Office Action 2: Notice of Allowance (2025-10-21)

CLAIMS:
Listing of Claims:

Serial No. 18/447,930AMENDMENTS TO CLAIMSThis listing of claims will replace all prior versions, and listings, of claims in the application:

1\. Cancelled

2\. (Currently Amended) A process to perform a controlled exothermic delignification of biomass, said process comprising the steps of:- providing a system comprising at least a first vessel and a second vessel;
\- providing abiomass comprising lignin, hemicellulose and cellulose fibers into said first vessel;
\- providing an aqueous acidic composition comprising a sulfuric acid component;
\- providing a modifier component;
\- providing a peroxide component;
\- exposing said biomass to said sulfuric acid, modifier and peroxide components, creating a reaction mass;
\- mixing said reaction mass;
\- allowing said sulfuric acid, modifier and peroxide components to come into contact with said reaction mass for a period of time sufficient to a delignification reaction to occur and remove a pre-determined amount of said lignin from said reaction mass thereby forming a first treated biomass;
wherein said pre-determined amount is assessed by testing a first kappa number, with a second suitable apparatus, of the first treated biomass, when said first kappa number of said first treated biomass is reached, the first treated biomass is transferred to said second vessel;
\- allowing the temperature of the first treated biomass to increase during the residence time of said first treated biomass in said second vessel;
\- allowing said sulfuric acid component and peroxide component to continue said delignification reaction at a second temperature and remove a second pre- determined amount of said lignin from said first treated biomass;
Serial No. 18/447,930
wherein said second pre-determined amount is assessed by testing a second kappa number, with a second suitable apparatus, of the first treated biomass, when said second kappa number of said first treated biomass is reached, the first treated biomass is removed from said second vessel;- optionally, a washing step is employed to separate a resulting liquid portion comprising said lignin and hemicellulose from the solid portion containing the cellulose extracted from the first treated biomass, said washing step thereby forming a second treated biomass.
3\. (Currently Amended) The process according to claim 2, wherein said system comprises a third vessel where the first treated biomass is sent to after being removed form said second vessel,
\- allowing the temperature of the first treated biomass mixture to increase during the residence time of said first treated biomass in said second vessel;
\- allowing said sulfuric acid, modifier and peroxide components to continue said delignification reaction at said second temperature and remove a third pre- determined amount of said lignin from said first treated biomass;
wherein said third pre-determined amount is assessed by testing a third kappa number, with a third suitable apparatus, of the first treated biomass, when said third kappa number of said first treated biomass is reached, the first treated biomass is removed from said third vessel.
4\. (Original) The process according to claim 3, where said process requires temperature control at said first vessel, said second vessel and said third vessel.
5\. (Original) The process according to claim 4, where said temperature control comprises a heat exchanger, jacketed vessel and baffles.
6\. (Previously Presented) The process according to claim 4, where said primary temperature control is a heat exchanger, secondary control is a jacketed tank and tertiary control is a baffle.
7\. (Previously Presented) The process according to claim 2, where said system has an outlet which allows the separation of solids from liquids.

Serial No. 18/447,930

8\. (Previously Presented) The process according to claim 2, where said mixing in said first vessel is performed by a recirculation of the reaction mass.

9\. (Currently Amended) The process according to claim 2, wherein mixing in said second vessel is performed by a paddle mixer.

10\. (Currently Amended) The process according to claim 2, wherein mixing in said third vessel is performed by a paddle mixer.

