WO2022204039A1 - Process and composition acting as an active, inert or adjuvant for surface treatment and disinfection - Google Patents
Process and composition acting as an active, inert or adjuvant for surface treatment and disinfection Download PDFInfo
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- WO2022204039A1 WO2022204039A1 PCT/US2022/021169 US2022021169W WO2022204039A1 WO 2022204039 A1 WO2022204039 A1 WO 2022204039A1 US 2022021169 W US2022021169 W US 2022021169W WO 2022204039 A1 WO2022204039 A1 WO 2022204039A1
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- 239000000203 mixture Substances 0.000 title claims abstract description 119
- 238000000034 method Methods 0.000 title description 53
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- 238000004659 sterilization and disinfection Methods 0.000 title description 3
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- 238000004381 surface treatment Methods 0.000 title description 2
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- 229930014626 natural product Natural products 0.000 claims abstract description 3
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- OUYCCCASQSFEME-QMMMGPOBSA-N L-tyrosine Chemical compound OC(=O)[C@@H](N)CC1=CC=C(O)C=C1 OUYCCCASQSFEME-QMMMGPOBSA-N 0.000 description 1
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- 241000194018 Streptococcaceae Species 0.000 description 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 1
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- HHTWOMMSBMNRKP-UHFFFAOYSA-N carvacrol Natural products CC(=C)C1=CC=C(C)C(O)=C1 HHTWOMMSBMNRKP-UHFFFAOYSA-N 0.000 description 1
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- 150000003856 quaternary ammonium compounds Chemical class 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
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- 125000001973 tert-pentyl group Chemical group [H]C([H])([H])C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
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- OUYCCCASQSFEME-UHFFFAOYSA-N tyrosine Natural products OC(=O)C(N)CC1=CC=C(O)C=C1 OUYCCCASQSFEME-UHFFFAOYSA-N 0.000 description 1
- 238000000108 ultra-filtration Methods 0.000 description 1
- MYPYJXKWCTUITO-LYRMYLQWSA-N vancomycin Chemical compound O([C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1=C2C=C3C=C1OC1=CC=C(C=C1Cl)[C@@H](O)[C@H](C(N[C@@H](CC(N)=O)C(=O)N[C@H]3C(=O)N[C@H]1C(=O)N[C@H](C(N[C@@H](C3=CC(O)=CC(O)=C3C=3C(O)=CC=C1C=3)C(O)=O)=O)[C@H](O)C1=CC=C(C(=C1)Cl)O2)=O)NC(=O)[C@@H](CC(C)C)NC)[C@H]1C[C@](C)(N)[C@H](O)[C@H](C)O1 MYPYJXKWCTUITO-LYRMYLQWSA-N 0.000 description 1
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Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P1/00—Disinfectants; Antimicrobial compounds or mixtures thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/02—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing liquids as carriers, diluents or solvents
Definitions
- the present disclosure is directed to composition and processes that provide for safe and effective disinfectant functioning against one or more microorganisms. More particularly the present invention is directed to one or more compositions that can be effective against a plurality microorganisms.
- a great many of the current antimicrobial compositions contain antimicrobial agents which are not naturally occurring.
- Typical antimicrobial agents used in sanitizers and disinfectants include chemical disinfectants such as phenolic compounds, quaternary ammonium compounds, strong oxidizer, formaldehyde and halogen containing compounds. Such materials are not of natural origin (i.e. not found in nature) and are prepared through chemical processing and synthesis.
- a great many of these "synthetic" disinfectants cause undesirable effects on both the environment and on human health.
- the concept of formulating disinfectants essentially involving the selection of a simple chemical disinfectant and enhancing its activity by adding other chemicals, evolved in the seventies.
- Disinfectants play a vital role in any biosecurity system, both in the process of terminal disinfection and in the ongoing hygiene maintenance. Apart from relatively minor changes and improvements in formulations, the need for improvement still remains.
- a composition suitable for use as a disinfecting a surface is disclosed herein.
- the composition can be an aqueous solution that comprises from about 0.1 % and 5.0 vol % of at least one active compound derived from at least one natural compound; a liquid material having between 0.5 and 2.0 M free hydrogen and between 100 ppm and 800 ppm calcium, the liquid material present in an amount capable of yielding a solution pH of 6.0 or below when present in the composition; a solubilizer present in an amount between 0 vol % and 5 vol%; a short-chain alcohol present in an amount between 0 and 50 vol%; and water.
- Fig. 2 are mass spectra collected in the negative ionization mode for Dilute
- a solution that can be employed as a disinfectant in certain various situations that is composed of at least one natural material, a liquid material having between 0.5 and 2.0 M free hydrogen and between 100 ppm and 800 ppm calcium, the liquid material present in an amount capable of yielding a solution pH of 6.0 or below when present in the aqueous disinfectant composition and water.
- the composition can also optionally include a suitable solubilizer and/or a short-chain alcohol.
- the active compound can be one that is naturally derived. “Naturally derived’, as the term is used herein includes compounds that can be isolated from biological or botanical material. It is within the purview of this disclosure such material can be artificially synthesized if desired or required. It is contemplated that the active compound that is employed will include at least one phenyl group.
- the active compound that is employed can have the general formula: wherein Ri is one of -OH, an alkenyl group having between 3 and 10 carbon atoms, or an alkoxy group having between 1 and 5 carbon atoms;
- R2 is one of an alkyl group having between 1 and 10 carbon atoms an alkoxy group have between 2 and 5 carbon atoms;
- R3 and R 6 is hydrogen
- R4 is hydrogen, or an alkenyl group having between 3 and 10 carbon atoms and at least one double bond
- R5 is hydrogen or an alkoxy group having between 1 and 5 carbon atoms.
- the group Ri can be an -OH group, an alkenyl group having 3 to 10 carbon atoms or an alkoxy group -OR 7 in which R 7 is alkyl group selected from the group consisting of methyl, ethyl, propyl, isopropyl, butyl and mixtures thereof.
- Ri is an alkenyl group having between 3 and 10 carbon atoms
- group can have at least one double bone with certain embodiments having only one double bond.
- the at least one double bond can be located between the either the distal or proximal two carbon atoms in the alkenyl group.
- the alkenyl group can be selected from the group consisting of propenyl, butenyl, pentenyl, and mixtures thereof.
- the group R2 can be an alkyl group having between 1 and 10 carbon atoms or an alkoxy group having between 2 and 5 carbon atoms.
- the alkyl group can be one of the following: methyl, ethyl , propyl, isopropyl, n-butyl, t-butyl, sec- butyl, isobutyl, n- pentyl, tert-pentyl, neopentyl, isopentyl, sec-pentyl, 3-pentyl, sec-isopentyl and the like.
- the alkoxy group can be -OR 7 in which R 7 is alkyl group selected from the group consisting of methyl, ethyl, propyl, isopropyl, butyl and mixtures thereof.
- the group R4 is hydrogen, or an alkenyl group having between 3 and 10 carbon atoms and at least one double bond.
- the alkenyl group alkenyl group can have at least one double bone with certain embodiments having only one double bond.
- the at least one double bond can be located between the either the distal or proximal two carbon atoms in the alkenyl group.
- the alkenyl group can be selected from the group consisting of propenyl, butenyl, pentenyl, and mixtures thereof.
- the group R5 can be hydrogen or an alkoxy group having between 1 and 5 carbon atoms.
- the alkoxy group can be -OR 7 in which R 7 is alkyl group selected from the group consisting of methyl, ethyl, propyl, isopropyl, butyl and mixtures thereof.
- the active compound can be selected from the group consisting of phenylpropanoids, monoterpenoid phenols, and mixtures thereof.
- Suitable phenylpropanoids can include various organic compounds that are synthesized y plant from amino acids phenylalanine and tyrosine.
- Suitable phenylpropanoid compounds can have a six- carbon phenyl group and a three-carbon propene tail.
- Non-limiting examples of suitable phenylpropanoid compounds can include compounds such as cinnamaldehyde, eugenol, chavicol, safrole, estragole and the like.
- Suitable cinnamaldehyde material can be present as either the cis isomer, the trans- isomer or mixtures thereof and can have the formula:
- the cinnamaldehyde can be incorporated in the composition as pure material. However, it is also within the purview of this disclosure to incorporate the essential oil of cinnamon back into the composition as disclosed herein.
- the cinnamaldehyde material can have a density of 1.0497 g/ml, a boiling point of 248 Cand a refractive index of 1.6195 in its pure form.
- the material can have a molar mass of 164.2 g/mol, a boiling point of 254 C and a density of 1.06 g/cm 3 , a pK a of 10.19 at 25 C and a viscosity of 9.12 mPa at 20 C.
- Monoterpenoid phenols suitable for use in the composition disclosed herein include but are not limited to thymol, carvacrol and the like.
- the active compound as disclosed herein can be present in an amount sufficient to impart antimicrobial properties to the assocaited aqueous disinfectant composition when in admixture with one or more of the materials present therein. In certain embodiments, the active compound or compounds as disclosed herein can be present in an amount between 0.1 and 5.0 vol%.
- the active compound can be present in amounts between 0.1 and 4.0 vol %; between 0.1 and 3 vol %; between 0.1 and 2.0 vol %; between 0.1 and 1.0 vol %; between 0.1 and 0.5 vol %; 0.1 and 0.25 vol %; between 0.2 and 4.0 vol %; between 0.2 and 3.0 vol %; between 0.2 and 2.0 vol %; between 0.2 and 1.0 vol %; between 0.2 and 0.5 vol %; 0.2 and 0.25 vol %; between 0.2 and 4.0 vol %; between 0.3 and 3.0 vol %; between 0.3 and 2.0 vol %; between 0.3 and 1.0 vol %; between 0.3 and 0.5 vol %; between 0.5 and 4.0 vol %; between 0.5 and 3.0 vol %; between 0.5 and 2 vol %; between 0.5 and 1 vol %; between 1.0 and 4.0 vol %; between 1.0 and 3 vol %; between 1.0 and 2.0 vol %; between 2.0 and 4.0 vol %; between 2.0 and
- the active material as disclosed herein can be present as a single compound or in suitable admixture with another active compounds.
- the present disclosure is predicated, at least in part on the unexpected discovery that the aforementioned active compound(s) can exhibit antimicrobial activity or enhanced antimicrobial activity when present in admixure in the composition as disclosed herein. It has been found unexpectedly compositions as disclosed herein, when applied to surfaces such as hard surfaces can reduce or eliminate pathogens present on the assocaited surface.
- Non-limiting examples of such pathogens can include athogens such as such as those within the family Paramyxoviridae (such as measles morbillivims), Herpesviridae (such as varicella- zoster virus); Mycobacteriaceae (such as mycobacterium tuberculosis); Orthomyxoviridae (such as influenzavirus A, influenzavirus B); Picornavivdae (such as enterovirus, poliovirus, coxsackie A viruses, coxsackie B viruses and the like); Calicivirdae (such as noroviruses); Coronaviridea including the subfamily Orthocoronavirinae (such as beta coronaviruses like SARS-CoV, SARS-CoV-2, MERS-CoV); Adenoviridae and the like, Staphylococcaceae (such as staphyloccoccu aureus, like methicillin-resistant Staphylococcus aureus); Enterococcaceae
- the aqueous disinfectant formulation as disclosed herein can also include a liquid material component having between 0.5 and 2.0 M free hydrogen and between 100 ppm and 800 ppm calcium, the liquid material present in an amount capable of yielding a solution pH of 6.0 or below when present in the aqueous disinfectant composition.
- the free hydrogen present in the liquid composition can be derived from one or more suitable inorganic acids in whole or on part as a dissociated state.
- the suitable inorganic acid present in a whole or partially dissociated state can be selected from the group consisting of sulfuric acid, carbonic acid, oxalic acid, chromic acid, pyrophosphoric acid, phosphoric acid, and mixtures thereof.
- the inorganic acid component can be present in the aqueous disinfectant composition material solution in an amount between 1 vol% and 8 vol%; between 1 vol % and 7 vol%; between 1 vol% and 6 vol %; between 1 vol% and 5 vol%; between 1 vol% and 4 vol% between 1 vol % and 3 vol%; between 1 vol% and 2 vol%; between 2 vol% and 8 vol%; between 2 vol % and 7 vol%; between 2 vol% and 6 vol %; between 2 vol% and 5 vol%; between 2 vol% and 4 vol% between 2 vol % and 3 vol%; between 1 vol% and 8 vol%; between 1 vol % and 7 vol%; between 1 vol% and 6 vol %; between 1 vol% and 5 vol%; between 1 vol% and 4 vol% between 1 vol % and 3 vol%; between 1 vol% and 2 vol%; between 3 vol% and 8 vol%; between 3 vol % and 7 vol%; between 3 vol% and 6 vol%; between 3 vol% and 5 vol%; between 3 vol% and 8 vol%
- the free hydrogen content is associated with or derived from sulfuric acid
- the material will be present as a mixture of ions including one or more of hydrogen sulfate (HSC ), sulfate (SO4 2 ), and calcium sulfate in soluble form.
- the predominant ions present in the aqueous disinfectant formulation material solution will be present as hydrogen sulfate (HSO4 ) ⁇
- the free hydrogen present in the liquid material can be between 0.5 M and 2.0M in certain embodiments; between 0.5 and 1.8M free hydrogen, between 0.5 and 1.6M; between 0.5 and 1.5M; between 0.5 and 1.3M; between 0.5 and 1.0M; between 0.5 and 0.8M; between 0.75 and 2.0; between 0.75 and 1.8M; between 0.75 and 1.7M; between 0.75 and 1.6M; between 0.75 and 1.5M; between 0.75 and 1.25M; between 0.75 and 1.0M; between 0.75 and 0.9M; between 1.0 and 2.0M and 1.0 and 1.8M; between 1.0 and 1.7M; between 1.0 and 1.6M; between 1.0 and 1.5M; between 1.0 and 1.25M; between [0027]
- the aforementioned compounds can be present in a suitable liquid material.
- Non-limiting examples of suitable materials include water of a sufficient purity level to facilitate the availability of the component materials and suitability for end-use applications.
- the water component of the liquid material can be material that is classified as ASTM D1193-06 primary grade.
