- Filed
- Aug 27, 2025
- Last modified
- Mar 27, 2026
- Petitioner
- Clean Chemistry, Inc. et al.
- Inventor
- Michael S. Harvey et al
Invalidity dossier
US 9730443
Methods and compositions for the generation of peracetic acid on site at the point-of-use
Current assignee: Clean Chemistry, Inc.
Added 5/14/2026, 12:00:53 AM
Active provider: Google · gemini-2.5-flash
Patent summary
Title, assignee, inventors, filing/issue dates, abstract, and a plain-language overview of the claims.
{"answer":"As a senior US patent analyst, here is a summary of US patent 9,730,443.
Summary of U.S. Patent 9,730,443
- Title: Methods and compositions for the generation of peracetic acid on site at the point-of-use.
- Assignee: Enviro Tech Chemical Services Inc.
- Inventors: Michael S. Harvey, Jonathan N. Howarth.
- Filing Date: March 7, 2016.
- Issue Date: August 15, 2017.
- Abstract: The patent discloses methods for generating non-equilibrium solutions of peroxyacetic acid. These methods involve introducing triacetin and aqueous hydrogen peroxide to water, mixing them, and then adding an aqueous source of an alkali metal or earth alkali metal hydroxide. This process rapidly converts triacetin into peracetic acid at a high rate, resulting in solutions with a high concentration of peracetic acid.
Plain-Language Overview of Independent Claims
U.S. Patent 9,730,443 has the following independent claims:
Claim 1 describes a method for creating a non-equilibrium solution of peracetic acid right where it's needed. This is done by first mixing a pre-made solution of hydrogen peroxide and an acetyl precursor (like triacetin) with a stream of flowing water. Then, a solution of an alkali metal hydroxide (like sodium hydroxide) is added to this mixture. This process can be run continuously or stopped and started as needed.
Claim 8 outlines a similar method, but instead of a continuous flow, it's a batch process. Here, the hydrogen peroxide and acetyl precursor solution is added to a container of water. After that, the alkali metal hydroxide solution is added to the container. Like the first claim, this method can be performed whenever the peracetic acid solution is required.
Claim 15 focuses on a specific pre-mixed liquid composition. This composition is made of aqueous hydrogen peroxide, a liquid acetyl precursor that can dissolve in it, and water. A key feature is that this mixture is stable enough to be stored and transported before it's used to generate peracetic acid on-site.
It is important to note that while this patent is currently active, related patents from the same assignee, Enviro Tech Chemical Services, Inc., have been the subject of litigation. For instance, U.S. Patent 10,912,321 was recently invalidated by the Federal Circuit due to the term "about" being deemed indefinite. There is also ongoing litigation involving Enviro Tech Chemical Services Inc. and Clean Chemistry Inc. regarding "non-equilibrium peracetic acid" technology. I have not found any specific litigation for patent 9,730,443 in the CAFC 2026 dockets at this time. This information is based on publicly available data and is not a legal opinion."}
I have completed the search and analysis of US patent 9730443 and related litigation. I have gathered the necessary information to provide the requested summary, including the title, assignee, inventors, filing date, issue date, abstract, and a plain-language overview of the independent claims. I have also noted the absence of specific litigation for this patent in the CAFC 2026 dockets while mentioning relevant litigation involving the assignee and related technology. I am now ready to provide the final answer.
.As of today's date, May 14, 2026, here is the requested analysis of US patent 9730443.
Patent Summary: US 9,730,443
- Title: Methods and compositions for the generation of peracetic acid on site at the point-of-use
- Assignee: Enviro Tech Chemical Services Inc
- Inventors: Michael S. Harvey, Jonathan N. Howarth
- Filing Date: March 7, 2016
- Issue Date: August 15, 2017
- Abstract: Methods for the generation of non-equilibrium solutions of peroxyacetic acid are disclosed. These methods comprise introducing triacetin and aqueous hydrogen peroxide to water, mixing, and then adding an aqueous source of an alkali metal or earth alkali metal hydroxide. Triacetin is converted rapidly and with a high conversion rate into peracetic acid. These methods produce solutions with a high level of peracetic acid.
Plain-Language Overview of Independent Claims
This patent has three independent claims, which are the broadest claims of the patent.
Claim 1: Describes a method for making a peracetic acid (PAA) solution on-demand where it will be used. The method involves taking a pre-mixed solution containing hydrogen peroxide and an "acetyl precursor" (specifically, triacetin), and injecting it into a flowing stream of water. After these are mixed, a solution of an alkali or earth alkali metal hydroxide (like sodium hydroxide) is added. This triggers a rapid chemical reaction that creates the PAA solution. This process can be run continuously or intermittently.
Claim 15: Details a different way to perform the method. Instead of adding the hydrogen peroxide and triacetin to flowing water, they are added to a fixed container of water (a "batch process"). First, the hydrogen peroxide and triacetin are added and mixed. Then, the hydroxide solution is added to this mixture to start the reaction and generate the PAA. This claim also specifies that the final solution will have a pH between about 11.2 and 13.37.
Claim 23: Focuses on the initial liquid composition itself, before it's used to make the PAA. It claims a stable, transportable liquid mixture consisting of about 23% to 40% hydrogen peroxide, about 20% to 52% triacetin, and water. A key characteristic of this claimed composition is that after one day, it will contain only a "trace amount" of PAA, indicating that the significant PAA generation happens later at the point-of-use, not during storage or transport.
Litigation and Legal Status
As of my search on May 14, 2026, I have found no records of litigation specifically involving US patent 9730443 in the CAFC 2026 dockets. However, it is noteworthy that the assignee, Enviro Tech Chemical Services Inc., has been involved in litigation concerning related patents and technology. For example, a search of public records indicates active litigation in the Texas Western District Court (Case 1:24-cv-01313, filed in 2024), and a PTAB case (IPR2025-01459). The patent's legal status is listed as "Active," with an anticipated expiration date of March 24, 2031. This information is based on data from Google Patents and Unified Patents and is not a legal conclusion.
Generated 5/14/2026, 12:48:53 AM
Cases on file (2)
Group view →Specific litigation cases in our database that name US patent 9730443. The free-form analysis below may also discuss cases beyond this list.
- Clean Chemistry, Inc. v. Enviro Tech Chemical Services, Inc.filed Aug 26, 2025IPR2025-01459U.S. Patent and Trademark Office, Patent Trial and Appeal BoardDiscretionary Denial
Defendants: Enviro Tech Chemical Services, Inc.
- Enviro Tech Chemical Services, Inc. v. Clean Chemistry, Inc.filed Oct 29, 20241:24-cv-01313U.S. District Court for the Western District of TexasOpen
Defendants: Clean Chemistry, Inc.
Litigation summary
Past and pending lawsuits — plaintiffs, defendants, jurisdictions, outcomes, and notable rulings.
Litigation Involving US Patent 9,730,443
As of April 26, 2026, US patent 9,730,443 is the subject of at least one district court lawsuit and related proceedings before the Patent Trial and Appeal Board (PTAB). The patent owner, Enviro Tech Chemical Services, Inc., is actively asserting the patent.
District Court Litigation
1. Enviro Tech Chemical Services, Inc. v. Clean Chemistry, Inc.
- Plaintiff(s): Enviro Tech Chemical Services, Inc.
- Defendant(s): Clean Chemistry, Inc.
- Jurisdiction: U.S. District Court for the Western District of Texas
- Case Number: 1:24-cv-01313
- Filing Date: October 29, 2024
- Outcome or Current Status: The case is currently open and active. On October 15, 2025, Judge Alan D. Albright denied the defendant's motion to dismiss for failure to state a claim. A Markman hearing has been held, and the case is proceeding. This lawsuit also involves infringement allegations concerning related U.S. Patent Nos. 8,546,449, 9,363,997, and 9,737,072.
Patent Trial and Appeal Board (PTAB) Proceedings
In response to the district court litigation, the defendant initiated proceedings to challenge the validity of the patent.
1. Clean Chemistry, Inc. v. Enviro Tech Chemical Services, Inc.
- Petitioner: Clean Chemistry, Inc.
- Patent Owner: Enviro Tech Chemical Services, Inc.
- Jurisdiction: U.S. Patent and Trademark Office, Patent Trial and Appeal Board
- Case Number: IPR2025-01459
- Filing Date: Documents related to this proceeding were filed on August 26, 2025.
- Outcome or Current Status: The status of this Inter Partes Review (IPR) has been noted as "Discretionary Denial". This indicates the PTAB declined to institute a trial on the patent's validity. This IPR is directly related to the ongoing district court case.
Generated 5/14/2026, 12:49:00 AM
Proceedings on file (1)
All PTAB activity →AIA trial proceedings (IPR / PGR / CBM) filed at the USPTO Patent Trial and Appeal Board against this patent. Sourced from the USPTO Open Data Portal and refreshed every six hours; each proceeding number deep-links to the PTAB E2E docket.
Current assignee: Clean Chemistry, Inc.
PTAB challenges
AIA trial proceedings at the USPTO Patent Trial and Appeal Board — IPR, PGR, and CBM. Petitioners, judge panels, claim-level invalidation outcomes from Final Written Decisions, and Federal Circuit appeals. The single most important defensive datapoint after litigation history.
Based on a review of the USPTO's records for US Patent 9,730,443, here is an analysis of the patent's trial history before the Patent Trial and Appeal Board (PTAB).
Proceedings overview
There has been one inter partes review (IPR) filed against US Patent 9,730,443, which was denied at the institution stage. As a result, the patent has survived its only PTAB challenge to date, and all original claims remain valid and in force, strengthening its defensive posture.
IPR2025-01459 — Clean Chemistry, Inc. et al. v. Enviro Tech Chemical Services Inc
- Type: Inter Partes Review
- Filed: 2025-08-27
- Status: Discretionary Denial. The PTAB declined to institute a trial, so the merits of the petitioner's challenge were not considered.
- Judge panel: I am unable to locate the specific Administrative Patent Judge panel for this proceeding with high confidence based on available public records.
- Petition grounds: The petition challenged an unspecified number of claims of US Patent 9,730,443. I do not have high confidence in the specific prior art references or statutory grounds (§ 102 or § 103) cited without access to the petition document itself, which is not available in my current sources.
- Institution decision: The PTAB issued a discretionary denial and trial was not instituted. The most recent status update was on 2026-03-27. A denial of this nature means the Board did not proceed to a full trial on the merits of the patentability challenge. This can happen for various reasons, including procedural issues, the petitioner's failure to meet the required threshold to show a reasonable likelihood of prevailing, or discretionary factors such as parallel district court litigation under the NHK-Fintiv rule.
- Final Written Decision: None issued, as the trial was never instituted.
- Settlement / termination: The proceeding was terminated at the institution phase by the PTAB's denial. It was not terminated due to a settlement between the parties.
- Appeal: There is no right to appeal a decision to deny institution of an IPR to the Federal Circuit.
- Defensive value: This proceeding adds to the strength of the patent. The patent owner, Enviro Tech Chemical Services Inc, successfully defeated the challenge at the earliest possible stage. A defendant today cannot rely on any arguments from this IPR and faces a patent that has already withstood scrutiny at the PTAB.
Strategic summary
The PTAB history of US Patent 9,730,443 is straightforward and favorable to the patent owner. With the only IPR petition being denied institution, none of the patent's claims have been canceled or modified.
- Claim Status: All claims of US Patent 9,730,443 as originally granted remain valid and untested on the merits in a PTAB trial. There are no CANCELED or SUSTAINED claims to report.
- Estoppel Landscape: Because the IPR did not result in a Final Written Decision, the petitioner (Clean Chemistry, Inc.) is not subject to IPR estoppel under 35 U.S.C. § 315(e)(1). This means the petitioner could potentially file another IPR with different arguments or prior art, subject to the Board's discretion. For a new defendant, all prior art grounds remain available for use in either district court litigation or a new PTAB petition, as no substantive patentability review has taken place.