11\. (Previously Presented) The process according to claim 2, where said sulfuric acid component comes from a modified Caro's acid composition selected from the group consisting of composition A; composition B and Composition C;wherein said composition A comprises:
\- sulfuric acid in an amount ranging from 20 to 70 wt% of the total weight of the composition;- a modifier component comprising an amine moiety and a sulfonic acid moiety selected from the group consisting of: taurine; taurine derivatives; and taurine-related compounds; and
\- a peroxide;
wherein said composition B comprises:- an alkylsulfonic acid; and
\- a peroxide; wherein the acid is present in an amount ranging from 40 to 80 wt% of the total weight of the composition and where the peroxide is present in an amount ranging from 10 to 40 wt% of the total weight of the composition;
wherein said composition C comprises:- sulfuric acid;
\- a two-part modifier component comprising:
\- a compound comprising an amine moiety; and
\- a compound comprising a sulfonic acid moiety; and
\- a peroxide.

Serial No. 18/447,930

12\. (Currently Amended) The process according to claim 2, where the temperature of the second treated biomass is maintained at a temperature ranging from 30 - 45°C.
13\. (Currently Amended) The process according to claim 2, wherein at least part of the resulting liquid after coming out of the second vessel is used to treat at least one additional biomass batch.
14\. (Currently Amended) The process according to claim 2, wherein at least part of the resulting liquid after coming out of the second vessel is used to treat at least four additional biomass batches.
15\. (Currently Amended) The process according to claim 2, wherein at least part of the resulting liquid after coming out of the second vessel is used to further treat additional biomass batches until the peroxide concentration reaches less than 1%.

OFFICE ACTION:
EXAMINER'S AMENDMENT
An examiner’s amendment to the record appears below. Should the changes and/or additions be unacceptable to applicant, an amendment may be filed as provided by 37 CFR 1.312. To ensure consideration of such an amendment, it MUST be submitted no later than the payment of the issue fee.
Authorization for this examiner’s amendment was given in an interview with Attorney Brent Johnson on 10/7/2025.
The application has been amended as follows:
Claim 2 has been replaced by the following:
A process to perform a controlled exothermic delignification of biomass, said process comprising the steps of:
- providing a system comprising at least a first vessel and a second vessel;
- providing biomass comprising lignin, hemicellulose and cellulose fibers into said first vessel;
- providing an aqueous acidic composition comprising a sulfuric acid component;
- providing a modifier component;
- providing a peroxide component;
- exposing said biomass to said sulfuric acid component, modifier and peroxide components, creating a reaction mass;
- mixing said reaction mass;
- allowing said sulfuric acid, modifier and peroxide components to come into contact with said reaction mass for a period of time sufficient to a delignification reaction to occur and remove a pre-determined amount of said lignin from said reaction mass;
wherein said pre-determined amount is assessed by testing a first kappa number, with a first suitable apparatus, of the reaction mass when said first kappa number of said reaction mass is reached a first treated biomass is formed, the first treated biomass is transferred to said second vessel;
- allowing the temperature of the first treated biomass to increase during the residence time of said first treated biomass in said second vessel;
- allowing said sulfuric acid component and peroxide component to continue said delignification reaction at a second temperature and remove a second pre-determined amount of said lignin from said first treated biomass;
wherein said second pre-determined amount is assessed by testing a second kappa number, with a second suitable apparatus, of the first treated biomass, when said second kappa number of said first treated biomass is reached a second treated biomass is formed, the second treated biomass is then removed from said second vessel;
- optionally, a washing step is employed to separate a resulting liquid portion comprising said lignin and hemicellulose from a solid portion containing the cellulose extracted from the second treated biomass, said washing step thereby forming a washed biomass.
---
Claim 3 has been replaced by the following:
The process according to claim 2, wherein said system comprises a third vessel where the second treated biomass is sent to after being removed form said second vessel,
- allowing the temperature of the second treated biomass to increase during the residence time of said second treated biomass in said third vessel;
- allowing said sulfuric acid, modifier and peroxide components to continue said
delignification reaction at said third temperature and remove a third pre-
determined amount of said lignin from said second treated biomass;
wherein said third pre-determined amount is assessed by testing a third kappa number, with a third suitable apparatus, of the second treated biomass, when said third kappa number of said second treated biomass is reached a third treated biomass is formed, the third treated biomass is removed from said third vessel.
--
Claim 12 has been replaced by the following:
The process according to claim 4, where the temperature of said first vessel or said second vessel is maintained at a temperature ranging from 30-45°C.
--
In claim 13 line 2 after the word “liquid” the word “portion” has been added.
In claim 14 line 2 after the word “liquid” the word “portion” has been added.
In claim 15 line 2 after the word “liquid” the word “portion” has been added.
Reasons for Allowance
The following is an examiner’s statement of reasons for allowance:  It is known to bleach pulp (delignified biomass) with sulfuric acid, peroxide, and modifiers.  The prior art did not suggest treating a biomass in a multi-stage system with peroxide, sulfuric acid, and a modifier and pulping to a first kappa number in the first stage and pulping to a second kappa number in the second stage.
Any comments considered necessary by applicant must be submitted no later than the payment of the issue fee and, to avoid processing delays, should preferably accompany the issue fee.  Such submissions should be clearly labeled “Comments on Statement of Reasons for Allowance.”
Conclusion