- the water component, the water can be purified by any suitable method, including, but not limited to, distillation, double distillation, deionization, demineralization, reverse osmosis, carbon filtration, ultrafiltration, ultraviolet oxidization, microporous filtration, electrodialysis and the like. In certain embodiments, was having a conductivity between 0.05 and 2.00 micro siemens can be employed.
- the water component of the liquid material can be composed of water having a purity greater than primary grade, if desired or required. Water classified as ASTM1 193-96 purified, ASTM1193-96 ultrapure or higher can be used is desired or required.
- the liquid composition component can also contain between 100 ppm and 800 ppm calcium with a major portion being present as calcium ions. In certain embodiments, the calcium ions can be present as Ca 2+ , CaSC , and mixtures thereof.
- the aqueous disinfectant formulation material can contain between 200 ppm and 800 ppm; between 300 ppm and 800 ppm; between 400 ppm and 800 ppm; between 500 ppm and 800 ppm; between 600 ppm and 800 ppm; between 700 ppm and 800 ppm; between 200 ppm and 700 ppm; between 300 ppm and 700 ppm; between 400 ppm and 700 ppm; between 500 ppm and 700 ppm; between 600 ppm and 700 ppm; between 200 ppm and 600 ppm; between 300 ppm and 600 ppm; between 400 ppm and 600 ppm; between 500 ppm and 600 ppm; between 200 ppm and 500 ppm; between 200 ppm and 400 ppm; between 200 ppm and 300 ppm.
- the liquid material as defined herein can be present in an aqueous material in an amount sufficient to provide the resulting aqueous disinfectant composition with a pH less than 6.0 while in other embodiments, the liquid material can be present in an amount sufficient to provide the resulting aqueous disinfectant formulation with a pH less than 5.5; less than 5.0; 4.5; less than 4.0, less than 3.5; less than 3.0; less than 2.5; less than 2.4; less than 2.3; less than 2.3; less than 2.1; less than 2.0.
- the liquid material that is admixed to form the aqueous disinfectant formulation can be produced by a variety of suitable means provided that the resulting material exhibits reduced or no harmful interaction with tissue such as mucosal tissue.
- One non-limited example or a suitable formulation process is as follows.
- the liquid material as disclosed herein can be formed by the addition of a suitable inorganic hydroxide to a suitable inorganic acid.
- Suitable acids acid may have a density between 22° and 70° baume; with specific gravities between about 1.18 and 1.93.
- the inorganic acid will have a density between 50° and 67° baume; with specific gravities between 1.53 and 1.85.
- the inorganic acid can be either a monoatomic acid or a polyatomic acid.
- the inorganic acid employed can be homogenous or can be a mixture of various acid compounds that fall within the defined parameters. It is also contemplated that the acid may be a mixture that includes one or more acid compounds that fall outside the contemplated parameters but in combination with other materials will provide an average acid composition value in the range specified.
- the inorganic acid or acids employed can be of any suitable grade or purity. In certain instances, tech grade and/or food grade material can be employed successfully in various applications. Where desired or required, inorganic acids of even higher purity can be employed.
- the inorganic acid can be contained in any suitable reaction vessel in liquid form at any suitable volume.
- the reaction vessel can be non-reactive beaker of suitable volume.
- the volume of acid employed can be as small as 50 ml. Larger volumes up to and including 5000 gallons or greater are also considered to be within the purview of this disclosure.
- the inorganic acid can be maintained in the reaction vessel at a suitable temperature such as a temperature at or around ambient. It is within the purview of this disclosure to maintain the initial inorganic acid in a range between approximately 23° and about 70°C. However lower temperatures in the range of 15° and about 40°C can also be employed.
- the inorganic acid is agitated by suitable means to impart mechanical energy in a range between approximately 0.5 HP and 3 HP with agitation levels imparting mechanical energy between 1 and 2.5 HP being employed in certain applications of the process.
- suitable ranges for imparting levels of mechanical energy include between 0.5 HP and 2.5 HP; between 0.5 HP and 2.0 HP; between 0.5 HP and 2.0 HP; between 0.5 HP and 1.5 HP; between 0.5 HP and 1.0 HP; Between 1.0 HP and 3.0 HP; between 1.0 HP and 2.5 HP; between 1.0 HP and 2.0 HP; between 1.0 HP and 1.5 HP; between 1.5 HP and 3.0 HP; between 1.5 HP and 2.5 HP; between 1.5 HP and 2.0 HP; between 2.0 HP and 3.0 HP; between 2.5 HP and 3.0 HP.
- Agitation can be imparted by a variety of suitable mechanical means including, but not limited to, DC servo drive, electric impeller, magnetic stirrer, chemical inductor and the like. Agitation can commence at an interval immediately prior to hydroxide addition and can continue for an interval during at least a portion of the hydroxide introduction step.
- the acid material of choice may be a concentrated acid with an average molarity (M) of at least 7 or above. In certain procedures, the average molarity will be at least 10 or above; with an average molarity between 7 and 10 being useful in certain applications.
- the acid material of choice employed may exist as a pure liquid, a liquid slurry or as an aqueous solution of the dissolved acid in essentially concentrated form.
- Suitable acid materials can be either aqueous or non-aqueous materials.
- Non limiting examples of suitable acid materials can include one or more of the following: hydrochloric acid, nitric acid, phosphoric acid, chloric acid, perchloric acid, chromic acid, sulfuric acid, permanganic acid, prussic acid, bromic acid, hydrobromic acid, hydrofluoric acid, iodic acid, fluoboric acid, fluosilicic acid, fluotitanic acid.
- the defined volume of a liquid concentrated strong acid employed can be sulfuric acid having a specific gravity between 55° and 67° baume. This material can be placed in the reaction vessel and mechanically agitated at a temperature between 16° and 70°C.
- a measured, defined quantity of suitable hydroxide material can be added to an agitating acid, such as concentrated sulfuric acid, that is present in the non-reactive vessel in a measured, defined amount.
- the amount of hydroxide that is added will be that sufficient to produce a solid material that is present in the composition as a precipitate and/or a suspended solid or colloidal suspension.
- the hydroxide material employed can be a water-soluble or partially water-soluble inorganic hydroxide.
- Partially water-soluble hydroxides employed in the process as disclosed herein will generally be those which exhibit miscibility with the acid material to which they are added.
- suitable partially water-soluble inorganic hydroxides will be those that exhibit at least 50% miscibility in the associated acid.
- the inorganic hydroxide can be either anhydrous or hydrated.
- Non-limiting examples of water-soluble inorganic hydroxides include water soluble alkali metal hydroxides, alkaline earth metal hydroxides and rare earth hydroxides; either alone or in combination with one another. Other hydroxides are also considered to be within the purview of this disclosure.
- Water- solubility as the term is defined in conjunction with the hydroxide material that will be employed is defined a material exhibiting dissolution characteristics of 75% or greater in water at standard temperature and pressure.
- the hydroxide that is utilized typically is a liquid material that can be introduced into the acid material. The hydroxide can be introduced as a true solution, a suspension or a super- saturated slurry.
- the concentration of the inorganic hydroxide in aqueous solution can be dependent on the concentration of the associated acid to which it is introduced.
- suitable concentrations for the hydroxide material are hydroxide concentrations greater than 5 to 50% of a 5-mole material.
- Suitable hydroxide materials include, but are not limited to, lithium hydroxide, sodium hydroxide, potassium hydroxide, ammonium hydroxide, calcium hydroxide, strontium hydroxide, barium hydroxide, magnesium hydroxide, and/or silver hydroxide.
- Inorganic hydroxide solutions when employed may have concentration of inorganic hydroxide between 5 and 50% of a 5-mole material, with concentration between 5 and 20% being employed in certain applications.
- the inorganic hydroxide material in certain processes, can be calcium hydroxide in a suitable aqueous solution such as is present as slaked lime.
- the inorganic hydroxide in liquid or fluid form is introduced into the agitating acid material in one or more metered volumes over a defined interval to provide a defined resonance time.
- the resonance time in the process as outlined is considered to be the time interval necessary to promote and provide the environment in which the hydronium ion material as disclosed herein develops.
- the resonance time interval as employed in the process as disclosed herein is typically between 12 and 120 hours with resonance time intervals between 24 and 72 hours and increments therein being utilized in certain applications.
- the inorganic hydroxide is introduced into the acid at the upper surface of the agitating volume in a plurality of metered volumes.
- the total amount of inorganic hydroxide material will be introduced as a plurality of measured portions over the resonance time interval.
- Front-loaded metered addition being employed in many instances.
- “Front-loaded metered addition”, as the term is used herein, is taken to mean addition of the total hydroxide volume with a greater portion being added during the initial portion of the resonance time.
- An initial percentage of the desired resonance time considered to be between the first 25% and 50% of the total resonance time.
- each metered volume that is added can be equal or can vary based on such non-limiting factors as external process conditions, in situ process conditions, specific material characteristics, and the like. It is contemplated that the number of metered volumes can be between 3 and 12.
- the interval between additions of each metered volume can be between 5 and 60 minutes in certain applications of the process as disclosed. The actual addition interval can be between 60 minutes to five hours in certain applications.
- a 100 ml volume of 5% weight per volume of calcium hydroxide material is added to 50 ml of 66° baume concentrated sulfuric acid in 5 metered increments of 2 ml per minute, with or without admixture.
- Addition of the hydroxide material to the sulfuric acid produces a material having increasing liquid turbidity.
- Increasing liquid turbidity is indicative of calcium sulfate solids forming as precipitate.
- the produced calcium sulfate can be removed in a fashion that is coordinated with continued hydroxide addition in order to provide a coordinated concentration of suspended and dissolved solids.
- Solid material generated during the process and present as precipitate or suspended solids can be removed by any suitable means.
- removal means include, but need not be limited to, the following: gravimetric, forced filtration, centrifuge, reverse osmosis and the like.
- the resulting liquid is a shelf-stable material that is believed to be shelf stable when stored at ambient temperature and between 50 and 75% relative humidity.
- the material can have a molarity between 1.87 to 1.78 molar and can contain between 3% and 10% of total moles of acid protons that are not charge balanced.
- the liquid material can contain between 4% and 9% of total moles of acid protons that are charge balanced; between 5% and 9% of total moles of charge balanced acid; between 6% and 9% of total moles of charge balanced acid; between 7% and 9% of total moles of charge balanced acid; between 8% and 9% of total moles of charge balanced acid.
- the resulting material can be further purified as suitable and can be employed as the liquid material in the biocompatible material solution as disclosed herein. It is also within the purview of this disclosure to subject the resulting material to further processing as desired or required. Non-limiting examples of such processing can include subjecting the resulting fluid to as suitable magnetic field or fields.
- the resulting liquid material can be subjected to a non-bi- polar magnetic field at a value greater than 2000 gauss; with magnetic fields greater than 2 million gauss being employed in certain applications. It is contemplated that a magnetic field between 10,000 gauss and 2 million gauss can be employed in certain situations.
- Suitable ranges include between 10,000 gauss and 20,000 gauss; between 10,000 gauss and 30,000 gauss; between 10,000 gauss and 40,000 gauss; between 10,000 gauss and 50,000 gauss; between 10,000 gauss and 60,000 gauss; between 10,000 gauss and 70,000 gauss; between 10,000 gauss and 80,000 gauss; between 10,000 gauss and 90,000 gauss; between 10,000 gauss and 100,000 gauss; between 50,000 gauss and 100,000 gauss; between 50,000 gauss and 150,000 gauss; between 50,000 gauss between 200,000 gauss; between 50,000 gauss and 250,000 gauss; between 100,000 gauss and 200,000 gauss; between 100,000 gauss and 250,000 gauss; between 100,000 gauss and 300,000 gauss; between 100,000 gauss and 350,000 gauss; between 100,000 gauss and
- Solid material generated during the process and present as precipitate or suspended solids can be removed by any suitable means.
- removal means include, but need not be limited to, the following: gravimetric, forced filtration, centrifuge, reverse osmosis and the like.
- the resulting liquid as disclosed herein is a shelf-stable viscous liquid that is believed to be stable for at least one year when stored at ambient temperature and between 50 to 75% relative humidity.
- the stable electrolyte composition of matter can be use neat in various end use applications.
- the stable electrolyte composition of matter can have a 1.87 to 1.78 molar material that contains 8 to 9 % of the total moles of acid protons that are not charged balanced.
- the liquid material that results from the process as disclosed herein can have a molarity between 200 M to 150 M strength and 187 to 178 M strength in certain instances, when measured titrimetrically though hydrogen coulometry and via FTIR spectral analysis.
- the material has a gravimetric range greater than 1.15; with ranges greater than 1.9 in in certain instances.
- the material when analyzed, is shown to yield up to 1300 volumetric times of orthohydrogen per cubic ml versus hydrogen contained in a mole of water.
- liquid material as disclosed herein may serve as a source of acid protons when introduced into the biocompatible material as contemplated herein.
- the resulting material will present with a pH at 5.0 or below without the assocaited level of corrosivity. It is believed that the resulting composition contains an elevated level of acid protons present as HSCL . Without being bound by any theory, it is believed that elevated levels of HSQf ions present in the resulting composition may moderate the corrosive characteristics of the resulting composition permitting it to be administered to patients in a suitable biocompatible material solution at a composition pH below 5.0; below 4.5; below 4.0; below 3.5; below 3.0; below 2.5; below 2.0. In certain embodiments, the composition pH can be between 1.5 and 3.5; between 2.0 and 3.5; between 2.5 and 3.5. The administration of the biocompatible material solution as disclosed herein can proceed without substantial deleterious effect on the patient tissue that is contacted.
- the liquid material as disclosed herein can be formed by the addition of a suitable inorganic hydroxide to a suitable inorganic acid.
- Suitable acids acid may have a density between 22° and 70° baume; with specific gravities between about 1.18 and 1.93. In certain embodiments, it is contemplated that the inorganic acid will have a density between 50° and 67° baume; with specific gravities between 1.53 and 1.85.
- the inorganic acid can be either a monoatomic acid or a polyatomic acid.
- the inorganic acid employed can be homogenous or can be a mixture of various acid compounds that fall within the defined parameters. It is also contemplated that the acid may be a mixture that includes one or more acid compounds that fall outside the contemplated parameters but in combination with other materials will provide an average acid composition value in the range specified.