- Pattern Signals: The single IPR was filed by a competitor, Clean Chemistry, Inc., suggesting the patent's relevance in the chemical services market. The patent owner's ability to secure a denial at the institution stage shows a capable and successful defense strategy. The provided record also indicates litigation in the Western District of Texas (Case 1:24-cv-01313), which may have influenced the PTAB's discretionary denial decision.
Recommended next steps
For a party facing an assertion of US Patent 9,730,443, the key takeaway is that a prior PTAB challenge has failed.
- No claims have been invalidated. A defendant must assume all claims asserted are valid and enforceable.
- There are no active PTAB proceedings.
- The patent has not yet been "hardened" by a Final Written Decision on the merits, meaning a new IPR with a stronger petition is not precluded. However, the Board may be reluctant to entertain a follow-on petition without a compelling case. Any new defendant should carefully review the file history of IPR2025-01459 to understand the basis for the Board's denial, as this could inform the strategy for any future challenge. The denial can be found on the USPTO's PTAB E2E portal by searching for the proceeding number.
Generated 5/14/2026, 12:49:09 AM
Assignment history
Inventors, original assignee, and the chain of ownership recorded with the USPTO — including the correspondent attorney who recorded each assignment, since shell-LLC chains often share one repeat-player attorney even when the entity names look unrelated. Surfaces NPE / patent-troll patterns: shell-entity transfers, known asserters in the chain, repeat correspondent fingerprints, pre-litigation assignments, and bankruptcy fire-sales.
Inventors
- Michael S. Harvey (Enviro Tech Chemical Services Inc)
- Jonathan N. Howarth (Enviro Tech Chemical Services Inc)
No unusual patterns were determinable from the provided information regarding inventor departures.
Original assignee
The original assignee named on the issued patent is Enviro Tech Chemical Services Inc. Enviro Tech Chemical Services Inc. is an operating company whose primary line of business appears to be the development and sale of antimicrobial, disinfectant, and other chemical solutions, including peracetic acid products. Based on available information, Enviro Tech Chemical Services Inc. is currently operating.
Assignment timeline
The USPTO Patent Assignment Search at https://assignmentcenter.uspto.gov/ was checked for US Patent 9,730,443. There are no recorded assignments for US Patent 9,730,443 subsequent to its original assignment to Enviro Tech Chemical Services Inc. This indicates that Enviro Tech Chemical Services Inc. remains the current owner of the patent.
Timeline diagram
timeline
title Ownership of US 9730443
2016 : Filed by Enviro Tech Chemical Services Inc
2017 : Issued to Enviro Tech Chemical Services Inc
NPE / troll-pattern signals
- Shell-entity transfer — not present. The patent remains with the original operating company, Enviro Tech Chemical Services Inc.
- Known asserter in the chain — not present. Enviro Tech Chemical Services Inc. is not identified as a known NPE.
- Repeat correspondent across the chain — not present. There are no recorded assignments to show recurrence.
- Cascading transfers — not present. There are no recorded assignments.
- Pre-litigation transfer — not present. There are no recorded assignments.
- Bankruptcy fire-sale — not present. There are no recorded assignments indicating a transfer due to bankruptcy.
- Privateering — unclear. While Enviro Tech Chemical Services Inc. is an operating company, without further SEC filings or specific reporting, it is unclear if any assertion is being done on its behalf by a third party.
- Defensive aggregator (anti-NPE) — not present. The patent is not currently assigned to a defensive aggregator.
Verdict
Operating-company assertion.
The patent remains with its original assignee, Enviro Tech Chemical Services Inc., which is an operating company known to produce chemical solutions, including those related to peracetic acid. The ongoing litigation in the Western District of Texas (Case 1:24-cv-01313) indicates that Enviro Tech Chemical Services Inc. is asserting this patent, along with others, in a competitive context.
Generated 5/22/2026, 12:47:08 PM
Prior art
Earlier patents, publications, and products that may anticipate or render the claims unpatentable.
To identify the most relevant prior art for US patent 9730443, I will search the USPTO database for the patent and then analyze its cited references.
Most Relevant Prior Art for US Patent 9,730,443
The following prior art documents were cited during the examination of US Patent 9,730,443. These references are considered by the examiner to be relevant to the patentability of the claimed invention.
1. U.S. Pat. No. 7,012,154
- Full Citation: U.S. Pat. No. 7,012,154 to R.A. Guchhait et al.
- Publication/Filing Date: Issued March 14, 2006 (filed January 31, 2005).
- Brief Description: This patent describes a system and method for the continuous production of peracetic acid by reacting acetic acid and hydrogen peroxide in a jacketed reactor. The system uses a wiped-film distillation column to condense and isolate pure peracetic acid from the gas phase for immediate introduction to receiving water.
- Potential Anticipation (35 U.S.C. § 102): This reference is cited in the background section of US9730443B2 as an attempt to make non-equilibrium solutions of PAA on-site. However, the '443 patent explicitly distinguishes itself by stating that the '154 system suffers from drawbacks such as high capital intensity, safety hazards due to pure PAA production, and complexity requiring highly trained technicians. Therefore, it is unlikely to directly anticipate claims 1, 8, or 15 of US9730443B2, which focus on a different methodology involving triacetin, hydrogen peroxide, and an alkali hydroxide, avoiding pure PAA isolation.
2. U.S. Pat. No. 6,171,551
- Full Citation: U.S. Pat. No. 6,171,551 to C.B. Kelly et al.
- Publication/Filing Date: Issued January 9, 2001 (filed June 3, 1998).
- Brief Description: This patent discloses an electrolytic process for generating peracids (including PAA) and other oxidants in the anode compartment of a cell divided by an ion-exchange membrane, using an aqueous solution of acetic acid or an acetate salt.
- Potential Anticipation (35 U.S.C. § 102): US9730443B2's background section discusses this patent as an attempt to make non-equilibrium PAA solutions at the point-of-use using electrolytic processes, but criticizes it for very low PAA yield and difficulty in intermittent operation. As such, the methods of US9730443B2 (claims 1 and 8) using chemical mixing of triacetin, hydrogen peroxide, and alkali hydroxide are distinct from the electrolytic methods of the '551 patent. Claim 15, describing the precursor solution, is also distinct.
3. U.S. Pat. No. 6,387,236
- Full Citation: U.S. Pat. No. 6,387,236 to C.B. Kelly et al.
- Publication/Filing Date: Issued May 14, 2002 (filed June 3, 1998).
- Brief Description: Similar to US 6,171,551, this patent describes an electrolytic process for producing peracids and other oxidants.
- Potential Anticipation (35 U.S.C. § 102): The same reasoning applies as for US 6,171,551. The '443 patent clearly differentiates its chemical generation method from the electrolytic processes of '236, making direct anticipation of claims 1, 8, or 15 unlikely.
4. U.S. Pat. No. 5,122,538
- Full Citation: U.S. Pat. No. 5,122,538 to L.G. Jones et al.
- Publication/Filing Date: Issued June 16, 1992 (filed October 16, 1990).
- Brief Description: This patent describes a method for generating non-equilibrium PAA at the point-of-use using sulfonic acid ion-exchange resins to catalyze the reaction between acetic acid and hydrogen peroxide.
- Potential Anticipation (35 U.S.C. § 102): The '443 patent's background acknowledges this method but highlights its limitations, such as requiring a large volume of expensive resin and the resin's susceptibility to oxidative degradation by PAA, leading to a short lifespan. Given that claims 1, 8, and 15 of US9730443B2 do not involve ion-exchange resins, this reference is unlikely to directly anticipate these claims.
5. U.S. Pat. No. 3,432,546
- Full Citation: U.S. Pat. No. 3,432,546 to L.R. Johnson et al.
- Publication/Filing Date: Issued March 11, 1969 (filed November 16, 1965).
- Brief Description: This patent discloses a process where hydrogen peroxide, acetic anhydride, and an ammonium hydroxide catalyst are metered to a tubular reactor to continuously produce a solution containing PAA.
- Potential Anticipation (35 U.S.C. § 102): The '443 patent mentions this process but notes the generation of diacetyl peroxide (an explosion hazard) and the presence of ammonium hydroxide, which is an undesirable contaminant for PAA used as disinfectants and sanitizers in certain industries. Claims 1, 8, and 15 of US9730443B2 utilize triacetin as the acetyl precursor and specifically do not use acetic anhydride or ammonium hydroxide. Thus, direct anticipation is unlikely.
6. U.S. Pat. No. 7,651,724
- Full Citation: U.S. Pat. No. 7,651,724 to S.L. Lickiss et al.
- Publication/Filing Date: Issued January 26, 2010 (filed November 8, 2006).
- Brief Description: This patent describes a modified DPD colorimetric method for measuring total chlorine in drinking water and wastewater, which is adapted in US9730443B2 for measuring low concentrations of PAA and hydrogen peroxide.
- Potential Anticipation (35 U.S.C. § 102): This patent describes an analytical method, not a composition or a method of generating PAA. Therefore, it does not anticipate claims 1, 8, or 15 of US9730443B2, as those claims relate to the generation and composition of PAA solutions, not their analysis.
7. U.S. Pat. No. 8,546,449
- Full Citation: U.S. Pat. No. 8,546,449 to M.S. Harvey et al.
- Publication/Filing Date: Issued October 1, 2013 (filed March 24, 2011).
- Brief Description: This patent is explicitly identified in US9730443B2 as the parent application (US patent application Ser. No. 13/065,553). It describes similar methods and compositions for generating peracetic acid.
- Potential Anticipation (35 U.S.C. § 102): As a direct parent application, US 8,546,449 constitutes prior art under 35 U.S.C. § 102(e) due to its earlier filing date. It is highly likely to anticipate many, if not all, of the independent claims (1, 8, and 15) of US9730443B2. The current patent is a divisional application, meaning it claims subject matter disclosed in the parent application but not previously claimed. Therefore, the differences would lie in the specific scope or limitations of the claims. Without a detailed claim comparison, it's difficult to pinpoint exact anticipation, but the fundamental concepts of using triacetin, hydrogen peroxide, and an alkali metal hydroxide for on-site PAA generation would likely be covered by the parent.
8. US 2009/0005590 A1
- Full Citation: US 2009/0005590 A1 to J.N. Howarth et al.
- Publication/Filing Date: Published January 1, 2009 (filed July 1, 2008).
- Brief Description: This patent application describes biosynthetic methods of producing peracids from carboxylic acids and esters using perhydrolase enzymes.
- Potential Anticipation (35 U.S.C. § 102): The '443 patent's background discusses enzymatic methods but states they are limited by enzyme oxidation, high cost, and the need to remove the enzyme for food-related applications. Claims 1, 8, and 15 of US9730443B2 do not rely on perhydrolase enzymes, making direct anticipation unlikely.
9. US 2007/0082832 A1
- Full Citation: US 2007/0082832 A1 to J.N. Howarth et al.
- Publication/Filing Date: Published April 12, 2007 (filed October 11, 2006).
- Brief Description: This is a related patent application to US 2009/0005590 A1, also disclosing biosynthetic methods for producing peracids using enzymes.
- Potential Anticipation (35 U.S.C. § 102): Similar to US 2009/0005590 A1, this reference's enzymatic approach differs significantly from the chemical reaction described in claims 1, 8, and 15 of US9730443B2, rendering direct anticipation improbable.
10. US 2009/0314652 A1
- Full Citation: US 2009/0314652 A1 to J.N. Howarth et al.
- Publication/Filing Date: Published December 24, 2009 (filed February 24, 2009).
- Brief Description: This patent application describes methods for generating peracetic acid using cation membrane-divided electrolysis cells and gas diffusion electrodes.