APPLICANT REBUTTAL: REMARKS/ARGUMENTS
Status of the Claims
In the Non-final Office Action mailed on May 20, 2025, claims 1-15 are pending in the application; Claims 1-15 stand rejected;
As set forth herein, reconsideration and withdrawal of the rejections and objections of the claims is respectfully requested.
Obj
ections to Drawings
The drawings are objected to as failing to comply with 37 CPR 1.84(p)(5) because they include reference character(s) not mentioned in the description. The drawings were further objected to as failing to comply with 37 CPR 1.84(p)(5) because they do not include the following reference sign(s) mentioned in the description. The specification and figures are amended herein to address each of the objections made to the drawings. It is believed that no new matter is added to the specification and drawings. Therefore, the drawing objections should be withdrawn.
Rej
ection Under 35 U.S.C.
Claims 2 to 15 are re
j
ected under 35 U.S.C. 112(b) or pre-AIA 35 U.S.C. 112
,
second paragraph
,
as being indefinite for failing to particularly point out and distinctly claim the sub
j
ect matter which the inventor or a
j
oint inventor (or for applications sub
j
ect to pre-AIA 35 U.S.C. 112
,
the applicant), regards as the invention.
The Applicant respectfully traverses this rejection.
The claims are amended to address each of the Examiner's points made in this rejection. Therefore, this rejection should be reconsidered and withdrawn.
Rej
ection Under 35 U.S.C.
Claim 1 is re
j
ected under 35 U.S.C. 102(a)(1) as being anticipated by WO Publication No. 98/02612 (hereinafter referred to as AKHTAR).
The Applicant respectfully traverses this rejection.
Claim 1 is cancelled. Therefore, this rejection is moot and should be withdrawn.
Allowable Sub
j
ect Matter
Claim 2 is indicated as allowable if rewritten or amended to overcome the rejection(s)
under 35 U.S.C. 1 12(b) or pre-AIA 35 U.S.C. 112, 2nd paragraph, set forth in this Office action.
The Applicant gratefully acknowledges the allowability of this claim.
Conclusion