- the inorganic acid or acids employed can be of any suitable grade or purity. In certain instances, tech grade and/or food grade material can be employed successfully in various applications. Where desired or required, inorganic acids of even higher purity can be employed.
- the inorganic acid can be contained in any suitable reaction vessel in liquid form at any suitable volume.
- the reaction vessel can be non-reactive beaker of suitable volume.
- the volume of acid employed can be as small as 50 ml. Larger volumes up to and including 5000 gallons or greater are also considered to be within the purview of this disclosure.
- the inorganic acid can be maintained in the reaction vessel at a suitable temperature such as a temperature at or around ambient. It is within the purview of this disclosure to maintain the initial inorganic acid in a range between approximately 23° and about 70°C. However lower temperatures in the range of 15° and about 40°C can also be employed.
- the inorganic acid is agitated by suitable means to impart mechanical energy in a range between approximately 0.5 HP and 3 HP with agitation levels imparting mechanical energy between 1 and 2.5 HP being employed in certain applications of the process.
- suitable ranges for imparting levels of mechanical energy include between 0.5 HP and 2.5 HP; between 0.5 HP and 2.0 HP; between 0.5 HP and 2.0 HP; between 0.5 HP and 1.5 HP; between 0.5 HP and 1.0 HP; Between 1.0 HP and 3.0 HP; between 1.0 HP and 2.5 HP; between 1.0 HP and 2.0 HP; between 1.0 HP and 1.5 HP; between 1.5 HP and 3.0 HP; between 1.5 HP and 2.5 HP; between 1.5 HP and 2.0 HP; between 2.0 HP and 3.0 HP; between 2.5 HP and 3.0 HP.
- Agitation can be imparted by a variety of suitable mechanical means including, but not limited to, DC servo drive, electric impeller, magnetic stirrer, chemical inductor and the like. Agitation can commence at an interval immediately prior to hydroxide addition and can continue for an interval during at least a portion of the hydroxide introduction step.
- the acid material of choice may be a concentrated acid with an average molarity (M) of at least 7 or above. In certain procedures, the average molarity will be at least 10 or above; with an average molarity between 7 and 10 being useful in certain applications.
- the acid material of choice employed may exist as a pure liquid, a liquid slurry or as an aqueous solution of the dissolved acid in essentially concentrated form.
- Suitable acid materials can be either aqueous or non-aqueous materials.
- Non limiting examples of suitable acid materials can include one or more of the following: hydrochloric acid, nitric acid, phosphoric acid, chloric acid, perchloric acid, chromic acid, sulfuric acid, permanganic acid, prussic acid, bromic acid, hydrobromic acid, hydrofluoric acid, iodic acid, fluoboric acid, fluosilicic acid, fluotitanic acid.
- the defined volume of a liquid concentrated strong acid employed can be sulfuric acid having a specific gravity between 55° and 67° baume. This material can be placed in the reaction vessel and mechanically agitated at a temperature between 16° and 70°C.
- a measured, defined quantity of suitable hydroxide material can be added to an agitating acid, such as concentrated sulfuric acid, that is present in the non-reactive vessel in a measured, defined amount.
- the amount of hydroxide that is added will be that sufficient to produce a solid material that is present in the composition as a precipitate and/or a suspended solid or colloidal suspension.
- the hydroxide material employed can be a water-soluble or partially water-soluble inorganic hydroxide.
- Partially water-soluble hydroxides employed in the process as disclosed herein will generally be those which exhibit miscibility with the acid material to which they are added.
- suitable partially water-soluble inorganic hydroxides will be those that exhibit at least 50% miscibility in the associated acid.
- the inorganic hydroxide can be either anhydrous or hydrated.
- Non-limiting examples of water-soluble inorganic hydroxides include water soluble alkali metal hydroxides, alkaline earth metal hydroxides and rare earth hydroxides; either alone or in combination with one another. Other hydroxides are also considered to be within the purview of this disclosure.
- Water- solubility as the term is defined in conjunction with the hydroxide material that will be employed is defined a material exhibiting dissolution characteristics of 75% or greater in water at standard temperature and pressure.
- the hydroxide that is utilized typically is a liquid material that can be introduced into the acid material. The hydroxide can be introduced as a true solution, a suspension or a super- saturated slurry.
- the concentration of the inorganic hydroxide in aqueous solution can be dependent on the concentration of the associated acid to which it is introduced.
- suitable concentrations for the hydroxide material are hydroxide concentrations greater than 5 to 50% of a 5-mole material.
- Suitable hydroxide materials include, but are not limited to, lithium hydroxide, sodium hydroxide, potassium hydroxide, ammonium hydroxide, calcium hydroxide, strontium hydroxide, barium hydroxide, magnesium hydroxide, and/or silver hydroxide.
- Inorganic hydroxide solutions when employed may have concentration of inorganic hydroxide between 5 and 50% of a 5-mole material, with concentration between 5 and 20% being employed in certain applications.
- the inorganic hydroxide material in certain processes, can be calcium hydroxide in a suitable aqueous solution such as is present as slaked lime.
- the inorganic hydroxide in liquid or fluid form is introduced into the agitating acid material in one or more metered volumes over a defined interval to provide a defined resonance time.
- the resonance time in the process as outlined is considered to be the time interval necessary to promote and provide the environment in which the hydronium ion material as disclosed herein develops.
- the resonance time interval as employed in the process as disclosed herein is typically between 12 and 120 hours with resonance time intervals between 24 and 72 hours and increments therein being utilized in certain applications.
- the inorganic hydroxide is introduced into the acid at the upper surface of the agitating volume in a plurality of metered volumes.
- the total amount of inorganic hydroxide material will be introduced as a plurality of measured portions over the resonance time interval.
- Front-loaded metered addition being employed in many instances. “Front-loaded metered addition”, as the term is used herein, is taken to mean addition of the total hydroxide volume with a greater portion being added during the initial portion of the resonance time. An initial percentage of the desired resonance time - considered to be between the first 25% and 50% of the total resonance time.
- each metered volume that is added can be equal or can vary based on such non-limiting factors as external process conditions, in situ process conditions, specific material characteristics, and the like. It is contemplated that the number of metered volumes can be between 3 and 12.
- the interval between additions of each metered volume can be between 5 and 60 minutes in certain applications of the process as disclosed. The actual addition interval can be between 60 minutes to five hours in certain applications.
- a 100 ml volume of 5% weight per volume of calcium hydroxide material is added to 50 ml of 66° baume concentrated sulfuric acid in 5 metered increments of 2 ml per minute, with or without admixture.
- Addition of the hydroxide material to the sulfuric acid produces a material having increasing liquid turbidity.
- Increasing liquid turbidity is indicative of calcium sulfate solids forming as precipitate.
- the produced calcium sulfate can be removed in a fashion that is coordinated with continued hydroxide addition in order to provide a coordinated concentration of suspended and dissolved solids.
- Solid material generated during the process and present as precipitate or suspended solids can be removed by any suitable means.
- removal means include, but need not be limited to, the following: gravimetric, forced filtration, centrifuge, reverse osmosis and the like.
- the resulting liquid is a shelf-stable material that is believed to be shelf stable when stored at ambient temperature and between 50 and 75% relative humidity.
- the material can have a molarity between 1.87 to 1.78 molar and can contain between 3% and 10% of total moles of acid protons that are not charge balanced.
- the liquid material can contain between 4% and 9% of total moles of acid protons that are charge balanced; between 5% and 9% of total moles of charge balanced acid; between 6% and 9% of total moles of charge balanced acid; between 7% and 9% of total moles of charge balanced acid; between 8% and 9% of total moles of charge balanced acid.
- the resulting material can be further purified as suitable and can be employed as the liquid material in the biocompatible material solution as disclosed herein. It is also within the purview of this disclosure to subject the resulting material to further processing as desired or required. Non-limiting examples of such processing can include subjecting the resulting fluid to as suitable magnetic field or fields.
- the resulting liquid material can be subjected to a non-bi- polar magnetic field at a value greater than 2000 gauss; with magnetic fields greater than 2 million gauss being employed in certain applications. It is contemplated that a magnetic field between 10,000 gauss and 2 million gauss can be employed in certain situations.
- Suitable ranges include between 10,000 gauss and 20,000 gauss; between 10,000 gauss and 30,000 gauss; between 10,000 gauss and 40,000 gauss; between 10,000 gauss and 50,000 gauss; between 10,000 gauss and 60,000 gauss; between 10,000 gauss and 70,000 gauss; between 10,000 gauss and 80,000 gauss; between 10,000 gauss and 90,000 gauss; between 10,000 gauss and 100,000 gauss; between 50,000 gauss and 100,000 gauss; between 50,000 gauss and 150,000 gauss; between 50,000 gauss between 200,000 gauss; between 50,000 gauss and 250,000 gauss; between 100,000 gauss and 200,000 gauss; between 100,000 gauss and 250,000 gauss; between 100,000 gauss and 300,000 gauss; between 100,000 gauss and 350,000 gauss; between 100,000 gauss and
- Solid material generated during the process and present as precipitate or suspended solids can be removed by any suitable means.
- removal means include, but need not be limited to, the following: gravimetric, forced filtration, centrifuge, reverse osmosis and the like.
- the resulting liquid as disclosed herein is a shelf-stable viscous liquid that is believed to be stable for at least one year when stored at ambient temperature and between 50 to 75% relative humidity.
- the stable electrolyte composition of matter can be use neat in various end use applications.
- the stable electrolyte composition of matter can have a 1.87 to 1.78 molar material that contains 8 to 9 % of the total moles of acid protons that are not charged balanced.
- the liquid material that results from the process as disclosed herein can have a molarity between 200 M to 150 M strength and 187 to 178 M strength in certain instances, when measured titrimetrically though hydrogen coulometry and via FTIR spectral analysis.
- the material has a gravimetric range greater than 1.15; with ranges greater than 1.9 in in certain instances.
- the material when analyzed, is shown to yield up to 1300 volumetric times of orthohydrogen per cubic ml versus hydrogen contained in a mole of water.
- liquid material as disclosed herein may serve as a source of acid protons when introduced into the biocompatible material as contemplated herein.
- the resulting material will present with a pH at 5.0 or below without the assocaited level of corrosivity. It is believed that the resulting composition contains an elevated level of acid protons present as HSCU .
- the aqueous disinfectant formulation can also optionally include a solubilizer.
- the solubilizer can be a surfactant capable of solubilizing the active material in an aqueous diluent such as water.
- a solubilizer can be a surfactant capable of solubilizing the active material in an aqueous diluent such as water.
- Suitable zwitterionic surfactants include, but are not limited to, materials such as lauryldimethylamine oxide, myristamine oxide, alkyl imidazolines, alkyl amines, as well as mixtures thereof.
- Non-limiting examples of suitable non-ionic surfactants include ethylene oxide adducts of Csto Cu alcohols, ethylene oxide/propylene oxide adducts of ethylene glycol, alkylene glycols, and mixtures thereof.
- suitable anionic surfactants include alkyl sulfonates and alkyl aryl sulfonates having about 8 to about 22 carbon atoms in the alkyl portion, alkali metal salts or mixtures thereof.
- the surfactant material can be present in an amount between 0 and
- the aqueous disinfectant formulation as disclosed herein can also contain a suitable short-chain alcohol component.
- the short-chain alcohol component when present, can be present in an amount between 0.1 and 50 vol%, with concentrations between 0.1 and 3 vol% being employed in certain embodiments.
- suitable alcohols include but are not limited to, Ci to Ce straight-chained or branched alcohols such as ethanol, methanol, propanol, isopropanol, butanol and mixtures thereof.
- the formulation can also include one or more weak organic acids which, when present, can be present in amounts between 0.1 and 2% and can be selected form the group consisting of and acetic acid, hydroxyacetic acid, citric acid, tartaric acid, maleic acid, fumaric acid and mixtures thereof.
- the formulation can also include a carboxylic acid component composed of ca carboxylic acid having the general formula: wherein Ri is an unsaturated hydrocarbon moiety having between four and fourteen carbon atoms or a hydrocarbon moiety having between four and fourteen carbon atoms and at least one double bond; and wherein R 2 is a one of -H, -OH, or -CH 3..
- the carboxylic acid compound can be selected from the group consisting of hexanoic acid, octanoic acid, decanoic acid, dodecanoic acid and mixtures thereof
- the carboxylic acid component can be present in an amount between 0.1 and 3.0 vol% .
- the formulation can also include a biosurfactant present in an amount between 0.1vol% and 3.0 vol% such as those selected from the group consisting of rhamnolipid, sophorolipids, lecithins, steroid acids conjugated with taurine, steroid acids conjugated with glycine.
- a biosurfactant present in an amount between 0.1vol% and 3.0 vol% such as those selected from the group consisting of rhamnolipid, sophorolipids, lecithins, steroid acids conjugated with taurine, steroid acids conjugated with glycine.
- material prepared by the process as disclosed herein may contain and elevated level of hydronium ions that can be stably present, in the whole or in part, in the resulting biocompatible material.
- the ion complex in the biocompatible material solution is generally stable and capable of functioning as an oxygen donor in the presence ofthe environment created to generate the same.
- the material may have any suitable structure and solvation that is generally stable and capable of functioning as an oxygen donor.
- Particular embodiments of the resulting solution will include a concentration of the ion as depicted by the following formula: wherein x is an odd integer > 3.
- hydronium ion complex can be broadly defined as the cluster ofmolecules that surround the cation ⁇ l ⁇ + where x is an integer greater than or equal to 3.
- the hydronium ion complex may include at least four additional hydrogen molecules and a stoichiometric proportion of oxygen molecules complexed thereto as water molecules.
- hydronium ion will be present as a population of ion configurations with elevated levels of hydronium ions in which x is an odd integer that is 9 or greater. In certain embodiments, the hydronium ion will be present as a population of ion configurations with elevated levels of hydronium ions in which x is an odd integer that is 21 or greater.
- hydronium ion complexes will exist as solvated structures of hydronium ions having the formula: wherein x is an integer between 1 and 4; and y is an integer between 0 and 2.
- an 4- core is protonated by multiple H2O molecules.
- the hydronium complexes present in the composition of matter as disclosed herein can exist as Eigen complex cations, Zundel complex cations or mixtures of the two.