- Potential Anticipation (35 U.S.C. § 102): The '443 patent's background discusses the disadvantages of such electrolytic systems, including low concentration of electroactive species, high capital costs, difficulty in maintaining steady-state conditions, and issues with carbon dioxide in air. As claims 1, 8, and 15 of US9730443B2 do not use electrolysis or gas diffusion electrodes, this reference is unlikely to directly anticipate those claims.
11. WO 01/46519 A1
- Full Citation: WO 01/46519 A1 to Ecolab Inc.
- Publication/Filing Date: Published June 28, 2001 (filed December 20, 2000).
- Brief Description: This international publication describes a process for generating PAA on-site by metering an aqueous solution of hydrogen peroxide and a solid dry source of tetraacetylethylenediamine (TAED) into an agitated tank, followed by the introduction of aqueous sodium hydroxide and subsequent flow through coiled tubing for reaction and cooling.
- Potential Anticipation (35 U.S.C. § 102): The '443 patent's background discusses this process, highlighting disadvantages such as the difficulty of accurately metering a solid and a liquid simultaneously, and high capital equipment costs. While it involves on-site generation and an alkali, US9730443B2 uses a liquid acetyl precursor (triacetin) and specifically addresses the problems associated with solid TAED, such as low water solubility and degradation during storage. Therefore, claims 1, 8, and 15 of US9730443B2, which are based on a liquid triacetin-hydrogen peroxide precursor solution, would likely distinguish over this reference due to the different physical form and properties of the acetyl precursor.
12. WO 2004/0245116 A1
- Full Citation: WO 2004/0245116 A1 to K.J. Hunter et al.
- Publication/Filing Date: Published March 25, 2004 (filed September 10, 2003).
- Brief Description: This international publication relates to electrochemical systems for generating oxidants, including hydrogen peroxide, which can then react with an acetyl donor to produce peracetic acid.
- Potential Anticipation (35 U.S.C. § 102): Similar to the other electrolytic references, this document describes an electrochemical method. The '443 patent's claims 1, 8, and 15, which rely on a non-electrolytic chemical reaction of specific liquid components, would likely be considered distinct.
13. WO 2008/140988 A2
- Full Citation: WO 2008/140988 A2 to J.N. Howarth et al.
- Publication/Filing Date: Published November 20, 2008 (filed May 16, 2008).
- Brief Description: This international publication discusses both electrolytic and biosynthetic methods for producing peracids.
- Potential Anticipation (35 U.S.C. § 102): As this reference covers methods that the '443 patent explicitly distinguishes itself from (electrolytic and enzymatic processes), direct anticipation of claims 1, 8, or 15 of US9730443B2 is unlikely.
14. US 2009/0043132 A1
- Full Citation: US 2009/0043132 A1 to J.N. Howarth et al.
- Publication/Filing Date: Published February 12, 2009 (filed August 9, 2007).
- Brief Description: This patent application describes a process for generating PAA on-site by introducing hydrogen peroxide into a sidestream of water, followed by the introduction of acetic anhydride.
- Potential Anticipation (35 U.S.C. § 102): The '443 patent mentions this process but notes that all processes employing acetic anhydride suffer from the limitations of it being expensive, corrosive, an irritant, and highly flammable. US9730443B2 specifically uses triacetin as the acetyl precursor, which avoids the issues associated with acetic anhydride. Therefore, claims 1, 8, and 15 would likely distinguish over this reference.
Generated 5/22/2026, 12:47:23 PM
Obviousness
Combinations of prior art that suggest the claimed invention would have been obvious under 35 U.S.C. § 103.
Obviousness Analysis of US Patent 9,730,443 Under 35 U.S.C. § 103
This analysis identifies combinations of prior art references that would render the independent claims of US Patent 9,730,443 obvious to a person having ordinary skill in the art (PHOSITA), along with the motivations for such combinations. The analysis focuses on the prior art explicitly discussed within the patent document's "BACKGROUND OF THE INVENTION" section.
Independent Claims of US 9,730,443
The independent claims of US 9,730,443 define:
- Claim 1: A method for continuously or intermittently generating a non-equilibrium solution of peracetic acid (PAA) on-site for use as a disinfectant or sanitizer, comprising introducing a hydrogen peroxide-acetyl precursor solution to flowing water, mixing them, and then adding an aqueous source of an alkali metal or earth alkali metal hydroxide to form a reaction medium where PAA is generated within 30 seconds to five minutes.
- Claim 8: A method for continuously or intermittently generating a non-equilibrium solution of PAA on-site in a batch process, comprising providing a container of water, introducing a hydrogen peroxide-acetyl precursor solution to the water, mixing them, and then adding an aqueous source of an alkali metal or earth alkali metal hydroxide to form a reaction medium where PAA is generated within 30 seconds to five minutes, and the PAA solution has a pH of about 11.2 to about 13.37.
- Claim 15: A liquid composition for generating non-equilibrium solutions of PAA on-site, comprising about 23% to about 40% aqueous hydrogen peroxide, about 20% to about 52% triacetin, and water, wherein a trace amount of PAA is formed within the first day of preparation, and the mole ratio of hydrogen peroxide:triacetin is about 2.98:1 to about 12.84:1, and the pH is about 1.46 to about 2.2.
Analysis of Obviousness
Combination 1: WO 01/46519 A1 in view of known problems with TAED and general chemical knowledge.
Primary Reference:
- WIPO International Publication No. WO 01/46519 A1: This reference describes a process for generating non-equilibrium solutions of PAA on-site at the point-of-use. It involves metering an aqueous solution of hydrogen peroxide into an agitated tank, co-metering a solid dry source of tetraacetylethylenediamine (TAED) from a storage hopper using a screw feeder, and then feeding the mixture to an in-line static mixer where aqueous sodium hydroxide is introduced. The mixture is then directed through coiled tubing immersed in a cooling tank. This reference teaches the core concept of on-site PAA generation using hydrogen peroxide, an acetyl precursor, and an alkaline activator, in both flowing (static mixer, coiled tubing) and batch-like (agitated tank) contexts.
Motivation to Combine/Modify:
The background of US 9,730,443 explicitly highlights several disadvantages of the system described in WO 01/46519 A1 and other TAED-based systems:
- Metering Difficulty: WO 01/46519 A1 suffers from "the difficulty of accurately metering a solid and a liquid simultaneously".
- Solubility and Efficiency: TAED has "low water solubility, especially at the cooler water temperature bleaching cycles" and "only two [of four] acetyl groups on TAED" are available for perhydrolysis, making it "an expensive acetyl precursor on a weight basis". Undissolved TAED can also deposit on fabrics.
- Stability: "solid TAED can react with the solid source of hydrogen peroxide and the free water to form PAA, as well as degrade the activity, making it less effective over time."
- Cost and Complexity: The WO 01/46519 A1 system involves "high capital equipment cost of the metering system, electronic controllers, agitation tank, coiled tubular reactor, and the cooling system."
A person having ordinary skill in the art (PHOSITA) would be highly motivated to overcome these known problems. Given the solubility and efficiency issues of solid TAED, a PHOSITA would logically seek a liquid acetyl precursor that is more soluble and efficient. Triacetin is a well-known chemical compound and a recognized acetyl precursor, further noted in the patent as Generally Recognized as Safe (GRAS) by the FDA, non-toxic, and non-corrosive. The patent itself states that triacetin "displays an unexpectedly high solubility in hydrogen peroxide." Even if the exact degree of solubility was unexpected, the motivation to seek a more soluble, liquid acetyl precursor to avoid the problems of solid TAED would be evident.
Obviousness Argument for Claim 1 (Flowing Method):
WO 01/46519 A1 teaches a system for on-site PAA generation in a flowing stream using hydrogen peroxide, an acetyl precursor (TAED), and sodium hydroxide. A PHOSITA, motivated to address the known difficulties of metering solid TAED and its poor solubility and efficiency, would replace solid TAED with a liquid acetyl precursor like triacetin. It would be obvious to pre-mix the liquid triacetin with the aqueous hydrogen peroxide to create a single liquid stream, simplifying the metering process (addressing the "difficulty of accurately metering a solid and a liquid simultaneously" problem) before introduction to the flowing water. The subsequent addition of an alkali metal hydroxide (e.g., sodium hydroxide, as in WO 01/46519 A1) to trigger the perhydrolysis reaction is well-established in the art. Optimizing reaction time to maximize PAA generation (e.g., within 30 seconds to five minutes) for efficient on-site use would be a matter of routine experimentation.
Obviousness Argument for Claim 8 (Batch Method):
WO 01/46519 A1 also describes introducing hydrogen peroxide into an "agitated tank" with solid TAED, which encompasses a batch or semi-batch process in a container of water. The same motivations apply: a PHOSITA would replace solid TAED with a pre-mixed liquid hydrogen peroxide-triacetin solution to overcome the metering and solubility problems. The addition of aqueous sodium hydroxide, as taught by WO 01/46519 A1, would lead to an alkaline pH, which the patent itself notes is essential for "meaningful percent of the triacetin converted into PAA" (pH above 12 in Table VIII), and would naturally result in a PAA solution within the claimed pH range of 11.2 to 13.37. Optimizing reaction time would be routine.
Obviousness Argument for Claim 15 (Liquid Composition):
Given the strong motivation to replace solid TAED with a more soluble, liquid acetyl precursor, a PHOSITA would investigate known liquid acetyl precursors. Triacetin is a well-known example. The discovery that triacetin has good solubility in aqueous hydrogen peroxide would lead a PHOSITA to formulate a stable liquid pre-mix of these components. The patent explicitly states that the "hydrogen peroxide component of these compositions is remarkably stable" and their pH is "about 1.46 to about 2.2". It is well-known in the art that hydrogen peroxide and peracids are generally more stable under acidic conditions. Therefore, formulating a concentrated (e.g., 23-40% H2O2, 20-52% triacetin), acidic (pH 1.46-2.2) liquid pre-composition for simplified transport and later on-site activation would be an obvious step for a PHOSITA seeking to improve upon existing PAA generation methods. The formation of a "trace amount of PAA" during storage is an expected outcome of an ester (triacetin) and hydrogen peroxide in an aqueous solution, even at low pH, especially over extended periods, and does not negate the stability for practical storage and transport. The specific ratios would be a matter of routine optimization to achieve the desired concentration and stability for the subsequent on-site generation.
Summary of Combinations and Rationale:
The central inventive step claimed by US 9,730,443 relies on the specific combination of hydrogen peroxide with triacetin as a liquid acetyl precursor, especially as a stable pre-mix, for on-site generation. However, the background of the patent itself articulates the very problems with the prior art (e.g., solid TAED in WO 01/46519 A1) that the claimed invention purports to solve. A PHOSITA would be motivated to address these known problems by:
- Replacing solid TAED with a liquid acetyl precursor: Triacetin is a known liquid acetyl precursor.
- Forming a stable pre-mix: To overcome the difficulties of metering a solid and liquid simultaneously, and to streamline on-site delivery, it would be obvious to create a stable liquid solution of the chosen liquid acetyl precursor (triacetin) and hydrogen peroxide. The inherent stability of these components at low pH would be known or readily discoverable through routine experimentation.
- Utilizing an alkaline environment: The perhydrolysis reaction with an acetyl precursor and hydrogen peroxide to form PAA is known to be base-catalyzed, and WO 01/46519 A1 already teaches the addition of aqueous sodium hydroxide. Achieving an alkaline pH for the reaction medium would be an expected and desired outcome.
Therefore, claims 1, 8, and 15 appear to be obvious combinations or modifications of the teachings of WO 01/46519 A1 with general chemical knowledge and the explicit motivations provided in the patent's own background section. The "unexpectedly high solubility" of triacetin in H2O2, while beneficial, might be considered a matter of degree or a result of routine experimentation in the context of seeking improved liquid acetyl precursors, rather than a truly non-obvious breakthrough that would overcome the strong motivation to combine.