CITED REFERENCE SUMMARIES: Ref US5433825A: Claims:
A process for pulping wood chips comprising the steps of: (a) contacting wood chips with a first alkaline liquor wherein said contact takes place at a temperature of from about 0Â° C. to about 80Â° C. and at a pressure in the range of from about 1 atm to about 15 atm; (b) maintaining said wood chips in contact with said alkaline liquors for a period of time sufficient to permit swelling of said wood chips wherein the wood structure becomes sufficiently permeable to allow the passage of an acidic oxidizing liquor and wherein the pH of said oxidizing liquor is between -0.3 and 1.99; (c) contacting said alkaline swollen wood chips with an acidic oxidizing liquor comprising peroxymonosulfate anion; (d) maintaining said wood chips in contact with said acidic oxidizing liquor for a time sufficient to oxidize a substantial amount of the lignin of said wood chips, wherein said contact with said acidic oxidizing liquor takes place at a temperature of from about 0Â° C. to about 50Â° C., at a pressure of from about 1 atm to about 15 atm, and for a time period of from about 0.5 hours to about 290 hours; and (e) contacting said acid treated wood chips with a second alkaline liquor for a period of time of from about 0.3 hours to about 72 hours at a temperature of from about 0Â° C. to about 80Â° C. and at a pressure of from about 1 atm to about 10 atm which is sufficient to solubilize and extract said oxidized lignin, wherein said alkaline treated wood chips are sufficiently fiberized to produce a pulp that does not require subsequent mechanical refiner step.
(a) contacting wood chips with a first alkaline liquor wherein said contact takes place at a temperature of from about 0Â° C. to about 80Â° C. and at a pressure in the range of from about 1 atm to about 15 atm;
(b) maintaining said wood chips in contact with said alkaline liquors for a period of time sufficient to permit swelling of said wood chips wherein the wood structure becomes sufficiently permeable to allow the passage of an acidic oxidizing liquor and wherein the pH of said oxidizing liquor is between -0.3 and 1.99;
(c) contacting said alkaline swollen wood chips with an acidic oxidizing liquor comprising peroxymonosulfate anion;
(d) maintaining said wood chips in contact with said acidic oxidizing liquor for a time sufficient to oxidize a substantial amount of the lignin of said wood chips, wherein said contact with said acidic oxidizing liquor takes place at a temperature of from about 0Â° C. to about 50Â° C., at a pressure of from about 1 atm to about 15 atm, and for a time period of from about 0.5 hours to about 290 hours; and
(e) contacting said acid treated wood chips with a second alkaline liquor for a period of time of from about 0.3 hours to about 72 hours at a temperature of from about 0Â° C. to about 80Â° C. and at a pressure of from about 1 atm to about 10 atm which is sufficient to solubilize and extract said oxidized lignin, wherein said alkaline treated wood chips are sufficiently fiberized to produce a pulp that does not require subsequent mechanical refiner step.
A process in accordance with claim 1 wherein said alkali in said first alkaline liquor is present at a level in the range of from about 0.001 to about 2.5 molar.
A process in accordance with claim 1 wherein said first alkali liquor to wood chips ratio on a dry basis is between 1:1 and 50:1.
A process in accordance with claim 1 wherein said wood chips is maintained in said first alkaline liquor for a period of from about 20 minutes to about 3 days.
A process in accordance with claim 1 wherein said acidic oxidizing liquor has peroxymonosulfate anion present at a level of from about 0.1% to about 20% by weight.
A process in accordance with claim 1 wherein said acidic oxidizing liquor has peroxymonosulfate anion present at a level of from about 0.5% to about 9% by weight.
A process in accordance with claim 1 wherein said acidic oxidizing liquor is present at a weight:weight ratio to wood chips of from about 1:1 to about 50:1.
A process in accordance with claim 1 wherein said acidic oxidizing liquor is present at a weight:weight ratio to wood chips of from about 10:1 to about 25:1.
A process in accordance with claim 1 wherein the pH of said acidic oxidizing liquor being from about -0.1 to 1.8.
A process in accordance with claim 1 wherein said contact with said acidic oxidizing liquor takes place at a temperature of from about 20Â° C. to about 50Â° C. and at a pressure of from about 1 atm to about 10 atm.
A process in accordance with claim 1 wherein the pH of said first alkaline liquor is above pH 11.