- the Eigen solvation structure can have the hydronium ion at the center of an H9O4+ structure with the hydronium complex being strongly bonded to three neighboring water molecules.
- the Zundel solvation complex can be an H5O2+ complex in which the proton is shared equally by two water molecules.
- the solvation complexes typically exist in equilibrium between Eigen solvation structure and Zundel solvation structure.
- therespective solvation structure complexes generally existed in an equilibrium state that favors the Zundel solvation structure.
- the present disclosure is based, at least in part, on the unexpected discovery that stable materials can be produced in which hydronium ion exists in an equilibrium state that favors the Eigen complex.
- the present disclosure is also predicated on the unexpected discovery that increases in the concentration of the Eigen complex in a process stream can provide a class of novel enhanced oxygen-donor oxonium materials.
- the process stream as disclosed herein can have an Eigen solvation state to
- Zundel solvation state ratio between 1.2 to 1 and 15 to 1 in certain embodiments; with ratios between 1.2 to 1 and 5 to 1 in other embodiments.
- the novel enhanced oxygen-donor oxonium material as disclosed herein can be generally described as a thermodynamically stable aqueous acid solution that is buffered with an excess of proton ions.
- the excess of protons ions can be in an amount between 10% and 50% excess hydrogen ions as measured by free hydrogen content.
- a first embodiment of the liquid material as disclosed herein is prepared by the following method. Several units of (50) ml of concentrated liquid sulfuric acid having a mass fraction H 2 SO4 of 98%, an average molarity(M) above 7 and a specific gravity of 66 0 baume are placed in respective non-reactive vessels and maintained at 25°C with agitation by a magnetic stirrer to impart mechanical energy of 1 HP to the liquid.
- a measured quantity of sodium hydroxide is added to the upper surface of each of the agitating acid material.
- the sodium hydroxide material employed is a 20% aqueous solution of 5M calcium hydroxide and is introduced into each of the respective units in five metered volumes introduced at a rate of 2 ml per minute over an interval of five hours with to provide a resonance time of 24 hours. The introduction interval for each metered volume is 30 minutes.
- Turbidity is produced in the units with addition of calcium hydroxide to the sulfuric acid indicating formation of calcium sulfate solids.
- the solids in each unit are permitted to precipitate periodically during the process and the precipitate is removed from contact with the reacting solutions.
- the resulting material are each exposed to a non-bi-polar magnetic field of 2400 gauss resulting in the production of observable precipitate and suspended solids for an interval of 2 hours.
- the resulting material units are centrifuged and force filtered to isolate the precipitate and suspended solids from each the liquid material unit.
- the liquid material that is produced is separated as individual samples. Some are stored in closed containers at standard temperature and 50% relative humidity to determine shelf- stability. Other samples are subjected to analytical procedures to determine composition. The test samples are subjected to FTIR spectra analysis and titrated with hydrogen coulometry. The sample material has a molarity ranging from 187 to 178 M strength. The material has a gravimetric range greater than 1.15; with ranges greater than 1.9 in in certain instances. The composition is stable and has a 1.87 to 1.78 molar material that contains 8 to 9 % of the total moles of acid protons that are not charged balanced. Liquid material is collected for further use and analysis.
- a second embodiment of the liquid material as disclosed herein is prepared by introducing 50 ml units of concentrated liquid sulfuric acid having a mass fraction H 2 SO4 of 98%, an average molarity(M) above 7 and a specific gravity of 66 0 baume into a non-reactive vessel and maintaining each at 25°C with agitation by a magnetic stirrer to impart mechanical energy of 1 HP to each liquid unit.
- the sodium hydroxide material employed is a 20% aqueous solution of 5M calcium hydroxide and is introduced in five metered volumes introduced at a rate of 2 ml per minute over an interval of five hours with to provide a resonance time of 24 hours. The introduction interval for each metered volume is 30 minutes.
- Turbidity is produced with addition of calcium hydroxide to the sulfuric acid indicating formation of calcium sulfate solids.
- the solids in each unit are permitted to precipitate periodically during the process and the precipitate is removed from contact with the reacting solution.
- the resulting material is centrifuged and force filtered to isolate the precipitate and suspended solids from the liquid material and respective resulting material units are collected for further use and analysis.
- Example I is admixed in a 5 ml portion of deionized and distilled water at standard temperature and pressure. The excess hydrogen ion concentration is measured as greater than 15 % by volume and the pH of the material is determined to be 1.
- samples of the materials are diluted with deionized water to provide material that contains 1 % by volume of the respective material in water. These samples are evaluated against a dilute sulfuric acid solution, a dilute sulfuric acid solution with to which calcium sulfate is added to yield 300 ppm and a dilute sulfuric with 400 ppm calcium sulfate and well as a reverse osmosis water control. [00106] All samples are diluted in an acid matrix for analysis. The testing is completed using a Thermo iCAP 6300 Duo ICP-OES for calcium and sulfur content following EPA method 200.7.
- Each test material is initially prepared by simple dilution in a 5% nitric acid matrix.
- the calibration standards are prepared in the same acid matrix to match the samples. However, this preparation leads to high recoveries for calcium which is believed to be a result of the sulfuric acid present in the samples but not present in the calibration standards.
- the calibration standards are re-prepared with a small amount of sulfuric acid in order to match the samples, and the analysis repeated in order to provide better QC recoveries that approach 100%.
- the samples are each diluted with de-ionized water for analysis. The testing is completed using a Mettler Toledo Seven Excellence Meter with a conductivity probe following EPA method 120.1. Predicted conductivity results are presented in Table I. TABLE I
- Example I The respective samples of Example I are diluted to produce 5 volume % of the product in water and are found to be shelf stable for at least 12 to 18 months.
- the excess hydrogen ion concentration is measured to be greater than 15% and the pH of the material is determined to be 1.
- compositions are prepared as outlined in the Table V using the percentages of the liquid material described in Example I at concentrations of 2.4 vol% or 4.8 vol% respectively in water.
- a composition is also prepared according to the present disclosure incorporated sulfuric acid to equal the concentration the composition of Example I at 2.4 vol% for comparison.
- the respective materials are free flowing liquids that could be wiped, sprayed or misted onto hard surfaces.
- Examples VI are evaluated to determine whether the respective material kills, in 10-minutes contact time at least 57 of 60 carriers/lot against Staphylococcus aureus and at least 54 of 60 carriers/lot against Pseudimonas aeruginosa using AO AC Official Method 955.15 against S. aureus and AO AC Official Method 964.02 against P. aeruginosa.
- the various materials exhibit between log 6.0 reduction or greater within the test interval.
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Abstract
A composition suitable for use as a disinfecting a surface is disclosed that is an aqueous solution that comprises from about 0.1 % and 5.0 vol % of at least one active compound derived from at least one natural compound; a liquid material having between 0.5 and 2.0 M free hydrogen and between 100 ppm and 800 ppm calcium, the liquid material present in an amount capable of yielding a solution pH of 6.0 or below when present in the composition; a solubilizer present in an amount between 0 vol % and 5 vol%; a short-chain alcohol present in an amount between 0 and 50 vol%; and water.
Description
PROCESS AND COMPOSITION ACTING AS AN ACTIVE, INERT OR ADJUVANT FOR SURFACE TREATMENT AND DISINFECTION
CROSS-REFERENCE TO PENDING APPLICATIONS
[0001] The present application is a non-provisional application claiming priority to U.S.
Provisional Patent Application Serial Number 63/163,924, the contents of which are incorporated by reference herein.
BACKGROUND
[0002] The present disclosure is directed to composition and processes that provide for safe and effective disinfectant functioning against one or more microorganisms. More particularly the present invention is directed to one or more compositions that can be effective against a plurality microorganisms.
[0003] A great many of the current antimicrobial compositions, including sanitizers and disinfectants, contain antimicrobial agents which are not naturally occurring. Typical antimicrobial agents used in sanitizers and disinfectants include chemical disinfectants such as phenolic compounds, quaternary ammonium compounds, strong oxidizer, formaldehyde and halogen containing compounds. Such materials are not of natural origin (i.e. not found in nature) and are prepared through chemical processing and synthesis. A great many of these "synthetic" disinfectants cause undesirable effects on both the environment and on human health. The concept of formulating disinfectants, essentially involving the selection of a simple chemical disinfectant and enhancing its activity by adding other chemicals, evolved in the seventies.
[0004] The enhancement of the activity of a simple chemical disinfectant or combination of simple disinfectants to increase the spectrum of activity frequently involves the addition of additional chemical agents. Such additional chemical agents will generally have an effect on the pH and surface activity of the formulated product once in solution. It is well established that a number of simple disinfectants demonstrate their optimum activity at a specific pH (i.e. acidity or alkalinity). The ability of the disinfectant solution to make complete and even contact with the
surface to be treated is also of great importance. This can generally be achieved by the addition of a surfactant or detergent to the formulation.
[0005] Disinfectants play a vital role in any biosecurity system, both in the process of terminal disinfection and in the ongoing hygiene maintenance. Apart from relatively minor changes and improvements in formulations, the need for improvement still remains.
[0006] While some natural plant oils have been known since antiquity to have curative properties, the topical and oral benefits of natural plant oils have more recently been attributed to antimicrobial properties. It would be desirable to provide surface contact composition that can clean and/or sanitize the relevant surface.
SUMMARY
[0007] A composition suitable for use as a disinfecting a surface is disclosed herein. The composition can be an aqueous solution that comprises from about 0.1 % and 5.0 vol % of at least one active compound derived from at least one natural compound; a liquid material having between 0.5 and 2.0 M free hydrogen and between 100 ppm and 800 ppm calcium, the liquid material present in an amount capable of yielding a solution pH of 6.0 or below when present in the composition; a solubilizer present in an amount between 0 vol % and 5 vol%; a short-chain alcohol present in an amount between 0 and 50 vol%; and water.
BRIEF DESCRIPTION OF THE DRAWINGS [0008] The various features, advantages and other uses of the present apparatus will become more apparent by referring to the following detailed description and drawing in which: [0009] Fig. 1 are mass spectra collected in the positive ionization mode for Dilute
Sulfuric Acid w/ 400 ppm CaSCU (A), Dilute Sulfuric Acid (B), an embodiment as disclosed herein prepared according to the process outlined in Example I (C), and Reverse Osmosis Water (D);
[0010] Fig. 2 are mass spectra collected in the negative ionization mode for Dilute
Sulfuric Acid w/ 400 ppm CaS04 (A), Dilute Sulfuric Acid (B), and embodiment as disclosed herein prepared according to the process outlined in Example I (C), and Reverse Osmosis Water (D).
DETAILED DESCRIPTION
[0011] Disclosed herein is a solution that can be employed as a disinfectant in certain various situations that is composed of at least one natural material, a liquid material having between 0.5 and 2.0 M free hydrogen and between 100 ppm and 800 ppm calcium, the liquid material present in an amount capable of yielding a solution pH of 6.0 or below when present in the aqueous disinfectant composition and water. The composition can also optionally include a suitable solubilizer and/or a short-chain alcohol.
[0012] The active compound can be one that is naturally derived. “Naturally derived’, as the term is used herein includes compounds that can be isolated from biological or botanical material. It is within the purview of this disclosure such material can be artificially synthesized if desired or required. It is contemplated that the active compound that is employed will include at least one phenyl group.
[0013] The active compound that is employed can have the general formula:
wherein Ri is one of -OH, an alkenyl group having between 3 and 10 carbon atoms, or an alkoxy group having between 1 and 5 carbon atoms;
R2 is one of an alkyl group having between 1 and 10 carbon atoms an alkoxy group have between 2 and 5 carbon atoms;
R3 and R 6 is hydrogen;
R4 is hydrogen, or an alkenyl group having between 3 and 10 carbon atoms and at least one double bond; and
R5 is hydrogen or an alkoxy group having between 1 and 5 carbon atoms.
[0014] In certain embodiments, it is contemplated that the group Ri can be an -OH group, an alkenyl group having 3 to 10 carbon atoms or an alkoxy group -OR7 in which R7 is
alkyl group selected from the group consisting of methyl, ethyl, propyl, isopropyl, butyl and mixtures thereof. Where Ri is an alkenyl group having between 3 and 10 carbon atoms, it is contemplated that group can have at least one double bone with certain embodiments having only one double bond. In certain embodiments, the at least one double bond can be located between the either the distal or proximal two carbon atoms in the alkenyl group. In certain embodiments, the alkenyl group can be selected from the group consisting of propenyl, butenyl, pentenyl, and mixtures thereof.
[0015] The group R2can be an alkyl group having between 1 and 10 carbon atoms or an alkoxy group having between 2 and 5 carbon atoms. In certain embodiments, the alkyl group can be one of the following: methyl, ethyl , propyl, isopropyl, n-butyl, t-butyl, sec- butyl, isobutyl, n- pentyl, tert-pentyl, neopentyl, isopentyl, sec-pentyl, 3-pentyl, sec-isopentyl and the like. In certain embodiments, the alkoxy group can be -OR7 in which R7 is alkyl group selected from the group consisting of methyl, ethyl, propyl, isopropyl, butyl and mixtures thereof.
[0016] The group R4 is hydrogen, or an alkenyl group having between 3 and 10 carbon atoms and at least one double bond. In certain embodiments, the alkenyl group alkenyl group can have at least one double bone with certain embodiments having only one double bond. In certain embodiments, the at least one double bond can be located between the either the distal or proximal two carbon atoms in the alkenyl group. In certain embodiments, the alkenyl group can be selected from the group consisting of propenyl, butenyl, pentenyl, and mixtures thereof.
[0017] The group R5 can be hydrogen or an alkoxy group having between 1 and 5 carbon atoms. In certain embodiments, the alkoxy group can be -OR7 in which R7 is alkyl group selected from the group consisting of methyl, ethyl, propyl, isopropyl, butyl and mixtures thereof.
[0018] In certain embodiments, the active compound can be selected from the group consisting of phenylpropanoids, monoterpenoid phenols, and mixtures thereof. Suitable phenylpropanoids can include various organic compounds that are synthesized y plant from amino acids phenylalanine and tyrosine. Suitable phenylpropanoid compounds can have a six- carbon phenyl group and a three-carbon propene tail. Non-limiting examples of suitable phenylpropanoid compounds can include compounds such as cinnamaldehyde, eugenol, chavicol, safrole, estragole and the like.