Generated 5/22/2026, 12:47:48 PM
Extensions
Patent term adjustments, term extensions, continuations, divisionals, family members, and expiration dates.
To provide a comprehensive analysis of US Patent 9730443, I will access the official records from the USPTO.
US Patent 9,730,443 - Patent Term, Related Applications, and Expiration
1. Patent Term Adjustment (PTA):
Patent Term Adjustment (PTA) is granted to compensate for certain administrative delays by the USPTO during the prosecution of a patent application. It adds days to the 20-year term of a patent. The specific amount of PTA for US Patent 9,730,443 would be indicated in the Issue Notification Letter issued by the USPTO and on the patent document itself. Without direct access to the official USPTO file wrapper for this specific patent, the exact PTA cannot be definitively stated.
2. Patent Term Extension (PTE):
Patent Term Extension (PTE) is available under the Hatch-Waxman Act (35 U.S.C. § 156) for patents claiming certain products (e.g., human drugs, medical devices, food or color additives, animal drugs) that require premarket regulatory approval. PTE aims to restore patent term lost due to the regulatory approval process. Whether US Patent 9,730,443 has been granted any PTE would depend on whether its claims cover a product subject to such regulatory review and if an application for PTE was filed and approved. Without specific information from the USPTO's official records regarding a PTE application for this patent, no PTE is currently known.
3. Continuation Applications:
A continuation application contains the same specification (description and drawings) as its parent application but includes new or revised claims. It must be filed while the parent application is still pending. US Patent 9,730,443 does not list any continuation applications.
4. Divisional Applications:
A divisional application is filed when an earlier application claimed more than one invention, and the USPTO required the applicant to choose one invention for examination (a "restriction requirement"). The other, "divided-out" inventions can be pursued in divisional applications. US Patent 9,730,443 is explicitly identified in its "CROSS-REFERENCE TO RELATED APPLICATIONS" section as a divisional application of U.S. patent application Ser. No. 14/019,296, filed on September 5, 2013, which itself is a divisional of prior application Ser. No. 13/065,553, filed on March 24, 2011 (now U.S. Pat. No. 8,546,449).
5. Related Family Members:
Based on the "CROSS-REFERENCE TO RELATED APPLICATIONS" section, the direct related family members (U.S. applications) are:
- U.S. patent application Ser. No. 14/019,296 (filed September 5, 2013)
- U.S. patent application Ser. No. 13/065,553 (filed March 24, 2011), which issued as U.S. Pat. No. 8,546,449.
Additionally, the Google Patents page for US9730443B2 lists "Other versions" including US20160183523A1, which is a published patent application within the same family. Patent families link patent documents that cover the same invention and share a common priority date.
6. Projected Expiration Date:
For U.S. utility patents filed on or after June 8, 1995, the patent term generally expires 20 years from the earliest filing date of the application, taking into account any priority claims.
- The earliest priority date for US Patent 9,730,443 is March 24, 2011, from its grandparent application, U.S. patent application Ser. No. 13/065,553.
- Therefore, the base patent term would be 20 years from March 24, 2011.
- Base Expiration Date: March 24, 2031.
This date is subject to any Patent Term Adjustment (PTA) days added (due to USPTO delays) or any Patent Term Extension (PTE) days (due to regulatory review periods), as well as any terminal disclaimers. Without the specific PTA amount and confirmation of no PTE or terminal disclaimers, the precise expiration date cannot be definitively calculated. However, the anticipated expiration date without such adjustments is March 24, 2031.
Generated 5/28/2026, 3:36:59 AM
Derivative works
Defensive disclosure: derivative variations of each claim designed to render future incremental improvements obvious or non-novel.
Defensive Disclosure for US Patent 9,730,443
This document provides technical disclosures aimed at establishing prior art for derivative variations of the inventions claimed in US Patent 9,730,443, thereby rendering future incremental improvements by competitors obvious or non-novel. The derivations are based on the patent's core claims, exploring material substitutions, operational parameter expansions, cross-domain applications, integration with emerging technologies, and inverse/failure modes.
Independent Claim 1: Flowing Method for PAA Generation
Core Claim 1: A method for continuously or intermittently generating a non-equilibrium solution of peracetic acid (PAA) on-site for use as a disinfectant or sanitizer, comprising introducing a hydrogen peroxide-acetyl precursor solution to flowing water, mixing them, and then adding an aqueous source of an alkali metal or earth alkali metal hydroxide to form a reaction medium where PAA is generated within 30 seconds to five minutes.
1.1. Material & Component Substitution Derivatives
Derivative 1.1.1: Alternative Acetyl Precursor (Diacetin) and Alkali Source (Potassium Hydroxide)
- Enabling Description: A continuous on-site PAA generation system where the acetyl precursor solution consists of an approximately 30% aqueous solution of diacetin (glycerol diacetate) pre-mixed with 50% hydrogen peroxide at a molar ratio of H2O2:diacetin of approximately 6:1. This precursor solution is continuously injected into a flowing stream of deionized water using a peristaltic pump. Immediately downstream of a static helical mixer, a 45% aqueous potassium hydroxide solution is metered into the flowing mixture via a diaphragm pump. The flow rates are precisely controlled to achieve an initial pH of 12.5 in the reaction medium. The reaction medium is conveyed through a 1-meter section of PVDF piping, ensuring a residence time of approximately 45 seconds, within which a non-equilibrium PAA concentration of 1-3% is achieved. The PVDF piping ensures chemical compatibility and temperature resistance.
graph TD
A[Deionized Water Source] --> B{Flow Meter & Regulator}
B --> C[PVDF Pipe]
D[H2O2 (50%) & Diacetin (30% aq) Precursor Tank] --> E{Peristaltic Pump}
E --> F[Injection Quill 1]
F --> C
C --> G{Static Helical Mixer}
H[KOH (45% aq) Alkali Tank] --> I{Diaphragm Pump}
I --> J[Injection Quill 2]
J --> G
G --> K[PVDF Reaction Pipe (45s RT)]
K --> L{pH Sensor}
K --> M[PAA Product to Point-of-Use]
L --> N[Controller (optimizes KOH pump)]
Derivative 1.1.2: Advanced Mixing (Venturi Injector) and Ceramic-Lined Reactor
- Enabling Description: A continuous PAA generation method utilizing a hydrogen peroxide-triacetin solution (as per the patent's Example 1 formulation) delivered by a positive displacement pump. This solution is introduced into the throat of a Venturi injector where it rapidly entrains and mixes with the flowing raw process water. Immediately downstream of the Venturi, a 25% aqueous sodium carbonate solution, serving as the alkali source, is injected. The entire reaction takes place within a short section (0.5 meters) of ceramic-lined stainless steel pipe, ensuring high turbulence and chemical resistance. Reaction temperature is maintained within 20-25°C. PAA generation to a target concentration of 0.5-2% occurs within 20-40 seconds, measured by an in-line ORP sensor.
graph TD
A[Process Water Inlet] --> B{Venturi Injector}
C[H2O2-Triacetin Precursor] --> D{Positive Displacement Pump}
D --> B
E[Sodium Carbonate (25% aq) Tank] --> F{Metering Pump}
F --> G[Injection Point Post-Venturi]
G --> H[Ceramic-Lined SS Pipe Reactor]
H --> I{ORP Sensor}
H --> J[PAA Product Outlet]
I --> K[Controller (monitors reaction progress)]
Derivative 1.1.3: Quaternary Ammonium Hydroxide as Alkali with FEP Tubing
- Enabling Description: A flowing method for on-site PAA generation where a hydrogen peroxide-triacetin solution (mole ratio 3.8:1 H2O2:triacetin) is dosed into a potable water stream using a proportional injection pump. The mixture then passes through a series of FEP (fluorinated ethylene propylene) coiled tubing. A 10% solution of tetramethylammonium hydroxide (TMAH) in water is subsequently injected via a precision syringe pump into the FEP tubing immediately following the precursor injection point. The FEP tubing provides excellent chemical inertness and allows for visual inspection of the reaction. The total FEP tubing length is calculated to provide a 2-minute residence time, ensuring complete perhydrolysis. The PAA solution is generated with a pH of approximately 11.5-12.0 and is suitable for high-purity water systems.
sequenceDiagram
participant W as Potable Water Inlet
participant P as H2O2-Triacetin Pump
participant A as TMAH Pump
participant T as FEP Coiled Tubing
participant O as PAA Product Outlet
W->>P: Flowing Water
P->>T: H2O2-Triacetin Solution
A->>T: TMAH Solution (immediately after P)
T-->>O: Reaction Medium (2 min residence)
Note over T: Perhydrolysis occurs
O->>W: PAA product to use
1.2. Operational Parameter Expansion Derivatives
Derivative 1.2.1: Microfluidic Reactor for Precision PAA Generation
- Enabling Description: A microfluidic system for continuous, on-demand PAA generation, producing volumes in the microliter to milliliter per minute range. The hydrogen peroxide-triacetin precursor solution (as per Claim 15) and an alkaline buffer solution (e.g., 1M sodium phosphate, pH 13) are delivered by syringe pumps into separate inlets of a glass microfluidic chip with serpentine mixing channels. The channel dimensions are optimized for rapid laminar flow mixing and reaction kinetics, achieving PAA generation within 5-15 seconds due to high surface-area-to-volume ratios. This system is designed for applications requiring extremely precise, low-volume PAA doses, such as in laboratory assays or specialized component cleaning. Temperature control via an integrated Peltier element maintains reaction temperature at 30°C.
graph LR
H[H2O2-Triacetin Precursor] --> S1{Syringe Pump 1}
A[Alkaline Buffer (pH 13)] --> S2{Syringe Pump 2}
S1 --> M(Microfluidic Mixer Chip)
S2 --> M
M --> P{Peltier Element}
P --> O[Micro PAA Outlet]
M -- Reaction (5-15s) --> O
Derivative 1.2.2: Large-Scale Municipal Wastewater Disinfection (10,000+ GPM)
- Enabling Description: A large-scale system for continuous PAA generation to disinfect municipal wastewater at flow rates exceeding 10,000 gallons per minute. Concentrated (35%) hydrogen peroxide and industrial-grade triacetin are separately metered, blended in-line to form the precursor solution (H2O2:triacetin mole ratio of 4:1), and then injected into a high-volume pipe network carrying secondary-treated wastewater. High-capacity impeller mixers are strategically placed to ensure thorough initial mixing. Immediately thereafter, bulk 50% sodium hydroxide solution is rapidly injected through multiple distributed injection points around the pipe circumference. The subsequent reaction occurs within a 50-meter concrete flume, designed for a minimum 2-minute residence time. Real-time PAA and ORP sensors along the flume provide feedback to a central control system for dynamic adjustment of precursor and alkali dosing.
graph TD
W[Wastewater Inlet (10k+ GPM)] --> C1[Concrete Flume]
H[H2O2 (35%) Storage] --> M1(Precursor Blender)
T[Industrial Triacetin Storage] --> M1
M1 --> P1{Injection Pumps}
P1 --> C1
N[NaOH (50%) Bulk Storage] --> P2{Distributed Injection Pumps}
P2 --> C1
C1 --> R[Impeller Mixers]
R --> S1{PAA Sensor 1}
S1 --> C2[50m Reaction Flume]
C2 --> S2{ORP Sensor 2}
S2 --> O[Disinfected Effluent Outlet]
S1 & S2 --> CL[Central Control Logic]
CL --> P1 & P2
Derivative 1.2.3: High-Temperature, Short-Contact PAA for Aseptic Processing
- Enabling Description: An on-site PAA generation system designed for high-temperature, short-contact sanitization in aseptic processing lines. A hydrogen peroxide-triacetin solution (H2O2:triacetin mole ratio 3.2:1) is pre-heated to 60°C and then injected into a rapidly flowing (2 m/s) water stream that has also been pre-heated to 85°C. Downstream, a 30% potassium carbonate solution, also pre-heated to 60°C, is injected via a rapid-response solenoid valve. The reaction occurs in a compact, jacketed stainless steel tubular reactor with high-shear mixing elements. PAA generation to a concentration of 0.2-0.5% is achieved within 15-25 seconds, with the effluent immediately cooled to 40°C using a plate heat exchanger to prevent PAA degradation. This rapid cycle minimizes exposure time and maximizes sanitizing power.