A process in accordance with claim 1 wherein the pH of said second alkaline liquor is above pH 10.
A process in accordance with claim 1 wherein the alkaline material used in said first alkaline liquor and said second alkaline liquor is selected from the group consisting of alkali metal and alkaline earth metal hydroxides, ammonium hydroxide and organic bases.
A process in accordance with claim 1 wherein said alkaline material used for said first alkaline liquor and said second alkaline liquor is sodium hydroxide.
Ref US5246543A: Claims:
A process for the bleaching and delignification effect wherein the essential steps are reacting lignocellulosic pulp for a sufficient period of time with a source of peroxomonosulfuric acid at a starting pH between 1 and 11 and wherein the final pH is from 3 to 5, optionally washing said pulp, subsequently subjecting said pulp to an oxygen or peroxide or oxygen peroxide delignifying and bleaching stage to obtain the desired degree of delignification or brightness or delignification and brightness without significant cellulose degradation or increase in viscosity loss, while strength properties of the pulp are improved.
The process according to claim 1, wherein a peroxide stabilizer is added to the treatment with peroxomonosulfuric acid.
The process according to claim 2, wherein the stabilizer is DTPA, EDTA, DTPMPA, silicate or Mg salts.
The process according to claim 1, wherein the pulp is initially contacted with an agent to remove heavy metal contamination.
The process according to claim 1, wherein the peroxomonosulfuric acid treatment is carried out at a temperature of 5Â° C. to 100Â° C.
The process according to claim 5, wherein the peroxomonosulfuric acid treatment is carried out at a temperature of 15Â° C. to 70Â° C.
The process according to claim 1, wherein the solids content in the peroxomonosulfuric acid treatment is 0.01 to 60%.
The process according to claim 7, wherein the solids content is 1 to 30%.
The process according to claim 1, wherein the reaction time in the peroxomonosulfuric acid treatment is 1 second up to 24 hours.
The process according to claim 9, wherein the reaction time is 1 second to 10 hours.
The process according to claim 1, wherein 0.01% active oxygen to 3% active oxygen is used in the peroxomonosulfuric acid treatment.
The process according to claim 11, wherein 0.05% active oxygen to 1.5% active oxygen is used.
The process according to claim 1, wherein the pressure in the peroxomonosulfuric acid treatment is atmospheric to 0.5 MPa.
The process according to claim 1, wherein the only oxidant used in the subsequent stage is oxygen.
The process according to claim 1, wherein the oxidant used in the subsequent stage is hydrogen peroxide, peroxomonosulfuric acid, and Na 2 O 2 alone or in combination.
The process according to claim 1, wherein the subsequent stage contains oxygen and peroxide.
The process according to claim 1, wherein the subsequent stage contains a combination of hypochlorite and oxygen.
The process according to claim 1, wherein the subsequent stage contains a combination of hypochlorite and peroxide.
The process according to claim 14, wherein the temperature is between 20Â° and 140Â° C. in the subsequent stage.
The process according to claim 19, wherein no cellulose protecting additives are used.
The process according to claim 19, wherein the cellulose protecting additives used are MgSO 4 or urea.
The process according to claim 19, whereby no peroxide stabilizers are used.
The process according to claim 19, wherein the peroxide stabilizers used are DTPA, HEDTA, DTPMPA and silicates.
The process according to claim 14, wherein the retention time is 1 second to 24 hours.
The process according to claim 14, wherein the consistency is between 5 and 30%.
The process according to claim 14, wherein the pressure in the subsequent stage is between 0.1 MPa and 2 MPa.
The process according to claim 14, wherein no intermediate washing is carried out between the peroxomonosulfuric acid treatment and the subsequent oxygen or peroxide or oxygen and peroxide treatment.
The process according to claim 1, wherein one or more intermediate washing steps are carried out between the peroxomonosulfuric acid treatment and the subsequent oxygen or peroxide or oxygen and peroxide treatment.
The process according to claim 28, wherein fresh water is used as dilution or wash water or dilution and wash water.
The process according to claim 28, wherein the filtrate of the subsequent oxygen or peroxide or oxygen and peroxide stage is used as dilution or wash water or dilution and wash water, in the one or more intermediate washing steps.