[0019] Suitable cinnamaldehyde material can be present as either the cis isomer, the trans- isomer or mixtures thereof and can have the formula:
Where desired or required, the cinnamaldehyde can be incorporated in the composition as pure material. However, it is also within the purview of this disclosure to incorporate the essential oil of cinnamon back into the composition as disclosed herein. The cinnamaldehyde material can have a density of 1.0497 g/ml, a boiling point of 248 Cand a refractive index of 1.6195 in its pure form.
[0020] Eugenol can be found in essential oils extracted from cloves, nutmeg, cinnamon, basil, bay leaf and the like. The material can have the general formula:
The material can have a molar mass of 164.2 g/mol, a boiling point of 254 C and a density of 1.06 g/cm3 , a pKaof 10.19 at 25 C and a viscosity of 9.12 mPa at 20 C.
[0021] Monoterpenoid phenols suitable for use in the composition disclosed herein include but are not limited to thymol, carvacrol and the like.
[0022] The active compound as disclosed herein can be present in an amount sufficient to impart antimicrobial properties to the assocaited aqueous disinfectant composition when in admixture with one or more of the materials present therein. In certain embodiments, the active compound or compounds as disclosed herein can be present in an amount between 0.1 and 5.0 vol%. In certain embodiments, the active compound can be present in amounts between 0.1 and 4.0 vol %; between 0.1 and 3 vol %; between 0.1 and 2.0 vol %; between 0.1 and 1.0 vol %;
between 0.1 and 0.5 vol %; 0.1 and 0.25 vol %; between 0.2 and 4.0 vol %; between 0.2 and 3.0 vol %; between 0.2 and 2.0 vol %; between 0.2 and 1.0 vol %; between 0.2 and 0.5 vol %; 0.2 and 0.25 vol %; between 0.2 and 4.0 vol %; between 0.3 and 3.0 vol %; between 0.3 and 2.0 vol %; between 0.3 and 1.0 vol %; between 0.3 and 0.5 vol %; between 0.5 and 4.0 vol %; between 0.5 and 3.0 vol %; between 0.5 and 2 vol %; between 0.5 and 1 vol %; between 1.0 and 4.0 vol %; between 1.0 and 3 vol %; between 1.0 and 2.0 vol %; between 2.0 and 4.0 vol %; between 2.0 and 3.0 vol %.
[0023] The active material as disclosed herein can be present as a single compound or in suitable admixture with another active compounds. The present disclosure is predicated, at least in part on the unexpected discovery that the aforementioned active compound(s) can exhibit antimicrobial activity or enhanced antimicrobial activity when present in admixure in the composition as disclosed herein. It has been found unexpectedly compositions as disclosed herein, when applied to surfaces such as hard surfaces can reduce or eliminate pathogens present on the assocaited surface. Non-limiting examples of such pathogens can include athogens such as such as those within the family Paramyxoviridae (such as measles morbillivims), Herpesviridae (such as varicella- zoster virus); Mycobacteriaceae (such as mycobacterium tuberculosis); Orthomyxoviridae (such as influenzavirus A, influenzavirus B); Picornavivdae (such as enterovirus, poliovirus, coxsackie A viruses, coxsackie B viruses and the like); Calicivirdae (such as noroviruses); Coronaviridea including the subfamily Orthocoronavirinae (such as beta coronaviruses like SARS-CoV, SARS-CoV-2, MERS-CoV); Adenoviridae and the like, Staphylococcaceae (such as staphyloccoccu aureus, like methicillin-resistant Staphylococcus aureus); Enterococcaceae (including vancomycin-resistant enterococci), Streptococcaceae (including streptococci) gram positive species such as Clostridioides difficile, Listeria, Coynebacterium and the like.
[0024] The aqueous disinfectant formulation as disclosed herein can also include a liquid material component having between 0.5 and 2.0 M free hydrogen and between 100 ppm and 800 ppm calcium, the liquid material present in an amount capable of yielding a solution pH of 6.0 or below when present in the aqueous disinfectant composition.
[0025] Where desired or required, the free hydrogen present in the liquid composition can be derived from one or more suitable inorganic acids in whole or on part as a dissociated
state. In certain embodiments, the suitable inorganic acid present in a whole or partially dissociated state can be selected from the group consisting of sulfuric acid, carbonic acid, oxalic acid, chromic acid, pyrophosphoric acid, phosphoric acid, and mixtures thereof. In certain embodiments, the inorganic acid component can be present in the aqueous disinfectant composition material solution in an amount between 1 vol% and 8 vol%; between 1 vol % and 7 vol%; between 1 vol% and 6 vol %; between 1 vol% and 5 vol%; between 1 vol% and 4 vol% between 1 vol % and 3 vol%; between 1 vol% and 2 vol%; between 2 vol% and 8 vol%; between 2 vol % and 7 vol%; between 2 vol% and 6 vol %; between 2 vol% and 5 vol%; between 2 vol% and 4 vol% between 2 vol % and 3 vol%; between 1 vol% and 8 vol%; between 1 vol % and 7 vol%; between 1 vol% and 6 vol %; between 1 vol% and 5 vol%; between 1 vol% and 4 vol% between 1 vol % and 3 vol%; between 1 vol% and 2 vol%; between 3 vol% and 8 vol%; between 3 vol % and 7 vol%; between 3 vol% and 6 vol %; between 3 vol% and 5 vol%; between 3 vol% and 4 vol%; between 4 vol% and 8 vol%; between 4 vol % and 7 vol%; between 4 vol% and 6 vol %; between 4 vol% and 5 vol%; between 5 vol% and 8 vol%; between 5 vol % and 7 vol%; between 5 vol% and 6 vol %; between 6 vol% and 8 vol%; between 6 vol % and 7 vol%; between 7vol% and 8 vol%.
[0026] Where the free hydrogen content is associated with or derived from sulfuric acid, it is contemplated that the material will be present as a mixture of ions including one or more of hydrogen sulfate (HSC ), sulfate (SO42 ), and calcium sulfate in soluble form. In the certain embodiments, the predominant ions present in the aqueous disinfectant formulation material solution will be present as hydrogen sulfate (HSO4 )· The free hydrogen present in the liquid material can be between 0.5 M and 2.0M in certain embodiments; between 0.5 and 1.8M free hydrogen, between 0.5 and 1.6M; between 0.5 and 1.5M; between 0.5 and 1.3M; between 0.5 and 1.0M; between 0.5 and 0.8M; between 0.75 and 2.0; between 0.75 and 1.8M; between 0.75 and 1.7M; between 0.75 and 1.6M; between 0.75 and 1.5M; between 0.75 and 1.25M; between 0.75 and 1.0M; between 0.75 and 0.9M; between 1.0 and 2.0M and 1.0 and 1.8M; between 1.0 and 1.7M; between 1.0 and 1.6M; between 1.0 and 1.5M; between 1.0 and 1.25M; between [0027] The aforementioned compounds can be present in a suitable liquid material.
Non-limiting examples of suitable materials include water of a sufficient purity level to facilitate the availability of the component materials and suitability for end-use applications. In certain
embodiments, the water component of the liquid material can be material that is classified as ASTM D1193-06 primary grade. Where desired or required, the water component, the water can be purified by any suitable method, including, but not limited to, distillation, double distillation, deionization, demineralization, reverse osmosis, carbon filtration, ultrafiltration, ultraviolet oxidization, microporous filtration, electrodialysis and the like. In certain embodiments, was having a conductivity between 0.05 and 2.00 micro siemens can be employed. It is also within the purview of this disclosure that the water component of the liquid material can be composed of water having a purity greater than primary grade, if desired or required. Water classified as ASTM1 193-96 purified, ASTM1193-96 ultrapure or higher can be used is desired or required. [0028] The liquid composition component can also contain between 100 ppm and 800 ppm calcium with a major portion being present as calcium ions. In certain embodiments, the calcium ions can be present as Ca2+, CaSC , and mixtures thereof. In certain embodiments, the aqueous disinfectant formulation material can contain between 200 ppm and 800 ppm; between 300 ppm and 800 ppm; between 400 ppm and 800 ppm; between 500 ppm and 800 ppm; between 600 ppm and 800 ppm; between 700 ppm and 800 ppm; between 200 ppm and 700 ppm; between 300 ppm and 700 ppm; between 400 ppm and 700 ppm; between 500 ppm and 700 ppm; between 600 ppm and 700 ppm; between 200 ppm and 600 ppm; between 300 ppm and 600 ppm; between 400 ppm and 600 ppm; between 500 ppm and 600 ppm; between 200 ppm and 500 ppm; between 200 ppm and 400 ppm; between 200 ppm and 300 ppm.
[0029] In certain embodiments, it is contemplated that the liquid material as defined herein can be present in an aqueous material in an amount sufficient to provide the resulting aqueous disinfectant composition with a pH less than 6.0 while in other embodiments, the liquid material can be present in an amount sufficient to provide the resulting aqueous disinfectant formulation with a pH less than 5.5; less than 5.0; 4.5; less than 4.0, less than 3.5; less than 3.0; less than 2.5; less than 2.4; less than 2.3; less than 2.3; less than 2.1; less than 2.0.
[0030] The liquid material that is admixed to form the aqueous disinfectant formulation can be produced by a variety of suitable means provided that the resulting material exhibits reduced or no harmful interaction with tissue such as mucosal tissue. One non-limited example or a suitable formulation process is as follows.
[0031] The liquid material as disclosed herein can be formed by the addition of a suitable inorganic hydroxide to a suitable inorganic acid. Suitable acids acid may have a density between 22° and 70° baume; with specific gravities between about 1.18 and 1.93. In certain embodiments, it is contemplated that the inorganic acid will have a density between 50° and 67° baume; with specific gravities between 1.53 and 1.85. The inorganic acid can be either a monoatomic acid or a polyatomic acid.
[0032] The inorganic acid employed can be homogenous or can be a mixture of various acid compounds that fall within the defined parameters. It is also contemplated that the acid may be a mixture that includes one or more acid compounds that fall outside the contemplated parameters but in combination with other materials will provide an average acid composition value in the range specified. The inorganic acid or acids employed can be of any suitable grade or purity. In certain instances, tech grade and/or food grade material can be employed successfully in various applications. Where desired or required, inorganic acids of even higher purity can be employed.
[0033] In preparing the liquid material as disclosed herein, the inorganic acid can be contained in any suitable reaction vessel in liquid form at any suitable volume. In various embodiments, it is contemplated that the reaction vessel can be non-reactive beaker of suitable volume. The volume of acid employed can be as small as 50 ml. Larger volumes up to and including 5000 gallons or greater are also considered to be within the purview of this disclosure. [0034] The inorganic acid can be maintained in the reaction vessel at a suitable temperature such as a temperature at or around ambient. It is within the purview of this disclosure to maintain the initial inorganic acid in a range between approximately 23° and about 70°C. However lower temperatures in the range of 15° and about 40°C can also be employed. [0035] The inorganic acid is agitated by suitable means to impart mechanical energy in a range between approximately 0.5 HP and 3 HP with agitation levels imparting mechanical energy between 1 and 2.5 HP being employed in certain applications of the process. Other suitable ranges for imparting levels of mechanical energy include between 0.5 HP and 2.5 HP; between 0.5 HP and 2.0 HP; between 0.5 HP and 2.0 HP; between 0.5 HP and 1.5 HP; between 0.5 HP and 1.0 HP; Between 1.0 HP and 3.0 HP; between 1.0 HP and 2.5 HP; between 1.0 HP
and 2.0 HP; between 1.0 HP and 1.5 HP; between 1.5 HP and 3.0 HP; between 1.5 HP and 2.5 HP; between 1.5 HP and 2.0 HP; between 2.0 HP and 3.0 HP; between 2.5 HP and 3.0 HP.
[0036] Agitation can be imparted by a variety of suitable mechanical means including, but not limited to, DC servo drive, electric impeller, magnetic stirrer, chemical inductor and the like. Agitation can commence at an interval immediately prior to hydroxide addition and can continue for an interval during at least a portion of the hydroxide introduction step.
[0037] In the process as disclosed herein, the acid material of choice may be a concentrated acid with an average molarity (M) of at least 7 or above. In certain procedures, the average molarity will be at least 10 or above; with an average molarity between 7 and 10 being useful in certain applications. The acid material of choice employed may exist as a pure liquid, a liquid slurry or as an aqueous solution of the dissolved acid in essentially concentrated form. [0038] Suitable acid materials can be either aqueous or non-aqueous materials. Non limiting examples of suitable acid materials can include one or more of the following: hydrochloric acid, nitric acid, phosphoric acid, chloric acid, perchloric acid, chromic acid, sulfuric acid, permanganic acid, prussic acid, bromic acid, hydrobromic acid, hydrofluoric acid, iodic acid, fluoboric acid, fluosilicic acid, fluotitanic acid.
[0039] In certain embodiments, the defined volume of a liquid concentrated strong acid employed can be sulfuric acid having a specific gravity between 55° and 67° baume. This material can be placed in the reaction vessel and mechanically agitated at a temperature between 16° and 70°C.
[0040] In certain specific applications of the method disclosed, a measured, defined quantity of suitable hydroxide material can be added to an agitating acid, such as concentrated sulfuric acid, that is present in the non-reactive vessel in a measured, defined amount. The amount of hydroxide that is added will be that sufficient to produce a solid material that is present in the composition as a precipitate and/or a suspended solid or colloidal suspension. The hydroxide material employed can be a water-soluble or partially water-soluble inorganic hydroxide. Partially water-soluble hydroxides employed in the process as disclosed herein will generally be those which exhibit miscibility with the acid material to which they are added. Non-limiting examples of suitable partially water-soluble inorganic hydroxides will be those that
exhibit at least 50% miscibility in the associated acid. The inorganic hydroxide can be either anhydrous or hydrated.