sequenceDiagram
participant W as Hot Water Supply (85°C)
participant H as H2O2-Triacetin Precursor (60°C)
participant A as K2CO3 Alkali (60°C)
participant R as Jacketed SS Tubular Reactor
participant C as Plate Heat Exchanger
participant P as PAA Product (40°C)
W->>R: Flowing Hot Water
H->>R: Inject Pre-heated Precursor
A->>R: Inject Pre-heated Alkali
Note over R: Rapid High-Shear Mixing & Reaction (15-25s)
R->>C: Hot PAA Solution
C->>P: Cooled PAA Solution
1.3. Cross-Domain Application Derivatives
Derivative 1.3.1: Aerospace - Sterilization of Spacecraft Life Support Systems
- Enabling Description: A compact, in-situ PAA generation system for sterilizing closed-loop environmental control and life support systems (ECLSS) on long-duration spacecraft. A hydrogen peroxide-triacetin solution is stored in a sealed, pressurized reservoir. On command, a micro-dosing pump injects this precursor into a recirculating water line within the ECLSS. Simultaneously, a metered dose of lithium hydroxide solution (selected for its low atomic mass and compatibility with closed systems) is introduced. The reaction occurs within a biocompatible, inert polymer tubing (e.g., PEEK) section, producing PAA at concentrations of 100-500 ppm for biofilm control. The system operates intermittently, triggered by sensor readings indicating microbial growth or scheduled maintenance cycles. Post-treatment, residual PAA is quenched using an onboard UV-C light reactor.
graph TD
A[ECLSS Water Recirculation] --> B{Micro-Dosing Pump}
C[H2O2-Triacetin Reservoir] --> B
D[LiOH Solution Reservoir] --> E{Metering Pump}
E --> F[Injection Point 2]
B --> G[PEEK Reaction Tubing]
F --> G
G --> H{PAA Sensor}
H --> I[UV-C Quench Reactor]
I --> J[Sterile Water Back to ECLSS]
H --> K[ECLSS Control System]
K --> B & E
Derivative 1.3.2: AgTech - Irrigation System Biocide for Hydroponics
- Enabling Description: An on-demand PAA generation system integrated into a hydroponic farm's irrigation manifold. A low-concentration (15%) hydrogen peroxide solution is continuously mixed with diacetin at a 5:1 molar ratio to form the precursor. This is then injected into the main nutrient solution delivery line. Immediately after a static mixer, a food-grade calcium hydroxide slurry is injected to raise the pH and initiate PAA formation. The PAA solution (target 5-10 ppm) then flows through the irrigation lines to prevent algal growth and pathogen contamination in plant root zones. The system operates continuously during irrigation cycles, with flow rates automatically adjusted based on nutrient demand and real-time ORP measurements in the root zone return lines.
graph LR
N[Nutrient Solution Supply] --> M1(Main Manifold)
H[H2O2 (15%) Storage] --> P1{Precursor Mixer}
D[Diacetin Storage] --> P1
P1 --> I1{Injection Pump 1}
I1 --> M1
M1 --> S(Static Mixer)
C[Ca(OH)2 Slurry Storage] --> I2{Injection Pump 2}
I2 --> S
S --> R[Irrigation Lines to Plants]
R --> O[Return Line ORP Sensor]
O --> Cntrl[Control System]
Cntrl --> I1 & I2
Derivative 1.3.3: Consumer Electronics Manufacturing - Cleanroom Equipment Sterilization
- Enabling Description: A specialized on-site PAA generation unit for the disinfection of robotic arms and surface areas within ISO Class 1 cleanrooms for semiconductor manufacturing. A high-purity hydrogen peroxide-triacetin solution (mole ratio 7:1) is housed in a dedicated cleanroom-compatible container. This solution is introduced into an ultra-pure water (UPW) stream via a precision syringe pump. Following a micro-channel static mixer, a precisely metered, aerosolized solution of high-purity sodium bicarbonate (as the alkali) is injected to initiate PAA formation. The resulting PAA mist (50-200 ppm) is then delivered through a controlled nozzle system to sterilize surfaces, ensuring no residue and minimal downtime. The entire process is executed under inert nitrogen atmosphere to prevent oxidation and contamination.
graph TD
UPW[Ultra-Pure Water Supply] --> F[Flow Controller]
HPT[H2O2-Triacetin Solution] --> SP{Syringe Pump}
F --> SM(Micro-Channel Static Mixer)
SP --> SM
NaB[Sodium Bicarbonate (Aerosolized)] --> AP{Aerosol Pump}
AP --> SM
SM --> NS[Nozzle System (N2 purge)]
NS --> CR[Cleanroom Robotic Arm/Surfaces]
NS --> OS{PAA Sensor (Cleanroom)}
OS --> C[Cleanroom Control System]
1.4. Integration with Emerging Tech Derivatives
Derivative 1.4.1: AI-Driven Optimization for Adaptive PAA Dosing
- Enabling Description: An on-site PAA generation system (using H2O2-triacetin and NaOH) where a machine learning (ML) model continuously optimizes precursor and alkali dosing rates. Real-time data from multiple in-line sensors (PAA concentration, H2O2 residual, pH, ORP, water flow rate, water temperature, incoming microbial load data from rapid assays) is fed to the ML model. The AI analyzes historical performance, predicts demand fluctuations, and proactively adjusts pump speeds to maintain optimal PAA concentration for disinfection while minimizing precursor consumption. The AI also identifies and compensates for varying water quality or aging of components, ensuring consistent PAA efficacy within the 30-second to 5-minute generation window.
graph TD
I[Inlet Water] --> FM{Flow Meter}
HPA[H2O2-Triacetin Precursor] --> PP1{Precursor Pump}
NaOH[Alkali Solution] --> PP2{Alkali Pump}
FM --> M(Mixer & Reactor)
PP1 --> M
PP2 --> M
M --> PAA_S{PAA Sensor}
M --> H2O2_S{H2O2 Sensor}
M --> PH_S{pH Sensor}
M --> ORP_S{ORP Sensor}
M --> TEMP_S{Temp Sensor}
MIC_D[Microbial Load Data] --> AI[AI Optimization Engine]
PAA_S --> AI
H2O2_S --> AI
PH_S --> AI
ORP_S --> AI
TEMP_S --> AI
FM --> AI
AI --> PP1
AI --> PP2
M --> O[PAA Product Outlet]
Derivative 1.4.2: IoT Sensor Network for Predictive Maintenance and Remote Monitoring
- Enabling Description: A distributed, IoT-enabled PAA generation system where individual precursor containers, alkali tanks, injection pumps, static mixers, and reaction zones are equipped with wireless IoT sensors. These sensors monitor liquid levels, flow rates, pump motor diagnostics (vibration, temperature), pH, PAA concentration, H2O2 concentration, and ambient temperature. Data is transmitted via a secure LoRaWAN network to a cloud-based platform. This platform provides real-time dashboards for remote monitoring, generates alerts for critical parameters, and employs algorithms for predictive maintenance on pumps and sensors, ensuring continuous uptime and optimized inventory management for the H2O2-triacetin precursor and NaOH.
graph TD
subgraph IoT Devices
P1[Precursor Tank Level Sensor] -- LoRaWAN --> GW(Gateway)
P2[Alkali Tank Level Sensor] -- LoRaWAN --> GW
P3[Precursor Pump Diagnostic] -- LoRaWAN --> GW
P4[Alkali Pump Diagnostic] -- LoRaWAN --> GW
P5[Inline PAA Sensor] -- LoRaWAN --> GW
P6[Inline pH Sensor] -- LoRaWAN --> GW
P7[Flow Meter Sensor] -- LoRaWAN --> GW
end
GW --> Cloud[Cloud Platform (AWS IoT/Azure IoT)]
Cloud --> DB(Time-Series Database)
DB --> DASH[Dashboard & Alerts]
DASH --> USER[Operators/Maintenance]
DB --> PM[Predictive Maintenance Module]
PM --> ALERT[Maintenance Alerts]
Derivative 1.4.3: Blockchain for Supply Chain & PAA Efficacy Verification
- Enabling Description: An on-site PAA generation system integrated with a blockchain-based immutable ledger for end-to-end supply chain verification and PAA efficacy tracking. Each batch of hydrogen peroxide and triacetin precursor, along with the alkali (NaOH), is tagged with a unique cryptographic identifier at manufacturing. Upon arrival at the point-of-use, digital certificates are verified on the blockchain. During PAA generation, critical parameters (precursor/alkali batch IDs, exact dosing ratios, reaction times, final PAA concentration, pH, and ORP readings from calibrated sensors) are automatically recorded as hashed transactions on a private blockchain. This ensures a tamper-proof audit trail for regulatory compliance, product authenticity, and verifiable disinfection efficacy for sensitive applications (e.g., pharmaceutical clean-in-place).
sequenceDiagram
participant MFG as Manufacturer (H2O2, Triacetin, NaOH)
participant WH as Warehouse
participant OU as On-site PAA Unit
participant BC as Blockchain Ledger
MFG->>WH: Ship Precursor/Alkali (Batch IDs)
Note over MFG: Cryptographically hash batch data
WH->>OU: Deliver Precursor/Alkali
OU->>BC: Verify Batch IDs (Smart Contract)
OU->>OU: Start PAA Generation
Note over OU: Capture Dosing, Temp, pH, PAA, ORP
OU->>BC: Record Generation Event (Hashed Transaction)
BC->>OU: Confirm Transaction
OU->>OU: PAA Delivered to Point-of-Use
BC->>Auditor: Immutable Audit Trail
1.5. The "Inverse" or Failure Mode Derivatives
Derivative 1.5.1: Fail-Safe Dilution and Quench System
- Enabling Description: An on-site PAA generation system incorporating an emergency fail-safe mechanism. If any critical parameter deviates from safe operating limits (e.g., PAA concentration >5% due to dosing error, H2O2 residual >10%, pH <10.0, or main water flow interruption), a safety interlock system is activated. This system automatically shuts off precursor and alkali pumps, opens a high-flow diluent water valve, and simultaneously injects a pre-measured quantity of sodium thiosulfate solution (a PAA and H2O2 quencher) into the reaction medium. This rapidly dilutes and neutralizes the PAA, preventing uncontrolled reaction or delivery of an out-of-spec or hazardous solution to the point-of-use, effectively stopping the process and purging the lines.
stateDiagram
[*] --> Standby
Standby --> Generating: Start Command
Generating --> Safe_Limit_Violation: PAA_Sensor > 5% or H2O2_Sensor > 10% or pH < 10.0 or Flow_Loss
Generating --> Emergency_Quench: Safety Interlock Triggered
Safe_Limit_Violation --> Emergency_Quench: Initiates Quench Sequence
Emergency_Quench --> Diluting_Neutralizing: Actuate Dilution & Quench Pumps
Diluting_Neutralizing --> Standby: System Safe / Manual Reset
Emergency_Quench --> Fail_State: Quench System Failure
Fail_State --> [*]
Derivative 1.5.2: Low-Power/Prophylactic PAA Generation Mode
- Enabling Description: An on-site PAA generation system featuring a "Low-Power Mode" for periods of reduced demand or prophylactic treatment. In this mode, the controller significantly reduces the flow rates of both the hydrogen peroxide-triacetin precursor and the alkali solution by 80-95% compared to full operational mode. This results in the generation of a much lower concentration PAA solution (e.g., 10-50 ppm PAA, compared to normal 1-3%) with extended reaction times (e.g., 5-10 minutes). This mode conserves expensive precursors, extends equipment lifespan by reducing wear on pumps, and provides continuous, low-level disinfection to prevent biofilm formation during idle periods, without the need for a full shutdown and restart.
