of known techniques – like those described in any of Applicants myriad other references - to separate/isolate is an obvious expedient. MPEP 2143; KSR.
To the extent activation with KOH is insufficient to address the functionalization recited in various claims, on of skill in the art would understand KOH activation of biomass creates various functional groups. Chen is provided as evidence. See e.g. (Chen Abstract: “The OH– from KOH rapidly entered these vacancies, forming a large amount of new O-containing groups (i.e., C––O, –OH, C–O, O–C––O, and –COOH groups…”).
III. Claim(s) 4-6 – or as stated below - is/are rejected under 35 U.S.C. 103 as being unpatentable over CN 112723343A to Liu, et al. (cited by Applicants, 04-30-2021; C01B32/184) in view of:
(i) Zhang, et al., Impact of Hot Water Treated Lotus Leaves on Interfacial and PhysicoMechanical of Gelatin/Lotus Leaf Composites, Journal of Polymers and the Environment 2020; 28: 3270-3278 (hereinafter “Zhang at __”) to show a state of fact,
(ii) US 2008/0048152 to Jang, et al. to show a state of fact, and further in view of:
(iii) US 2013/0087446 to Zhamu, et al., and
(iv) Safian, et al., A Review on Bio-based Graphene Derived from Biomass Wastes, BioResourses 2020; 15(4): 9756-9785 (hereinafter “Safian at __”).
The discussion accompanying “Rejections I-II” above are incorporated herein by reference.
As to Claim 4, Liu teaches carbonization at the claimed temperatures (Liu at 2, step S2) followed by a higher temperature activation. (Liu at 3, step S4). Liu does not specify hydrothermal carbonization. This difference does not impart patentabilty. Hydrothermal carbonization is a well-known technique in biomass based graphene synthesis. Safian is offered as evidence. The combination reflects substitution of one known heating technique for another to achieve predictable results, namely carbonization. This does not impart patentability. MPEP 2143; KSR. Alternatively, or additionally, one of skill in the art would be motivated to employ hydrothermal carbonization, for example “to overcome the high moisture content in certain biomass,” which “makes pyrolysis difficult, as it necessitates high heat for vaporization.” (Safian at 9761) (citations omitted). Other motivations may be present, for example less amorphous carbon formation. Id. Safian also states “any other thermal treatment can be used as long as the outcome increases the fixed carbon content.” Id. This reinforces the interchangeability of these heating steps.
As to Claim 5, an activator (e.g. KOH) is taught. (Liu at 3: “The activator in step S3 is…”).
As to Claim 6, the activation treatment is interpreted as a “chemical means” (Liu at 4: “S4. Activation treatment under inert atmosphere: Put the carbonized material and KOH mixture into a high temperature…”).
IV. Claim(s) 12-14 – or as stated below - is/are rejected under 35 U.S.C. 103 as being unpatentable over CN 112723343A to Liu, et al. (cited by Applicants, 04-30-2021; C01B32/184) in view of:
(i) Zhang, et al., Impact of Hot Water Treated Lotus Leaves on Interfacial and PhysicoMechanical of Gelatin/Lotus Leaf Composites, Journal of Polymers and the Environment 2020; 28: 3270-3278 (hereinafter “Zhang at __”) to show a state of fact,
(ii) US 2008/0048152 to Jang, et al. to show a state of fact, and further in view of:
(iii) US 2013/0087446 to Zhamu, et al., and
(iv) Sasikala, et al., Prospects of Supercritical Fluids in Realizing Graphene-Based Functional Materials, Adv. Mater. 2016; 28: 2663-2691 (hereinafter “Sasikala at __”).
The discussion accompanying “Rejections I-II” above are incorporated herein by reference.
As to Claim 12, to the extent Liu may not teach the separating/isolation techniques, this difference does not impart patentability. Sasikala teaches any number of supercritical techniques used to prepare graphene. (Sasikala at 2668-2669, Table 3; entire reference). Use of known techniques to achieve predictable results does not impart patentability. MPEP 2143; KSR.
As to Claim 13, water and carbon dioxide are taught. (Sasikala at 2668-2669, Table 3; entire reference).
As to Claim 14, ultrasonication is taught. (Sasikala at 2669). Note the discussion of enhancing the fraction of mono- and double-layer graphene, understood as a motivation to employ ultrasonication. Id.