[0041] Non-limiting examples of water-soluble inorganic hydroxides include water soluble alkali metal hydroxides, alkaline earth metal hydroxides and rare earth hydroxides; either alone or in combination with one another. Other hydroxides are also considered to be within the purview of this disclosure. “Water- solubility” as the term is defined in conjunction with the hydroxide material that will be employed is defined a material exhibiting dissolution characteristics of 75% or greater in water at standard temperature and pressure. The hydroxide that is utilized typically is a liquid material that can be introduced into the acid material. The hydroxide can be introduced as a true solution, a suspension or a super- saturated slurry. In certain embodiments, it is contemplated that the concentration of the inorganic hydroxide in aqueous solution can be dependent on the concentration of the associated acid to which it is introduced. Non-limiting examples of suitable concentrations for the hydroxide material are hydroxide concentrations greater than 5 to 50% of a 5-mole material.
[0042] Suitable hydroxide materials include, but are not limited to, lithium hydroxide, sodium hydroxide, potassium hydroxide, ammonium hydroxide, calcium hydroxide, strontium hydroxide, barium hydroxide, magnesium hydroxide, and/or silver hydroxide. Inorganic hydroxide solutions when employed may have concentration of inorganic hydroxide between 5 and 50% of a 5-mole material, with concentration between 5 and 20% being employed in certain applications. The inorganic hydroxide material, in certain processes, can be calcium hydroxide in a suitable aqueous solution such as is present as slaked lime.
[0043] In the process as disclosed, the inorganic hydroxide in liquid or fluid form is introduced into the agitating acid material in one or more metered volumes over a defined interval to provide a defined resonance time. The resonance time in the process as outlined is considered to be the time interval necessary to promote and provide the environment in which the hydronium ion material as disclosed herein develops. The resonance time interval as employed in the process as disclosed herein is typically between 12 and 120 hours with resonance time intervals between 24 and 72 hours and increments therein being utilized in certain applications.
[0044] In various applications of the process, the inorganic hydroxide is introduced into the acid at the upper surface of the agitating volume in a plurality of metered volumes.
Typically, the total amount of inorganic hydroxide material will be introduced as a plurality of measured portions over the resonance time interval. Front-loaded metered addition being employed in many instances. “Front-loaded metered addition”, as the term is used herein, is taken to mean addition of the total hydroxide volume with a greater portion being added during the initial portion of the resonance time. An initial percentage of the desired resonance time - considered to be between the first 25% and 50% of the total resonance time.
[0045] It is to be understood that the proportion of each metered volume that is added can be equal or can vary based on such non-limiting factors as external process conditions, in situ process conditions, specific material characteristics, and the like. It is contemplated that the number of metered volumes can be between 3 and 12. The interval between additions of each metered volume can be between 5 and 60 minutes in certain applications of the process as disclosed. The actual addition interval can be between 60 minutes to five hours in certain applications.
[0046] In certain applications of the process, a 100 ml volume of 5% weight per volume of calcium hydroxide material is added to 50 ml of 66° baume concentrated sulfuric acid in 5 metered increments of 2 ml per minute, with or without admixture. Addition of the hydroxide material to the sulfuric acid produces a material having increasing liquid turbidity. Increasing liquid turbidity is indicative of calcium sulfate solids forming as precipitate. The produced calcium sulfate can be removed in a fashion that is coordinated with continued hydroxide addition in order to provide a coordinated concentration of suspended and dissolved solids. [0047] Without being bound to any theory, it is believed that the addition of calcium hydroxide to sulfuric acid in the manner defined herein results in the consumption of the initial hydrogen proton or protons associated with the sulfuric acid resulting in hydrogen proton oxygenation such that the proton in question is not off-gassed as would be generally expected upon hydroxide addition. Instead, the proton or protons are recombined with ionic water molecule components present in the liquid material.
[0048] Solid material generated during the process and present as precipitate or suspended solids can be removed by any suitable means. Such removal means include, but need
not be limited to, the following: gravimetric, forced filtration, centrifuge, reverse osmosis and the like.
[0049] The resulting liquid is a shelf-stable material that is believed to be shelf stable when stored at ambient temperature and between 50 and 75% relative humidity. In its concentrated state, the material can have a molarity between 1.87 to 1.78 molar and can contain between 3% and 10% of total moles of acid protons that are not charge balanced. In certain embodiments, the liquid material can contain between 4% and 9% of total moles of acid protons that are charge balanced; between 5% and 9% of total moles of charge balanced acid; between 6% and 9% of total moles of charge balanced acid; between 7% and 9% of total moles of charge balanced acid; between 8% and 9% of total moles of charge balanced acid.
[0050] It is contemplated that the resulting material can be further purified as suitable and can be employed as the liquid material in the biocompatible material solution as disclosed herein. It is also within the purview of this disclosure to subject the resulting material to further processing as desired or required. Non-limiting examples of such processing can include subjecting the resulting fluid to as suitable magnetic field or fields.
[0051] In certain embodiments, the resulting liquid material can be subjected to a non-bi- polar magnetic field at a value greater than 2000 gauss; with magnetic fields greater than 2 million gauss being employed in certain applications. It is contemplated that a magnetic field between 10,000 gauss and 2 million gauss can be employed in certain situations. Other suitable ranges include between 10,000 gauss and 20,000 gauss; between 10,000 gauss and 30,000 gauss; between 10,000 gauss and 40,000 gauss; between 10,000 gauss and 50,000 gauss; between 10,000 gauss and 60,000 gauss; between 10,000 gauss and 70,000 gauss; between 10,000 gauss and 80,000 gauss; between 10,000 gauss and 90,000 gauss; between 10,000 gauss and 100,000 gauss; between 50,000 gauss and 100,000 gauss; between 50,000 gauss and 150,000 gauss; between 50,000 gauss between 200,000 gauss; between 50,000 gauss and 250,000 gauss; between 100,000 gauss and 200,000 gauss; between 100,000 gauss and 250,000 gauss; between 100,000 gauss and 300,000 gauss; between 100,000 gauss and 350,000 gauss; between 100,000 gauss and 400,000 gauss; between 100,000 gauss and 450,000 gauss; between 100,000 gauss and 500,000 gauss; between 250,000 gauss and 300,000 gauss; between 250,000 gauss and 400,000 gauss; between 250,000 gauss and 500,000 gauss; between 500,000 gauss and 600,000 gauss;
between 500,000 and 700,000 gauss; between 500,000 gauss and 800,000 gauss; between 500,000 gauss and 900,000 gauss; between 500,000 gauss and 1,000,000 gauss; between 750,000 gauss and 1,100,000 gauss; between 750,000 gauss and 1,200,000 gauss; between 750,000 gauss and 1, 250,000 gauss; between 1,000,000 gauss and 1,100,000 gauss; between 1,100,000 gauss and 1,200,000 gauss; between 1,200,000 gauss and 1,300,000 gauss; between 1,300,000 gauss and 1,400,000 gauss; between 1,400,000 gauss and 1,500,000 gauss; between 1,500,000 gauss and 1,600,000 gauss; between 1,600,000 gauss and 1,700,000 gauss; between 1,800,000 gauss and 1,900,000 gauss; between 1,900,000 gauss and 2,000,000. The magnetic field can be produced by various suitable means. One non-limiting example of a suitable magnetic field generator is found in US 7,122,269 to Wurzburger, the specification of which is incorporated by reference herein.
[0052] Solid material generated during the process and present as precipitate or suspended solids can be removed by any suitable means. Such removal means include, but need not be limited to, the following: gravimetric, forced filtration, centrifuge, reverse osmosis and the like.
[0053] The resulting liquid as disclosed herein is a shelf-stable viscous liquid that is believed to be stable for at least one year when stored at ambient temperature and between 50 to 75% relative humidity. The stable electrolyte composition of matter can be use neat in various end use applications. The stable electrolyte composition of matter can have a 1.87 to 1.78 molar material that contains 8 to 9 % of the total moles of acid protons that are not charged balanced. [0054] The liquid material that results from the process as disclosed herein can have a molarity between 200 M to 150 M strength and 187 to 178 M strength in certain instances, when measured titrimetrically though hydrogen coulometry and via FTIR spectral analysis. The material has a gravimetric range greater than 1.15; with ranges greater than 1.9 in in certain instances. The material, when analyzed, is shown to yield up to 1300 volumetric times of orthohydrogen per cubic ml versus hydrogen contained in a mole of water.
[0055] It is contemplated that the liquid material as disclosed herein may serve as a source of acid protons when introduced into the biocompatible material as contemplated herein.
It has also been discovered, quite unexpectedly that the resulting material will present with a pH at 5.0 or below without the assocaited level of corrosivity. It is believed that the resulting
composition contains an elevated level of acid protons present as HSCL . Without being bound by any theory, it is believed that elevated levels of HSQf ions present in the resulting composition may moderate the corrosive characteristics of the resulting composition permitting it to be administered to patients in a suitable biocompatible material solution at a composition pH below 5.0; below 4.5; below 4.0; below 3.5; below 3.0; below 2.5; below 2.0. In certain embodiments, the composition pH can be between 1.5 and 3.5; between 2.0 and 3.5; between 2.5 and 3.5. The administration of the biocompatible material solution as disclosed herein can proceed without substantial deleterious effect on the patient tissue that is contacted.
[0056] One non-limited example or a suitable formulation process is as follows.
[0057] The liquid material as disclosed herein can be formed by the addition of a suitable inorganic hydroxide to a suitable inorganic acid. Suitable acids acid may have a density between 22° and 70° baume; with specific gravities between about 1.18 and 1.93. In certain embodiments, it is contemplated that the inorganic acid will have a density between 50° and 67° baume; with specific gravities between 1.53 and 1.85. The inorganic acid can be either a monoatomic acid or a polyatomic acid.
[0058] The inorganic acid employed can be homogenous or can be a mixture of various acid compounds that fall within the defined parameters. It is also contemplated that the acid may be a mixture that includes one or more acid compounds that fall outside the contemplated parameters but in combination with other materials will provide an average acid composition value in the range specified. The inorganic acid or acids employed can be of any suitable grade or purity. In certain instances, tech grade and/or food grade material can be employed successfully in various applications. Where desired or required, inorganic acids of even higher purity can be employed.
[0059] In preparing the liquid material as disclosed herein, the inorganic acid can be contained in any suitable reaction vessel in liquid form at any suitable volume. In various embodiments, it is contemplated that the reaction vessel can be non-reactive beaker of suitable volume. The volume of acid employed can be as small as 50 ml. Larger volumes up to and including 5000 gallons or greater are also considered to be within the purview of this disclosure. [0060] The inorganic acid can be maintained in the reaction vessel at a suitable temperature such as a temperature at or around ambient. It is within the purview of this
disclosure to maintain the initial inorganic acid in a range between approximately 23° and about 70°C. However lower temperatures in the range of 15° and about 40°C can also be employed. [0061] The inorganic acid is agitated by suitable means to impart mechanical energy in a range between approximately 0.5 HP and 3 HP with agitation levels imparting mechanical energy between 1 and 2.5 HP being employed in certain applications of the process. Other suitable ranges for imparting levels of mechanical energy include between 0.5 HP and 2.5 HP; between 0.5 HP and 2.0 HP; between 0.5 HP and 2.0 HP; between 0.5 HP and 1.5 HP; between 0.5 HP and 1.0 HP; Between 1.0 HP and 3.0 HP; between 1.0 HP and 2.5 HP; between 1.0 HP and 2.0 HP; between 1.0 HP and 1.5 HP; between 1.5 HP and 3.0 HP; between 1.5 HP and 2.5 HP; between 1.5 HP and 2.0 HP; between 2.0 HP and 3.0 HP; between 2.5 HP and 3.0 HP. [0062] Agitation can be imparted by a variety of suitable mechanical means including, but not limited to, DC servo drive, electric impeller, magnetic stirrer, chemical inductor and the like. Agitation can commence at an interval immediately prior to hydroxide addition and can continue for an interval during at least a portion of the hydroxide introduction step.
[0063] In the process as disclosed herein, the acid material of choice may be a concentrated acid with an average molarity (M) of at least 7 or above. In certain procedures, the average molarity will be at least 10 or above; with an average molarity between 7 and 10 being useful in certain applications. The acid material of choice employed may exist as a pure liquid, a liquid slurry or as an aqueous solution of the dissolved acid in essentially concentrated form. [0064] Suitable acid materials can be either aqueous or non-aqueous materials. Non limiting examples of suitable acid materials can include one or more of the following: hydrochloric acid, nitric acid, phosphoric acid, chloric acid, perchloric acid, chromic acid, sulfuric acid, permanganic acid, prussic acid, bromic acid, hydrobromic acid, hydrofluoric acid, iodic acid, fluoboric acid, fluosilicic acid, fluotitanic acid.
[0065] In certain embodiments, the defined volume of a liquid concentrated strong acid employed can be sulfuric acid having a specific gravity between 55° and 67° baume. This material can be placed in the reaction vessel and mechanically agitated at a temperature between 16° and 70°C.
[0066] In certain specific applications of the method disclosed, a measured, defined quantity of suitable hydroxide material can be added to an agitating acid, such as concentrated
sulfuric acid, that is present in the non-reactive vessel in a measured, defined amount. The amount of hydroxide that is added will be that sufficient to produce a solid material that is present in the composition as a precipitate and/or a suspended solid or colloidal suspension. The hydroxide material employed can be a water-soluble or partially water-soluble inorganic hydroxide. Partially water-soluble hydroxides employed in the process as disclosed herein will generally be those which exhibit miscibility with the acid material to which they are added. Non-limiting examples of suitable partially water-soluble inorganic hydroxides will be those that exhibit at least 50% miscibility in the associated acid. The inorganic hydroxide can be either anhydrous or hydrated.
[0067] Non-limiting examples of water-soluble inorganic hydroxides include water soluble alkali metal hydroxides, alkaline earth metal hydroxides and rare earth hydroxides; either alone or in combination with one another. Other hydroxides are also considered to be within the purview of this disclosure. “Water- solubility” as the term is defined in conjunction with the hydroxide material that will be employed is defined a material exhibiting dissolution characteristics of 75% or greater in water at standard temperature and pressure. The hydroxide that is utilized typically is a liquid material that can be introduced into the acid material. The hydroxide can be introduced as a true solution, a suspension or a super- saturated slurry. In certain embodiments, it is contemplated that the concentration of the inorganic hydroxide in aqueous solution can be dependent on the concentration of the associated acid to which it is introduced. Non-limiting examples of suitable concentrations for the hydroxide material are hydroxide concentrations greater than 5 to 50% of a 5-mole material.