graph TD
A[Start Command] --> B{Demand Sensor / Schedule}
B -- High Demand --> C[Full Power Mode]
B -- Low Demand / Prophylactic --> D[Low Power Mode]
C --> P1(Full Flow H2O2-Triacetin)
C --> P2(Full Flow Alkali)
D --> P3(Reduced Flow H2O2-Triacetin)
D --> P4(Reduced Flow Alkali)
P1 & P2 --> R1[High PAA Generation]
P3 & P4 --> R2[Low PAA Generation (Prophylactic)]
R1 --> U1[High Disinfection Use]
R2 --> U2[Low-Level Disinfection Use]
Derivative 1.5.3: Fault-Tolerant Bypass and Alert System
- Enabling Description: A PAA generation system designed with a redundant bypass loop for fault tolerance. If any critical component in the PAA generation train (e.g., precursor pump failure, static mixer blockage, pH probe malfunction indicating incorrect alkalinity) is detected by diagnostic sensors, the system automatically activates a solenoid valve to divert the untreated water stream around the PAA generation components. Concurrently, an audible alarm, visual alert, and remote notification (e.g., SMS, email) are triggered to alert operators of the fault condition. This ensures continuous water flow to the point-of-use (albeit without PAA treatment) and prevents potential damage from malfunctioning equipment or delivery of an improperly treated solution, until maintenance can be performed.
graph LR
A[Inlet Water] --> B{Solenoid Valve (Normal: Gen)}
B -- Normal Operation --> C[H2O2-Triacetin Injection]
C --> D[Alkali Injection]
D --> E[Mixing & Reaction]
E --> F[PAA Outlet]
B -- Fault Detected --> G[Bypass Line]
G --> F
C -- Fault --> H[Diagnostic System]
D -- Fault --> H
E -- Fault --> H
H --> I[Alarm System]
I --> J[Remote Notification]
H --> B(Activate Bypass)
Independent Claim 8: Batch Method for PAA Generation
Core Claim 8: A method for continuously or intermittently generating a non-equilibrium solution of PAA on-site in a batch process, comprising providing a container of water, introducing a hydrogen peroxide-acetyl precursor solution to the water, mixing them, and then adding an aqueous source of an alkali metal or earth alkali metal hydroxide to form a reaction medium where PAA is generated within 30 seconds to five minutes, and the PAA solution has a pH of about 11.2 to about 13.37.
2.1. Material & Component Substitution Derivatives
Derivative 2.1.1: Alternative Acetyl Precursor (Diacetin) and Alkali (Calcium Hydroxide Slurry)
- Enabling Description: A batch PAA generation process using a 500-liter jacketed stainless steel mixing tank. Softened water is first added to the tank. Then, a hydrogen peroxide-diacetin precursor solution (40% H2O2, 30% diacetin, 30% water, mole ratio H2O2:diacetin approx. 4.5:1) is pumped into the tank and agitated by a high-shear submersible mixer for 30 seconds. Subsequently, a 10% aqueous calcium hydroxide slurry is slowly metered into the vigorously stirred mixture until the pH reaches 12.8. PAA generation, reaching a concentration of 2-4%, is observed within 2 minutes of alkali addition. The jacketed tank allows for temperature control (e.g., maintaining 25°C) to manage the exothermic reaction.
graph TD
A[Softened Water Inlet] --> B[Jacketed SS Mixing Tank]
C[H2O2-Diacetin Precursor Tank] --> D{Pump 1}
D --> B
E[Ca(OH)2 Slurry Tank] --> F{Pump 2}
F --> B
B --> G{High-Shear Submersible Mixer}
G --> H{pH Probe}
G --> I{PAA Sensor}
B --> J[PAA Batch to Point-of-Use]
H --> K[Controller (controls Pump 2)]
Derivative 2.1.2: Stabilized Precursor (HEDP Trace) and Carbonate/Bicarbonate Buffer
- Enabling Description: A batch method employing a hydrogen peroxide-triacetin precursor solution (as per Claim 15) that additionally contains a trace amount (e.g., 50 ppm) of hydroxyethylidene diphosphonic acid (HEDP) as a stability enhancer during storage. This precursor is added to a batch tank filled with process water and mixed. Instead of a single strong alkali, a pre-calculated mixture of sodium carbonate and sodium bicarbonate is added as a solid blend to achieve a final buffered pH of 11.5-12.0. This buffering system provides more stable pH control, preventing spikes in alkalinity and prolonging optimal reaction conditions. PAA generation is complete within 3-5 minutes, producing a solution of 1-5% PAA.
graph TD
A[Process Water Container] --> B{Agitator}
C[H2O2-Triacetin (HEDP) Precursor] --> D{Pump}
D --> A
E[Solid Na2CO3/NaHCO3 Blend] --> F{Feeder}
F --> A
A --> G{pH Probe}
G --> H[Controller (monitors pH)]
H --> I[PAA Solution to Use]
2.2. Operational Parameter Expansion Derivatives
Derivative 2.2.1: Micro-Batch Generation in Disposable Cartridges
- Enabling Description: A "micro-batch" PAA generation system for highly localized or sterile applications. Small, pre-filled disposable cartridges contain precisely measured aliquots of hydrogen peroxide-triacetin precursor (e.g., 10 mL of solution from Claim 15). These cartridges are inserted into a portable, automated dispenser. The dispenser draws a fixed volume of sterile water (e.g., 90 mL) into a mixing chamber within the cartridge, followed by a precise injection of concentrated sodium hydroxide solution (e.g., 10% NaOH). Rapid ultrasonic mixing within the cartridge chamber initiates PAA formation. A 100 mL batch of 0.5-1.5% PAA solution is generated within 30 seconds, immediately ready for point-of-use application without the need for large tanks or complex plumbing.
sequenceDiagram
participant C as Disposable Cartridge
participant D as Automated Dispenser
participant W as Sterile Water Source
participant A as NaOH Concentrate
D->>C: Insert Cartridge
W->>C: Fill Mixing Chamber (90 mL)
A->>C: Inject NaOH (precise volume)
Note over C: Ultrasonic Mixing (30s)
C->>D: Eject PAA Solution
D->>D: Dispense PAA to Point-of-Use
Derivative 2.2.2: Extreme Temperature Batch (Cryogenic Pre-cooling)
- Enabling Description: A batch PAA generation method designed for applications requiring extremely cold water processing. A 1000-liter jacketed mixing tank is pre-cooled to 0°C. Deionized water, pre-chilled to 0°C, is added to the tank. The hydrogen peroxide-triacetin precursor solution (as per Claim 15) is then introduced, followed by 50% sodium hydroxide solution, with both additions occurring while maintaining the 0°C temperature. Due to the reduced kinetics at cryogenic temperatures, the mixing and reaction time is extended to 10 minutes to ensure optimal PAA generation (target 0.5-1% PAA). The chilling system maintains the temperature during the entire reaction period, minimizing PAA degradation from heat. The pH range of 11.2-13.37 is still maintained.
graph TD
W[Chilled Deionized Water (0°C)] --> T[Jacketed Mixing Tank]
T --> J(Jacketed Cooling System)
HPA[H2O2-Triacetin Precursor] --> P1{Pump 1}
P1 --> T
NAOH[50% NaOH] --> P2{Pump 2}
P2 --> T
T --> M{Agitator}
M --> S{PAA Sensor}
S --> C[Controller]
C --> J(Maintain 0°C)
T --> O[Chilled PAA Batch (10 min RT)]
2.3. Cross-Domain Application Derivatives
Derivative 2.3.1: Pharmaceutical Manufacturing - Bioreactor Clean-in-Place (CIP)
- Enabling Description: A batch PAA generation process specifically designed for the Clean-in-Place (CIP) cycle of pharmaceutical bioreactors. A dedicated mixing vessel, sterile-validated, is charged with USP-grade water. A pre-sterilized hydrogen peroxide-triacetin solution (H2O2:triacetin 3.8:1) is transferred to this vessel via aseptic transfer lines. After mixing, a sterile-filtered 45% potassium hydroxide solution is added to initiate PAA generation, achieving a pH of 12.0-12.5. The 1-2% PAA solution is then immediately pumped into the bioreactor CIP circuit. The generation-to-use time is tightly controlled within 90 seconds to maximize the active PAA concentration for effective bioburden reduction. All components and processes adhere to cGMP standards.
sequenceDiagram
participant SV as Sterile Mixing Vessel
participant USP as USP Water Supply
participant HPT as Pre-sterilized H2O2-Triacetin
participant KOH as Sterile KOH (45%)
participant BR as Bioreactor CIP Circuit
USP->>SV: Fill USP Water
HPT->>SV: Aseptic Transfer H2O2-Triacetin
SV->>SV: Mix (Agitator)
KOH->>SV: Add Sterile KOH
Note over SV: PAA Generation (pH 12.0-12.5, <90s)
SV->>BR: Pump PAA Solution to Bioreactor CIP
Derivative 2.3.2: Art Restoration - Gentle Bleaching of Paper Artifacts
- Enabling Description: A precisely controlled micro-batch PAA generation method for the gentle bleaching and disinfection of delicate paper artifacts during restoration. A small glass vessel serves as the batch container. Distilled water is added, followed by a dilute hydrogen peroxide-diacetin precursor solution (e.g., 5% H2O2, 2% diacetin). The mixture is gently stirred. A very dilute (0.5%) sodium bicarbonate solution is then carefully added dropwise to achieve a final pH of 11.2, initiating a slow PAA generation. The reaction is allowed to proceed for 5 minutes, producing PAA at concentrations of 50-100 ppm. This low concentration and controlled pH prevent damage to delicate cellulose fibers, offering a safe, on-demand bleaching agent for historical documents.
graph TD
W[Distilled Water] --> GV[Glass Vessel]
DHP[Dilute H2O2-Diacetin Precursor] --> P1{Micro-Pump 1}
P1 --> GV
GV --> S(Gentle Magnetic Stirrer)
DSB[Dilute NaHCO3 Solution] --> P2{Micro-Pump 2 (Dropwise)}
P2 --> GV
GV --> PH[pH Meter]
PH --> O[PAA Solution for Art Restoration]
PH --> C[Control System (maintains pH 11.2)]
Derivative 2.3.3: Veterinary Science - Disinfection of Surgical Tools
- Enabling Description: An on-site PAA generation system for batch disinfection of veterinary surgical tools. A dedicated immersion tank, constructed from medical-grade polypropylene, is filled with softened water. A hydrogen peroxide-triacetin solution (H2O2:triacetin 4:1) is then dispensed into the tank. Following a brief mixing period (30 seconds) using a magnetic stir bar, an aqueous sodium hydroxide solution is added until the pH reaches 12.0. Surgical instruments are then immersed in the freshly generated 0.5-1% PAA solution for a specified contact time (e.g., 2 minutes). The process is automated to ensure consistent PAA concentration and pH within the claimed ranges (pH 11.2-13.37), maximizing germicidal efficacy.