V. Claim(s) 16-20 – or as stated below - is/are rejected under 35 U.S.C. 103 as being unpatentable over CN 112723343A to Liu, et al. (cited by Applicants, 04-30-2021; C01B32/184) in view of:
(i) Zhang, et al., Impact of Hot Water Treated Lotus Leaves on Interfacial and PhysicoMechanical of Gelatin/Lotus Leaf Composites, Journal of Polymers and the Environment 2020; 28: 3270-3278 (hereinafter “Zhang at __”) to show a state of fact,
(ii) US 2008/0048152 to Jang, et al. to show a state of fact, and further in view of:
(iii) US 2013/0087446 to Zhamu, et al., and
(iv) US 2011/0017587 to Zhamu, et al.
The discussion accompanying “Rejections I-II” above are incorporated herein by reference.
As to Claim 16, to the extent Liu may not teach the functionalization claimed (no such concession is made), Zhamu ‘587 does. (Zhaum ‘587, entire reference). One would be motivated to functionalize the graphene for any number of reasons, for example “improved solubility … in a liquid medium, improved dispersibility … in a matrix material, or enhanced interfacial bonding. (Zhamu ‘587 1: [0002]).
As to Claim 17, at least carboxyl functionalization is taught. (Zhamu ‘587 6: [0059]; 8: [0074]). The discission in the rejection of Claim 16 is relied upon.
As to Claim 18, functionalization of graphene with at least 2-azidoethanol is known. (Zhamu ‘587 [0071]). The discission in the rejection of Claim 16 is relied upon.
As to Claim 19, at least hydroxyl groups are taught. (Zhamu ‘587 6: [0059]).
As to Claim 20, at least carboxyl functionalization is taught. (Zhamu ‘587 6: [0059]; 8: [0074]). The discission in the rejection of Claim 16 is relied upon.
VI. Claim(s) 21 and 23 – or as stated below - is/are rejected under 35 U.S.C. 103 as being unpatentable over CN 112723343A to Liu, et al. (cited by Applicants, 04-30-2021; C01B32/184) in view of:
(i) Zhang, et al., Impact of Hot Water Treated Lotus Leaves on Interfacial and PhysicoMechanical of Gelatin/Lotus Leaf Composites, Journal of Polymers and the Environment 2020; 28: 3270-3278 (hereinafter “Zhang at __”) to show a state of fact,
(ii) US 2008/0048152 to Jang, et al. to show a state of fact, and further in view of:
(iii) US 2013/0087446 to Zhamu, et al., and
(iv) US 2011/0017955 to Zhamu, et al.
The discussion accompanying “Rejections I-II” above are incorporated herein by reference.
As to Claim 21, to the extent Ramsurn may not teach the functionalization claimed, Zhamu ‘955 teaches functionalization with at least DETA. (Zhamu ‘955 4: [0039]).One of skill in the art would be motivated to functionalize graphene with DETA as it is “capable of bonding to the edge or surface of graphene using one of their ends and, during subsequent epoxy curing stage, are able to react with epoxide or epoxy resin at one or two other ends.” Id.
As to Claim 23, phenolic resins are taught. (Zhamu ‘955 4-5: [0040]).
VII. Claim(s) 22 – or as stated below - is/are rejected under 35 U.S.C. 103 as being unpatentable over CN 112723343A to Liu, et al. (cited by Applicants, 04-30-2021; C01B32/184) in view of:
(i) Zhang, et al., Impact of Hot Water Treated Lotus Leaves on Interfacial and PhysicoMechanical of Gelatin/Lotus Leaf Composites, Journal of Polymers and the Environment 2020; 28: 3270-3278 (hereinafter “Zhang at __”) to show a state of fact,
(ii) US 2008/0048152 to Jang, et al. to show a state of fact, and further in view of:
(iii) US 2013/0087446 to Zhamu, et al., and
(iv) US 2017/0158513 to Zhamu, et al.
The discussion accompanying “Rejections I-II” above are incorporated herein by reference.
As to Claim 22, to the extent Liu may not teach the functionalization claimed, Zhamu ‘513 does. (Zhamu ‘523 4: [0040]). The combination reflects use of known techniques to achieve predictable results. This does not impart patentability. MPEP 2143; KSR.
Conclusion
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/DANIEL C. MCCRACKEN/Primary Examiner, Art Unit 1736
1 Made of record with the Final Office Action dated 2/26/2025.