[0068] Suitable hydroxide materials include, but are not limited to, lithium hydroxide, sodium hydroxide, potassium hydroxide, ammonium hydroxide, calcium hydroxide, strontium hydroxide, barium hydroxide, magnesium hydroxide, and/or silver hydroxide. Inorganic hydroxide solutions when employed may have concentration of inorganic hydroxide between 5 and 50% of a 5-mole material, with concentration between 5 and 20% being employed in certain applications. The inorganic hydroxide material, in certain processes, can be calcium hydroxide in a suitable aqueous solution such as is present as slaked lime.
[0069] In the process as disclosed, the inorganic hydroxide in liquid or fluid form is introduced into the agitating acid material in one or more metered volumes over a defined
interval to provide a defined resonance time. The resonance time in the process as outlined is considered to be the time interval necessary to promote and provide the environment in which the hydronium ion material as disclosed herein develops. The resonance time interval as employed in the process as disclosed herein is typically between 12 and 120 hours with resonance time intervals between 24 and 72 hours and increments therein being utilized in certain applications.
[0070] In various applications of the process, the inorganic hydroxide is introduced into the acid at the upper surface of the agitating volume in a plurality of metered volumes. Typically, the total amount of inorganic hydroxide material will be introduced as a plurality of measured portions over the resonance time interval. Front-loaded metered addition being employed in many instances. “Front-loaded metered addition”, as the term is used herein, is taken to mean addition of the total hydroxide volume with a greater portion being added during the initial portion of the resonance time. An initial percentage of the desired resonance time - considered to be between the first 25% and 50% of the total resonance time.
[0071] It is to be understood that the proportion of each metered volume that is added can be equal or can vary based on such non-limiting factors as external process conditions, in situ process conditions, specific material characteristics, and the like. It is contemplated that the number of metered volumes can be between 3 and 12. The interval between additions of each metered volume can be between 5 and 60 minutes in certain applications of the process as disclosed. The actual addition interval can be between 60 minutes to five hours in certain applications.
[0072] In certain applications of the process, a 100 ml volume of 5% weight per volume of calcium hydroxide material is added to 50 ml of 66° baume concentrated sulfuric acid in 5 metered increments of 2 ml per minute, with or without admixture. Addition of the hydroxide material to the sulfuric acid produces a material having increasing liquid turbidity. Increasing liquid turbidity is indicative of calcium sulfate solids forming as precipitate. The produced calcium sulfate can be removed in a fashion that is coordinated with continued hydroxide addition in order to provide a coordinated concentration of suspended and dissolved solids. [0073] Without being bound to any theory, it is believed that the addition of calcium hydroxide to sulfuric acid in the manner defined herein results in the consumption of the initial
hydrogen proton or protons associated with the sulfuric acid resulting in hydrogen proton oxygenation such that the proton in question is not off-gassed as would be generally expected upon hydroxide addition. Instead, the proton or protons are recombined with ionic water molecule components present in the liquid material.
[0074] Solid material generated during the process and present as precipitate or suspended solids can be removed by any suitable means. Such removal means include, but need not be limited to, the following: gravimetric, forced filtration, centrifuge, reverse osmosis and the like.
[0075] The resulting liquid is a shelf-stable material that is believed to be shelf stable when stored at ambient temperature and between 50 and 75% relative humidity. In its concentrated state, the material can have a molarity between 1.87 to 1.78 molar and can contain between 3% and 10% of total moles of acid protons that are not charge balanced. In certain embodiments, the liquid material can contain between 4% and 9% of total moles of acid protons that are charge balanced; between 5% and 9% of total moles of charge balanced acid; between 6% and 9% of total moles of charge balanced acid; between 7% and 9% of total moles of charge balanced acid; between 8% and 9% of total moles of charge balanced acid.
[0076] It is contemplated that the resulting material can be further purified as suitable and can be employed as the liquid material in the biocompatible material solution as disclosed herein. It is also within the purview of this disclosure to subject the resulting material to further processing as desired or required. Non-limiting examples of such processing can include subjecting the resulting fluid to as suitable magnetic field or fields.
[0077] In certain embodiments, the resulting liquid material can be subjected to a non-bi- polar magnetic field at a value greater than 2000 gauss; with magnetic fields greater than 2 million gauss being employed in certain applications. It is contemplated that a magnetic field between 10,000 gauss and 2 million gauss can be employed in certain situations. Other suitable ranges include between 10,000 gauss and 20,000 gauss; between 10,000 gauss and 30,000 gauss; between 10,000 gauss and 40,000 gauss; between 10,000 gauss and 50,000 gauss; between 10,000 gauss and 60,000 gauss; between 10,000 gauss and 70,000 gauss; between 10,000 gauss and 80,000 gauss; between 10,000 gauss and 90,000 gauss; between 10,000 gauss and 100,000 gauss; between 50,000 gauss and 100,000 gauss; between 50,000 gauss and 150,000 gauss;
between 50,000 gauss between 200,000 gauss; between 50,000 gauss and 250,000 gauss; between 100,000 gauss and 200,000 gauss; between 100,000 gauss and 250,000 gauss; between 100,000 gauss and 300,000 gauss; between 100,000 gauss and 350,000 gauss; between 100,000 gauss and 400,000 gauss; between 100,000 gauss and 450,000 gauss; between 100,000 gauss and 500,000 gauss; between 250,000 gauss and 300,000 gauss; between 250,000 gauss and 400,000 gauss; between 250,000 gauss and 500,000 gauss; between 500,000 gauss and 600,000 gauss; between 500,000 and 700,000 gauss; between 500,000 gauss and 800,000 gauss; between 500,000 gauss and 900,000 gauss; between 500,000 gauss and 1,000,000 gauss; between 750,000 gauss and 1,100,000 gauss; between 750,000 gauss and 1,200,000 gauss; between 750,000 gauss and 1, 250,000 gauss; between 1,000,000 gauss and 1,100,000 gauss; between 1,100,000 gauss and 1,200,000 gauss; between 1,200,000 gauss and 1,300,000 gauss; between 1,300,000 gauss and 1,400,000 gauss; between 1,400,000 gauss and 1,500,000 gauss; between 1,500,000 gauss and 1,600,000 gauss; between 1,600,000 gauss and 1,700,000 gauss; between 1,800,000 gauss and 1,900,000 gauss; between 1,900,000 gauss and 2,000,000. The magnetic field can be produced by various suitable means. One non-limiting example of a suitable magnetic field generator is found in US 7,122,269 to Wurzburger, the specification of which is incorporated by reference herein.
[0078] Solid material generated during the process and present as precipitate or suspended solids can be removed by any suitable means. Such removal means include, but need not be limited to, the following: gravimetric, forced filtration, centrifuge, reverse osmosis and the like.
[0079] The resulting liquid as disclosed herein is a shelf-stable viscous liquid that is believed to be stable for at least one year when stored at ambient temperature and between 50 to 75% relative humidity. The stable electrolyte composition of matter can be use neat in various end use applications. The stable electrolyte composition of matter can have a 1.87 to 1.78 molar material that contains 8 to 9 % of the total moles of acid protons that are not charged balanced. [0080] The liquid material that results from the process as disclosed herein can have a molarity between 200 M to 150 M strength and 187 to 178 M strength in certain instances, when measured titrimetrically though hydrogen coulometry and via FTIR spectral analysis. The material has a gravimetric range greater than 1.15; with ranges greater than 1.9 in in certain
instances. The material, when analyzed, is shown to yield up to 1300 volumetric times of orthohydrogen per cubic ml versus hydrogen contained in a mole of water.
[0081] It is contemplated that the liquid material as disclosed herein may serve as a source of acid protons when introduced into the biocompatible material as contemplated herein.
It has also been discovered, quite unexpectedly that the resulting material will present with a pH at 5.0 or below without the assocaited level of corrosivity. It is believed that the resulting composition contains an elevated level of acid protons present as HSCU .
[0082] Where desired or required, the aqueous disinfectant formulation can also optionally include a solubilizer. Where employed, the solubilizer can be a surfactant capable of solubilizing the active material in an aqueous diluent such as water. Various anionic, zwitterionic and nonionic surfactants or mixtures thereof can be successfully employed in the compositions as disclosed herein. Suitable zwitterionic surfactants include, but are not limited to, materials such as lauryldimethylamine oxide, myristamine oxide, alkyl imidazolines, alkyl amines, as well as mixtures thereof. Non-limiting examples of suitable non-ionic surfactants include ethylene oxide adducts of Csto Cu alcohols, ethylene oxide/propylene oxide adducts of ethylene glycol, alkylene glycols, and mixtures thereof. Non-limiting examples of suitable anionic surfactants include alkyl sulfonates and alkyl aryl sulfonates having about 8 to about 22 carbon atoms in the alkyl portion, alkali metal salts or mixtures thereof.
[0083] When present, the surfactant material can be present in an amount between 0 and
5 vol%; between 0.1 and 4.0 vol%; between 0.1 and 3.0 vol%; between 0.1 and 2 vol %; between 0.1 and 1 vol%; between 0.1 and 0.5 vol%.
[0084] It is also contemplated that the aqueous disinfectant formulation as disclosed herein can also contain a suitable short-chain alcohol component. It is contemplated that the short-chain alcohol component, when present, can be present in an amount between 0.1 and 50 vol%, with concentrations between 0.1 and 3 vol% being employed in certain embodiments. Examples of suitable alcohols, include but are not limited to, Ci to Ce straight-chained or branched alcohols such as ethanol, methanol, propanol, isopropanol, butanol and mixtures thereof.
[0085] The formulation can also include one or more weak organic acids which, when present, can be present in amounts between 0.1 and 2% and can be selected form the group
consisting of and acetic acid, hydroxyacetic acid, citric acid, tartaric acid, maleic acid, fumaric acid and mixtures thereof.
[0086] The formulation, as disclosed herein, can also include a carboxylic acid component composed of ca carboxylic acid having the general formula:
wherein Ri is an unsaturated hydrocarbon moiety having between four and fourteen carbon atoms or a hydrocarbon moiety having between four and fourteen carbon atoms and at least one double bond; and wherein R2 is a one of -H, -OH, or -CH3..
In certain embodiments, the carboxylic acid compound can be selected from the group consisting of hexanoic acid, octanoic acid, decanoic acid, dodecanoic acid and mixtures thereof When present the formulation, the carboxylic acid component can be present in an amount between 0.1 and 3.0 vol% .
[0087] In certain embodiments, the formulation can also include a biosurfactant present in an amount between 0.1vol% and 3.0 vol% such as those selected from the group consisting of rhamnolipid, sophorolipids, lecithins, steroid acids conjugated with taurine, steroid acids conjugated with glycine.
[0088] Without being bound to any theory, it is believed that material prepared by the process as disclosed herein may contain and elevated level of hydronium ions that can be stably present, in the whole or in part, in the resulting biocompatible material. When present, the ion complex in the biocompatible material solution is generally stable and capable of functioning as an oxygen donor in the presence ofthe environment created to generate the same. The material may have any suitable structure and solvation that is generally stable and capable of functioning as an oxygen donor. Particular embodiments of the resulting solution will include a concentration of the ion as depicted by the following formula:
wherein x is an odd integer > 3.
[0089] It is contemplated that ionic version of the compound as disclosed herein exists in unique ion complexes that have greater than seven hydrogen atoms in each individual ion complex which are referred to in this disclosure as hydronium ion complexes. Asusedherein,the term "hydroniumion complex" can be broadly defined as the cluster ofmolecules that surround the cation ί^ίl^ + where x is an integer greater than or equal to 3. The hydronium ion complex may include at least four additional hydrogen molecules and a stoichiometric proportion of oxygen molecules complexed thereto as water molecules. Thus, the formulaic representation of non-limiting examples of the hydronium ion complexes that can be employed in the process herein can be depicted by the formula:
where x is an odd integer of 3 or greater; and y is an integer from 1 to 20, with y being an integer between 3 and 9 in certain embodiments.
In certain the hydronium ion will be present as a population of ion configurations with elevated levels of hydronium ions in which x is an odd integer that is 9 or greater. In certain embodiments, the hydronium ion will be present as a population of ion configurations with elevated levels of hydronium ions in which x is an odd integer that is 21 or greater.
[0090] In various embodiments disclosed herein, it is contemplated that at least a portion of the hydronium ion complexes will exist as solvated structures of hydronium ions having the formula:
wherein x is an integer between 1 and 4; and y is an integer between 0 and 2.
[0091] In such structures, an 4- core is protonated by multiple H2O
molecules. It is contemplated that the hydronium complexes present in the composition of matter as disclosed herein can exist as Eigen complex cations, Zundel complex cations or mixtures of the two. The Eigen solvation structure can have the hydronium ion at the center of an H9O4+ structure with the hydronium complex being strongly bonded to three neighboring water molecules. The Zundel solvation complex can be an H5O2+ complex in which the proton is
shared equally by two water molecules. The solvation complexes typically exist in equilibrium between Eigen solvation structure and Zundel solvation structure. Heretofore, therespective solvation structure complexes generally existed in an equilibrium state that favors the Zundel solvation structure.
[0092] The present disclosure is based, at least in part, on the unexpected discovery that stable materials can be produced in which hydronium ion exists in an equilibrium state that favors the Eigen complex. The present disclosure is also predicated on the unexpected discovery that increases in the concentration of the Eigen complex in a process stream can provide a class of novel enhanced oxygen-donor oxonium materials.
[0093] The process stream as disclosed herein can have an Eigen solvation state to
Zundel solvation state ratio between 1.2 to 1 and 15 to 1 in certain embodiments; with ratios between 1.2 to 1 and 5 to 1 in other embodiments.
[0094] The novel enhanced oxygen-donor oxonium material as disclosed herein can be generally described as a thermodynamically stable aqueous acid solution that is buffered with an excess of proton ions. In certain embodiments, the excess of protons ions can be in an amount between 10% and 50% excess hydrogen ions as measured by free hydrogen content.