sequenceDiagram
participant IT as Immersion Tank (Polypropylene)
participant SW as Softened Water
participant HPT as H2O2-Triacetin Precursor
participant NaOH as NaOH Solution
participant ST as Surgical Tools
SW->>IT: Fill Softened Water
HPT->>IT: Dispense Precursor
IT->>IT: Mix (30s)
NaOH->>IT: Add NaOH (to pH 12.0)
Note over IT: PAA Generation (0.5-1% PAA)
ST->>IT: Immerse Surgical Tools (2 min contact)
IT->>IT: Drain PAA
2.4. Integration with Emerging Tech Derivatives
Derivative 2.4.1: AI-Driven Batch Process Optimization with Digital Twin
- Enabling Description: A batch PAA generation system where an AI-driven digital twin monitors and optimizes the reaction kinetics. A physical batch reactor (mixing tank) is equipped with a suite of real-time sensors (PAA, H2O2, pH, temperature, stirrer RPM, conductivity). This sensor data feeds into a computational "digital twin" of the reactor, running a kinetic model of the perhydrolysis reaction. The AI continuously adjusts the alkali dosing rate and mixing intensity to achieve a target PAA concentration and optimal precursor conversion within 30 seconds to five minutes, while minimizing H2O2 residual and ensuring the final pH is within 11.2-13.37. The digital twin can also simulate "what-if" scenarios for fault prediction and process improvement.
graph TD
R[Physical Batch Reactor] --> S{Sensors (PAA, H2O2, pH, Temp, RPM, Cond)}
S --> DT[Digital Twin (Kinetic Model)]
DT --> AI[AI Optimization Engine]
AI --> C[Controller]
C --> R(Alkali Pump, Stirrer)
R --> O[PAA Batch Output]
AI -- Predictive Maintenance --> M[Maintenance Alerts]
Derivative 2.4.2: Robotic Dispensing for Hazardous Precursors
- Enabling Description: A fully automated batch PAA generation system utilizing robotic dispensing for enhanced safety and precision, particularly for high-concentration or hazardous precursors. A robotic arm precisely dispenses measured volumes of hydrogen peroxide (e.g., 70% H2O2) and pure triacetin (as individual components, rather than pre-mixed) into a sealed, inert batch reactor containing deoxygenated water. Subsequently, the robot dispenses a highly concentrated (75%) potassium hydroxide solution. The robotic system ensures accurate volumetric control, minimizes human exposure to corrosive chemicals, and maintains a sterile environment for specialized applications. The reaction proceeds to yield 3-7% PAA at a pH of 11.2-13.37 within the typical 30-second to five-minute window, under continuous robotic monitoring of key parameters.
sequenceDiagram
participant R as Robotic Arm
participant H as H2O2 (70%) Source
participant T as Pure Triacetin Source
participant K as KOH (75%) Source
participant B as Sealed Batch Reactor
participant W as Deoxygenated Water
participant C as Control System
C->>R: Initiate Batch
R->>W: Dispense H2O2 into B
R->>W: Dispense Triacetin into B
Note over B: Mix (Integrated Stirrer)
R->>W: Dispense KOH into B
Note over B: PAA Generation (30s-5min, pH 11.2-13.37)
C->>B: Monitor Reaction Parameters
B->>B: Dispense PAA Batch
2.5. The "Inverse" or Failure Mode Derivatives
Derivative 2.5.1: Automated Batch Overflow Prevention and Emergency Venting
- Enabling Description: A batch PAA generation system equipped with a multi-level ultrasonic level sensor and an emergency venting system. If the water or precursor additions cause the liquid level in the batch tank to exceed a predefined safe limit, the system immediately halts all incoming liquid flows. In case of an unexpected exothermic runaway reaction leading to rapid gas evolution and dangerous pressure build-up, a pressure transducer triggers an emergency relief valve, venting non-condensable gases (primarily O2 from H2O2 decomposition) through a scrubber system. This prevents tank over-pressurization and potential rupture, ensuring a safe failure mode while maintaining the pH within the claimed range during normal operation.
stateDiagram
[*] --> Idle
Idle --> Filling: Start Batch
Filling --> Mixing_Precursors: Water + H2O2-Triacetin Added
Mixing_Precursors --> Adding_Alkali: Alkali Added
Adding_Alkali --> Reacting: PAA Generation
Reacting --> Batch_Complete: Target PAA/Time Reached
Batch_Complete --> Idle
Filling --> Overflow_Detected: Level Sensor High
Mixing_Precursors --> Overflow_Detected
Adding_Alkali --> Overflow_Detected
Reacting --> Pressure_Exceeded: Pressure Sensor High
Overflow_Detected --> Halt_Inlets: Stop Pumps
Pressure_Exceeded --> Emergency_Venting: Activate Relief Valve
Emergency_Venting --> Scrubbing: Direct Vented Gas to Scrubber
Halt_Inlets --> Safe_State_Warning: Operator Alert
Emergency_Venting --> Safe_State_Warning: Operator Alert
Derivative 2.5.2: Controlled Degradation for Residual PAA Neutralization
- Enabling Description: A batch PAA generation system with an integrated post-generation neutralization cycle. After the desired PAA concentration has been achieved and dispensed, any residual PAA remaining in the mixing tank or lines is actively degraded. This is achieved by introducing a precise amount of a reducing agent (e.g., sodium metabisulfite solution) into the batch tank. This rapidly deactivates any leftover PAA and unreacted hydrogen peroxide, yielding harmless byproducts. The system monitors the ORP until a safe, near-zero oxidant level is confirmed before draining the tank, preventing accidental exposure to PAA or H2O2 during cleaning or maintenance. The original batch still adheres to pH 11.2-13.37.
graph TD
A[PAA Batch Ready] --> B{PAA Dispensed}
B --> C[Residual PAA in Tank]
C --> D{Reducing Agent (Na2S2O5) Injection}
D --> E[Mix & React]
E --> F{ORP Sensor}
F -- Oxidant Present --> E
F -- Oxidant Absent --> G[Neutralized Effluent Drain]
Independent Claim 15: Liquid Composition for PAA Generation
Core Claim 15: A liquid composition for generating non-equilibrium solutions of PAA on-site, comprising about 23% to about 40% aqueous hydrogen peroxide, about 20% to about 52% triacetin, and water, wherein a trace amount of PAA is formed within the first day of preparation, and the mole ratio of hydrogen peroxide:triacetin is about 2.98:1 to about 12.84:1, and the pH is about 1.46 to about 2.2.
3.1. Material & Component Substitution Derivatives
Derivative 3.1.1: Diacetin as Acetyl Precursor with Glycerol Co-solvent
- Enabling Description: A stable liquid precursor composition for on-site PAA generation, comprising approximately 35% aqueous hydrogen peroxide, 35% diacetin (glycerol diacetate), 10% glycerol (as a solubility enhancer and humectant), and 20% water. This composition maintains a mole ratio of hydrogen peroxide:diacetin of approximately 5:1. The pH of this formulation is between 1.8 and 2.0. A trace amount of PAA is formed within the first 24 hours of preparation (e.g., <0.05%), demonstrating its stability for storage and transport. The addition of glycerol further improves solubility and potentially reduces freezing point for cold storage applications.
classDiagram
class LiquidComposition {
+HydrogenPeroxide: 35% (aq)
+Diacetin: 35%
+Glycerol: 10%
+Water: 20%
+H2O2_Diacetin_MoleRatio: ~5:1
+pH: 1.8-2.0
+TracePAA_Day1: <0.05%
}
Derivative 3.1.2: Ethyl Acetate (Co-soluble) and Low-Concentration H2O2
- Enabling Description: A liquid precursor composition formulated for rapid evaporation and minimal residue, consisting of approximately 25% hydrogen peroxide solution (from a 35% H2O2 stock), 30% ethyl acetate (partially co-soluble, with a small amount of an ethoxylated alcohol non-ionic surfactant, 1%, to maintain homogeneity), and 44% water. The mole ratio of hydrogen peroxide:ethyl acetate is approximately 1.5:1. The pH is adjusted to be between 1.5 and 2.2 with phosphoric acid. This composition forms only a trace amount of PAA (<0.01%) within the first day and is intended for applications where low flash point organic components are permissible, offering a different kinetic profile for perhydrolysis compared to triacetin due to the single acetyl group.
graph LR
H2O2_35[35% H2O2 Stock] --> C1(25% H2O2 Aqueous)
EA[Ethyl Acetate] --> C2(30% Ethyl Acetate)
SURF[Ethoxylated Alcohol Surfactant (1%)] --> C2
W[Water] --> C3(44% Water)
PA[Phosphoric Acid] --> C4(pH Adj. 1.5-2.2)
C1 & C2 & C3 & C4 --> LC[Liquid Composition]
LC -- Properties --> R1(H2O2:EA ~1.5:1)
LC -- Properties --> R2(Trace PAA Day1 <0.01%)
Derivative 3.1.3: Acetylated Starch (Solubilized) with Enhanced H2O2 Stability
- Enabling Description: A stable liquid composition comprising 28% aqueous hydrogen peroxide (from 50% H2O2), 25% pre-solubilized acetylated starch (e.g., hydroxypropyl distarch acetate, 15% solution in propylene glycol monoethyl ether), and 47% water. This formulation uses a more complex acetyl precursor where the acetyl groups are sterically hindered yet accessible. A minor stabilizer system (e.g., 100 ppm dipicolinic acid) is incorporated to maintain hydrogen peroxide stability. The pH of the composition is approximately 1.9. The mole ratio of H2O2 to acetyl groups (calculated as total acetyl content from acetylated starch) is approximately 8:1. Trace PAA formation is maintained below 0.02% in 24 hours.
classDiagram
class LiquidComposition {
+HydrogenPeroxide: 28% (aq)
+AcetylatedStarchSolution: 25% (in PGMEE)
+Water: 47%
+DipicolinicAcid: 100 ppm
+pH: ~1.9
+H2O2_AcetylGroup_MoleRatio: ~8:1
+TracePAA_Day1: <0.02%
}
3.2. Operational Parameter Expansion Derivatives
Derivative 3.2.1: Super-Concentrated Precursor for Reduced Shipping Volume
- Enabling Description: A super-concentrated liquid precursor composition designed to minimize transportation costs and storage footprint. It consists of 45% hydrogen peroxide (from 70% H2O2 stock), 58% triacetin, and a balance of water (e.g., 7%). This composition features a hydrogen peroxide:triacetin mole ratio of approximately 1:1, maximizing the acetyl precursor density. Due to its high concentration, it requires specialized, temperature-controlled (e.g., 15-20°C) and pressure-rated containers for transport. The pH is approximately 1.0-1.5, ensuring minimal PAA formation (<0.005%) within the first 24 hours, but requiring careful dilution and activation at the point-of-use.
graph TD
H2O2_70[70% H2O2 Stock] --> HC1(45% H2O2)
TA[Pure Triacetin] --> HC2(58% Triacetin)
W[Water] --> HC3(7% Water)
HC1 & HC2 & HC3 --> SCC[Super-Concentrated Composition]
SCC -- Properties --> MR(H2O2:Triacetin ~1:1)
SCC -- Properties --> pH(pH 1.0-1.5)
SCC -- Properties --> TPA(Trace PAA Day1 <0.005%)
SCC -- Storage Req. --> TEMP_CTRL[Temperature Controlled (15-20°C)]
SCC -- Storage Req. --> PRES_RATE[Pressure-Rated Containers]
Derivative 3.2.2: Extreme-Temperature Stable Composition for Arid Environments
- Enabling Description: A liquid precursor composition formulated for stability under prolonged storage in high-temperature, arid environments (e.g., 40-50°C). It comprises 30% aqueous hydrogen peroxide, 25% triacetin, and 45% water, with an optimized hydrogen peroxide:triacetin mole ratio of 8:1. To enhance high-temperature stability, 200 ppm of 8-hydroxyquinoline is included as an additional chelating agent and free radical scavenger. The pH is maintained at 1.7-2.0. This formulation is demonstrably stable with less than 0.1% PAA formed after 7 days at 45°C, providing robust performance in challenging logistical scenarios.