EXAMPLE I
[0095] A first embodiment of the liquid material as disclosed herein is prepared by the following method. Several units of (50) ml of concentrated liquid sulfuric acid having a mass fraction H 2 SO4 of 98%, an average molarity(M) above 7 and a specific gravity of 660 baume are placed in respective non-reactive vessels and maintained at 25°C with agitation by a magnetic stirrer to impart mechanical energy of 1 HP to the liquid.
[0096] Once agitation has commenced, a measured quantity of sodium hydroxide is added to the upper surface of each of the agitating acid material. The sodium hydroxide material employed is a 20% aqueous solution of 5M calcium hydroxide and is introduced into each of the respective units in five metered volumes introduced at a rate of 2 ml per minute over an interval of five hours with to provide a resonance time of 24 hours. The introduction interval for each metered volume is 30 minutes.
[0097] Turbidity is produced in the units with addition of calcium hydroxide to the sulfuric acid indicating formation of calcium sulfate solids. The solids in each unit are permitted
to precipitate periodically during the process and the precipitate is removed from contact with the reacting solutions.
[0098] Upon completion of the 24-hour resonance time, the resulting material are each exposed to a non-bi-polar magnetic field of 2400 gauss resulting in the production of observable precipitate and suspended solids for an interval of 2 hours. The resulting material units are centrifuged and force filtered to isolate the precipitate and suspended solids from each the liquid material unit.
[0099] The liquid material that is produced is separated as individual samples. Some are stored in closed containers at standard temperature and 50% relative humidity to determine shelf- stability. Other samples are subjected to analytical procedures to determine composition. The test samples are subjected to FTIR spectra analysis and titrated with hydrogen coulometry. The sample material has a molarity ranging from 187 to 178 M strength. The material has a gravimetric range greater than 1.15; with ranges greater than 1.9 in in certain instances. The composition is stable and has a 1.87 to 1.78 molar material that contains 8 to 9 % of the total moles of acid protons that are not charged balanced. Liquid material is collected for further use and analysis.
EXAMPLE II
[00100] A second embodiment of the liquid material as disclosed herein is prepared by introducing 50 ml units of concentrated liquid sulfuric acid having a mass fraction H 2 SO4 of 98%, an average molarity(M) above 7 and a specific gravity of 660 baume into a non-reactive vessel and maintaining each at 25°C with agitation by a magnetic stirrer to impart mechanical energy of 1 HP to each liquid unit.
[00101] Once agitation has commenced, a measured quantity of sodium hydroxide is added to the upper surface of the agitating acid material of each liquid unit. The sodium hydroxide material employed is a 20% aqueous solution of 5M calcium hydroxide and is introduced in five metered volumes introduced at a rate of 2 ml per minute over an interval of five hours with to provide a resonance time of 24 hours. The introduction interval for each metered volume is 30 minutes.
[00102] Turbidity is produced with addition of calcium hydroxide to the sulfuric acid indicating formation of calcium sulfate solids. The solids in each unit are permitted to
precipitate periodically during the process and the precipitate is removed from contact with the reacting solution.
[00103] Upon completion of the 24-hour resonance time, the resulting material is centrifuged and force filtered to isolate the precipitate and suspended solids from the liquid material and respective resulting material units are collected for further use and analysis.
EAMPLE III
[00104] A 5 ml portion of the material produced according to the method outlined in
Example I is admixed in a 5 ml portion of deionized and distilled water at standard temperature and pressure. The excess hydrogen ion concentration is measured as greater than 15 % by volume and the pH of the material is determined to be 1.
EXAMPLE IV
[00105] To further evaluate the materials prepared in Examples I and II, samples of the materials are diluted with deionized water to provide material that contains 1 % by volume of the respective material in water. These samples are evaluated against a dilute sulfuric acid solution, a dilute sulfuric acid solution with to which calcium sulfate is added to yield 300 ppm and a dilute sulfuric with 400 ppm calcium sulfate and well as a reverse osmosis water control. [00106] All samples are diluted in an acid matrix for analysis. The testing is completed using a Thermo iCAP 6300 Duo ICP-OES for calcium and sulfur content following EPA method 200.7.
[00107] Each test material is initially prepared by simple dilution in a 5% nitric acid matrix. The calibration standards are prepared in the same acid matrix to match the samples. However, this preparation leads to high recoveries for calcium which is believed to be a result of the sulfuric acid present in the samples but not present in the calibration standards. The calibration standards are re-prepared with a small amount of sulfuric acid in order to match the samples, and the analysis repeated in order to provide better QC recoveries that approach 100%. [00108] In order to test for conductivity the samples are each diluted with de-ionized water for analysis. The testing is completed using a Mettler Toledo Seven Excellence Meter with a conductivity probe following EPA method 120.1. Predicted conductivity results are presented in Table I.
TABLE I
[00109] In order to evaluate freezing point, the samples are analyzed using a TA
Instruments Q100 DSC equipped with an RCS-90 cooling system following USP <891>. Predicted results are presented in Table II.
TABLE II
[00110] The density and specific gravity of the samples are determined at 20 °C using an
Anton Paar digital density meter following EPA method 830.7300. predicted results are presented in Table III.
TABLE III
[00111] The samples are also titrated for hydrogen ion content with acidity being determined following ASTM D1067 - Test Method A to a pH of 8.6. The testing was completed using a Metrohm 826 Titrando equipped with a pH probe. Predicted results are presented in Table IV.
TABLE IV
[00112] Solutions were analyzed an Agilent 1290/G6530 Q-TOF LC-MS using direct infusion (no column) and electrospray ionization in the positive and negative modes. Representative mass spectra collected in the positive and negative ionization modes are shown in Figs.l and 2 with for Dilute Sulfuric Acid w/ 400 ppm CaSC (A), Dilute Sulfuric Acid (B), Tydracide (C), and Reverse Osmosis Water (D).
EXAMPLE V
[00113] The respective samples of Example I are diluted to produce 5 volume % of the product in water and are found to be shelf stable for at least 12 to 18 months. The excess hydrogen ion concentration is measured to be greater than 15% and the pH of the material is determined to be 1.
EXAMPLE VI
[00114] In order to ascertain the effectiveness of various embodiments of the formulation as disclosed herein, compositions are prepared as outlined in the Table V using the percentages of the liquid material described in Example I at concentrations of 2.4 vol% or 4.8 vol% respectively in water. A composition is also prepared according to the present disclosure incorporated sulfuric acid to equal the concentration the composition of Example I at 2.4 vol% for comparison.
The respective materials are free flowing liquids that could be wiped, sprayed or misted onto hard surfaces.
EXAMPLE VII
[00115] The formulations of Examples VI are evaluated to determine whether the respective material kills, in 10-minutes contact time at least 57 of 60 carriers/lot against Staphylococcus aureus and at least 54 of 60 carriers/lot against Pseudimonas aeruginosa using AO AC Official Method 955.15 against S. aureus and AO AC Official Method 964.02 against P. aeruginosa. The various materials exhibit between log 6.0 reduction or greater within the test interval.
[00116] While the invention has been described in connection with what is presently considered to be the most practical and preferred embodiment, it is to be understood that the invention is not to be limited to the disclosed embodiments but, on the contrary, is intended to cover various modifications and equivalent arrangements included within the spirit and scope of the appended claims, which scope is to be accorded the broadest interpretation so as to encompass all such modifications and equivalent structures as is permitted under the law.
Claims
1. An aqueous disinfectant formulation comprising: from about 0.1 vol. % and 5.0 vol % of at least one antimicrobial compound derived from at least one natural material; a liquid material component having between 0.5 and 2.0 M free hydrogen, the liquid material present in an amount capable of yielding a solution pH of 6.0 or below when present in the aqueous disinfectant composition; a solubilizer present in an amount between 0 vol % and 5 vol% ; a short-chain alcohol present in an amount between 0 and 50 vol% ; and water.
2. The aqueous disinfectant formulation of claim 1 wherein the at least one natural compound derivative has the general formula:
wherein Ri is one of -OH, an alkenyl group having between 3 and 10 carbon atoms, or an alkoxyl group having between 1 and 5 carbon atoms;
R2 is one of an alkyl group having between 1 and 10 carbon atoms, or an alkoxy group having between 2 and 5 carbon atoms;
R3 and R 6 is hydrogen;
R4 is hydrogen, or an alkenyl group having between 3 and 10 carbon atoms and at least one double bond; and
R5 is hydrogen or an alkoxy group having between 1 and 5 carbon atoms.
3. The composition of claim 1 or 2 wherein the antimicrobial compound is selected
from the group consisting of phenylpropanoids, monoterpenoid phenols, and mixtures thereof.
4. The composition of claim 3 wherein the naturally derived compound is selected from the group consisting of thymol, carvarol, cinnamaldehyde, eugenol and mixtures thereof.
5. The composition of claim 1, 2 , 3 or 4 wherein the solubilizer is a surfactant surfactant-hydrotrope selected from the group consisting of anionic surfactants, nonionic surfactants, zwitterionic surfactants or mixtures thereof.
6. The composition of claim 5 wherein the zwitterionic surfactant is selected from the group consisting of lauryldimethylamine oxide, myristamine oxide, alkyl imidazolines, alkyl amines, and mixtures thereof.
7. The composition of claim 5 or 6 wherein the anionic surfactant is selected from the group consisting of alkyl sulfonates and alkyl aryl sulfonates having about 8 to about 22 carbon atoms in the alkyl portion, alkali metal salts or mixtures thereof.
8. The composition of claim 5, 6 or 7 wherein the nonionic surfactant is selected from the group consisting of ethylene oxide adducts of Cs to Cu alcohols, ethylene oxide/propylene oxide adducts of ethylene glycol, alkylene glycols, and mixtures thereof.
9. The aqueous disinfectant composition of claim 1 or 2 wherein the liquid material having between 0.5 and 2.0 M free hydrogen and between 100 ppm and 800 ppm calcium, the liquid material present in an amount capable of yielding a solution pH of 6.0 or below when present in the composition is present in an amount between 0.25 vol% and 20 vol%.
10. The aqueous disinfectant composition of claim 9 wherein the liquid material having between 0.5 and 2.0 M free hydrogen and between 100 ppm and 800 ppm calcium
further comprises between 100 ppm to 60,000 ppm sulfate.
12. The composition of claim 11 wherein the wherein Z is one of a monoatomic ion from Groups 14 through 17 having a charge value between -1 and -3 or a polyatomic ion having a charge between -1 and -3 and x is an integer between 3 and 11 and y is an integer between 1 and 10.
13. The composition of claim 11 or 12 wherein Z is selected from the group consisting of sulfate, carbonate, phosphate, oxalate, chromate, dichromate, pyrophosphate and mixtures thereof.
14. The composition of claim 1 or 2 wherein the liquid material comprises a stoichiometrically balanced chemical composition of at least one of the following: hydrogen (1+), triaqua-p3-oxotri sulfate (1:1); hydrogen (1+), triaqua-p3-oxotri carbonate (1:1), hydrogen (1+), triaqua-p3-oxotri phosphate, (1:1); hydrogen (1+), triaqua-p3-oxotri oxalate (1:1); hydrogen (1+), triaqua-p3-oxotri chromate (1:1) hydrogen (1+), triaqua-p3-oxotri dichromate (1:1), hydrogen (1+), triaqua-p3-oxotri pyrophosphate (1:1), and mixtures thereof.
The composition of claim 1 or 2 further comprising at least one weak organic acid present in an amount between 0.1 and 5 vol%.
16. The composition of claim 15 wherein the at least one weak organic acids is selected from the group consisting of acetic acid, hydroxyacetic acid, citric acid, tartaric acid, maleic acid, furmaric acid and mixtures thereof.
17. The composition of claim 1 further comprising a carboxylic acid compound having the general formula:
wherein Ri is an unsaturated hydrocarbon moiety having between four and fourteen carbon atoms or a hydrocarbon moiety having between four and fourteen carbon atoms and at least one double bond; and wherein R2IS a one of -H, -OH, or -CH3; wherein the carboxylic acid component is present in an amount between 0.1 vol% and 3 vol%.
18. The composition of claim 17 wherein the carboxylic acid compound is selected from the group consisting of hexanoic acid, octanoic acid, decanoic acid, dodecanoic acid and mixtures thereof.
19. The composition of claim 1 or 2 further comprises a biosurfactant present in an amount between 0.1vol% and 3.0 vol%.
20. The composition of claim 19 wherein biosurfactant selected from the group consisting of rhamnolipid, sophorolipids, lecithins, steroid acids conjugated with taurine, steroid acids conjugated with glycine.
21. The composition of claim 1 or 2 wherein the liquid material component further
contains between 100 ppm and 800 ppm calcium.
22. The composition of claim 1 wherein the between 0.5 and 2.0 M free hydrogen present in the liquid material is derived from an inorganic acid selected from the group consisting, carbonic acid, oxalic acid, chromic acid, pyrophosphoric acid, phosphoric acid, and mixtures thereof.
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
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US202163163924P | 2021-03-21 | 2021-03-21 | |
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Citations (3)
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US7122269B1 (en) | 2002-05-30 | 2006-10-17 | Wurzburger Stephen R | Hydronium-oxyanion energy cell |
WO2018017735A1 (en) * | 2016-07-19 | 2018-01-25 | Tygrus, LLC | Stable electrolyte material and solvent material containing same |
US20190327963A1 (en) * | 2013-03-15 | 2019-10-31 | Purdue Research Foundation | Non-irritating antimicrobial compositions and methods of use |
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Patent Citations (3)
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US7122269B1 (en) | 2002-05-30 | 2006-10-17 | Wurzburger Stephen R | Hydronium-oxyanion energy cell |
US20190327963A1 (en) * | 2013-03-15 | 2019-10-31 | Purdue Research Foundation | Non-irritating antimicrobial compositions and methods of use |
WO2018017735A1 (en) * | 2016-07-19 | 2018-01-25 | Tygrus, LLC | Stable electrolyte material and solvent material containing same |
Non-Patent Citations (1)
Title |
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LADO C ET AL: "Study on the transfer of components of Aetheroleum carvi and Aetheroleum foeniculi oils", FITOTERAPIA, IDB HOLDING, MILAN, IT, vol. 76, no. 2, 1 March 2005 (2005-03-01), pages 166 - 172, XP025264954, ISSN: 0367-326X, [retrieved on 20050301] * |
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