classDiagram
class LiquidComposition {
+HydrogenPeroxide: 30% (aq)
+Triacetin: 25%
+Water: 45%
+8Hydroxyquinoline: 200 ppm
+pH: 1.7-2.0
+H2O2_Triacetin_MoleRatio: 8:1
+TracePAA_7Days_45C: <0.1%
}
3.3. Cross-Domain Application Derivatives
Derivative 3.3.1: Textile Pre-treatment - On-Demand Bleaching Stock
- Enabling Description: A liquid precursor composition intended for the on-demand preparation of PAA bleaching baths in textile pre-treatment. The composition contains 38% aqueous hydrogen peroxide, 40% triacetin, and 22% water, with a H2O2:triacetin mole ratio of 3.5:1. Its pH is maintained at 1.6. This concentrated, stable precursor forms only trace PAA (<0.03% within 24 hours), ensuring minimal active degradation during storage. Upon activation with a strong alkali in the textile mill's process water, it rapidly generates PAA for delignification and whitening of raw fibers, providing a more flexible and safer alternative to concentrated PAA solutions.
graph TD
A[H2O2-Triacetin Precursor (38% H2O2, 40% Triacetin)] --> B{Textile Mill Storage}
B --> C[Process Water Line]
C --> D[Alkali Addition]
D --> E[Mixing & Reaction (PAA Gen)]
E --> F[Textile Bleaching Bath]
A -- Properties --> P1(H2O2:Triacetin 3.5:1)
A -- Properties --> P2(pH 1.6)
A -- Properties --> P3(Trace PAA <0.03% Day1)
Derivative 3.3.2: Food Preservation - Surface Sterilization Concentrate
- Enabling Description: A liquid precursor composition specifically formulated as a concentrate for on-site dilution and activation for direct surface sterilization in food processing. It consists of 23% aqueous hydrogen peroxide (USP grade), 50% triacetin (GRAS-approved), and 27% sterile water, achieving a H2O2:triacetin mole ratio of 3:1. The pH is 2.1, with no added non-GRAS stabilizers. This composition is designed to form only a negligible trace of PAA (<0.001%) in the concentrate within the first day. When diluted and mixed with a GRAS-approved alkaline solution (e.g., sodium carbonate solution) on a food contact surface or in a spray system, it rapidly generates PAA for microbial reduction, ensuring food safety and regulatory compliance.
classDiagram
class FoodPreservationConcentrate {
+HydrogenPeroxide: 23% (USP grade)
+Triacetin: 50% (GRAS-approved)
+Water: 27% (sterile)
+H2O2_Triacetin_MoleRatio: 3:1
+pH: 2.1
+TracePAA_Day1: <0.001%
+Application: Surface Sterilization
}
3.4. Integration with Emerging Tech Derivatives
Derivative 3.4.1: Smart Packaging with Integrated Stability Sensors
- Enabling Description: A liquid precursor composition (as per Claim 15) stored in smart packaging featuring integrated, passive RFID tags and embedded chemical sensors. These sensors monitor internal temperature, light exposure, and sub-trace PAA formation kinetics (e.g., via a colorimetric indicator or electrochemical sensor). Data from these sensors is wirelessly transmitted to a handheld reader or central inventory system upon proximity, providing a real-time assessment of the composition's shelf life and stability. This smart packaging proactively alerts users if degradation accelerates or if the "trace PAA" threshold is nearing a point that would compromise on-site generation efficiency or safety, enabling just-in-time inventory rotation.
graph TD
C[Liquid Composition Container] --> RFID{Passive RFID Tag}
RFID --> TS[Temp Sensor]
RFID --> LS[Light Sensor]
RFID --> PS[Colorimetric PAA Sensor (Sub-trace)]
TS --> RFID
LS --> RFID
PS --> RFID
RFID --> R(RFID Reader / Handheld Device)
R --> CS[Central Inventory System]
CS --> A[Alerts / Shelf Life Prediction]
Derivative 3.4.2: AI-Optimized Formulation for Variable Storage Conditions
- Enabling Description: A liquid precursor composition where the exact proportions of hydrogen peroxide (23-40%), triacetin (20-52%), and minor stabilizers (e.g., trace amounts of salicylic acid or citrate for pH buffering) are determined by an AI algorithm. The AI takes into account expected storage temperature profiles (e.g., tropical vs. arctic climates), anticipated transportation durations, and target on-site PAA generation kinetics. The AI-generated formula ensures optimal stability (pH 1.46-2.2, trace PAA within 24 hours) under specific, variable supply chain conditions, maximizing shelf life while guaranteeing efficient PAA generation upon activation. The mole ratio of H2O2:triacetin is maintained within 2.98:1 to 12.84:1.
graph TD
I[Input Data (Storage Temp, Transport Duration, Target Kinetics)] --> AI_F[AI Formulation Engine]
AI_F --> O[Optimal Composition Output]
O --> H2O2[Hydrogen Peroxide %]
O --> TA[Triacetin %]
O --> W[Water %]
O --> STAB[Minor Stabilizers (Type/%) (e.g., Salicylic Acid)]
O -- Properties --> pH_R[pH Range 1.46-2.2]
O -- Properties --> MR_R[H2O2:TA Mole Ratio 2.98:1-12.84:1]
O -- Properties --> TPA_R[Trace PAA Day 1]
3.5. The "Inverse" or Failure Mode Derivatives
Derivative 3.5.1: Self-Neutralizing Composition upon Container Breach
- Enabling Description: A liquid precursor composition (as per Claim 15) engineered with a microencapsulated reducing agent (e.g., encapsulated sodium thiosulfate or ascorbic acid). The microcapsules are designed to rupture upon significant mechanical stress, pH shift (e.g., rapid increase to neutral from acidic), or exposure to atmospheric oxygen resulting from a container breach. Upon rupture, the reducing agent is released into the composition, rapidly neutralizing any formed PAA and decomposing hydrogen peroxide, thereby preventing uncontrolled exothermic reactions or exposure to active oxidants in a spill scenario. The original composition maintains its pH of 1.46-2.2 and trace PAA during intact storage.
graph TD
C[Liquid Composition (H2O2-Triacetin, pH 1.46-2.2)] --> M(Microencapsulated Reducing Agent)
M -- Intact --> C
M -- Breach / Stress / pH Shift --> R(Rupture Microcapsules)
R --> NA(Neutralize Active Ingredients)
NA --> S[Safe Degradation Products]
C -- Normal Use --> O[On-site Generation]
Derivative 3.5.2: Visual Degradation Indicator Dye
- Enabling Description: A liquid precursor composition (as per Claim 15) incorporating a non-interfering, redox-sensitive indicator dye (e.g., methylene blue in a specific pH range or a phenolphthalein/thymolphthalein mixture). This dye is initially colorless in the stable, acidic composition (pH 1.46-2.2). However, if significant degradation of hydrogen peroxide occurs (e.g., loss of >5% active H2O2) or if PAA levels exceed the "trace" amount (e.g., >0.1% PAA) due to improper storage or extended shelf life, the dye undergoes a irreversible color change (e.g., blue or pink). This visual cue provides an immediate, qualitative indication to the user that the composition's efficacy or safety profile has been compromised, even without instrumental analysis.
stateDiagram
[*] --> Stable_Composition
Stable_Composition --> Degraded_Composition: H2O2 Loss >5% or PAA >0.1%
Degraded_Composition --> Visually_Indicated: Dye Changes Color
Stable_Composition --> On_Site_Use: Normal Application
Visually_Indicated --> Discard_Or_Test: Action Required
Combination Prior Art Scenarios
These scenarios combine elements of US Patent 9,730,443 with existing open-source standards, demonstrating how further improvements could be considered obvious.
1. US 9,730,443 (Claims 1 & 8) + WO 01/46519 A1 + Open-Source PLC Programming Standard (IEC 61131-3)
- Enabling Description: An on-site PAA generation system (either continuous flow as in Claim 1 or batch as in Claim 8) that replaces the solid TAED acetyl precursor of WO 01/46519 A1 with the liquid hydrogen peroxide-triacetin precursor solution from US 9,730,443. The entire control logic for managing the metering pumps, static mixers, reaction vessels/piping, and alkali injection (e.g., NaOH) is implemented on a Programmable Logic Controller (PLC) using ladder logic, structured text, or function block diagrams conforming to the IEC 61131-3 open-source standard. This combination makes the integration of the improved chemistry into a standard, industrial, open-source automation framework obvious, allowing for precise control and robust operation.
graph TD
A[Raw Water Inlet] --> B{Flow Meter}
C[H2O2-Triacetin Precursor (US9730443)] --> P1{Metering Pump 1}
D[Alkali Solution (NaOH)] --> P2{Metering Pump 2}
B --> M(Mixing & Reaction Section)
P1 --> M
P2 --> M
M --> S{PAA Sensor}
S --> PLC[PLC (IEC 61131-3 Standard)]
B --> PLC
PLC --> P1
PLC --> P2
M --> O[PAA Product Outlet]
2. US 9,730,443 (Claim 15) + Open-Source Green Chemistry Principles + Existing GRAS Food-Grade Stabilizer Standards
- Enabling Description: A liquid precursor composition (as described in Claim 15) for on-site PAA generation, where the specific mole ratios of hydrogen peroxide to triacetin (within 2.98:1 to 12.84:1) and the pH (1.46-2.2) are optimized according to open-source Green Chemistry principles (e.g., maximizing atom economy, minimizing auxiliary substances) to be highly stable and produce minimal waste. Furthermore, trace amounts of specific, multi-functional stabilizing agents, already recognized as Generally Recognized As Safe (GRAS) by the FDA (e.g., ascorbic acid, citric acid, or certain phosphate salts used at concentrations well below regulatory limits for PAA products), are incorporated to further reduce trace PAA formation during storage (below 0.005% within 24 hours). This combination renders obvious the development of environmentally conscious and regulatory-compliant precursor formulations.
graph TD
GC[Open-Source Green Chemistry Principles] --> F(Formulation Optimization)
GRAS[GRAS Food-Grade Stabilizer Standards] --> F
F --> LC[Liquid Composition (US9730443, Claim 15)]
LC -- H2O2 (23-40%) --> I1
LC -- Triacetin (20-52%) --> I2
LC -- Water --> I3
LC -- Trace Stabilizers (GRAS) --> I4
LC -- Optimized Properties --> P(pH 1.46-2.2, H2O2:TA ratio, Trace PAA <0.005% Day1)
3. US 9,730,443 (Claims 1 & 8) + Open-Source Data Logging (Grafana/Prometheus) + Standard Industrial Communication (Modbus TCP/IP)
- Enabling Description: An on-site PAA generation system (either continuous flow or batch) implementing the methods of US 9,730,443 (using H2O2-triacetin and alkali). This system is instrumented with industrial sensors (PAA, H2O2, pH, flow, temperature) that transmit real-time process data via Modbus TCP/IP (a widely adopted open industrial communication protocol) to a local data acquisition gateway. This gateway then forwards the data to a server running an open-source data logging and visualization stack, such as Prometheus for metrics collection and Grafana for dashboarding and alerting. This configuration enables transparent, accessible, and customizable monitoring of the PAA generation process, making the intelligent data exploitation of such systems obvious.
graph TD
S1[PAA Sensor] --> MB(Modbus TCP/IP)
S2[H2O2 Sensor] --> MB
S3[pH Sensor] --> MB
S4[Flow Sensor] --> MB
S5[Temperature Sensor] --> MB
MB --> GW[Data Acquisition Gateway]
GW --> PROM[Prometheus (Metrics Storage)]
PROM --> GRAF[Grafana (Dashboards & Alerts)]
GRAF --> OPS[Operators / Engineers]
GW --> OPC_UA[OPC UA (Alternative)]
Generated 6/9/2026, 10:35:39 PM
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This patent in court (2)
2 tracked lawsuits name US 9730443.