Quick-acting aerosol for air disinfection and sterilization
By using an air purification preparation containing a high content of dipropylene glycol, combined with pressurized liquefied petroleum gas and a special nozzle, spraying the preparation into the air, the problem of insufficient sterilization efficiency in the prior art is solved, and rapid and effective air disinfection and sterilization are achieved.
Patent Information
- Application Number
- CN202280098914.9
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2022-06-17
- Publication Date
- 2025-03-21
AI Technical Summary
The prior art still has the problem of insufficient efficiency when developing bactericidal preparations that are effective for airborne pathogens, especially in the absence of significant bactericidal effect under low concentration dipropylene glycol preparations.
The formulation is introduced into the air through an aerosol can with an air purification formulation containing about 10% to 43% of dipropylene glycol, alcohol and water, combined with pressurized liquefied petroleum gas and a two-piece mechanical decomposition nozzle with a vortex chamber, to achieve rapid disinfection and sterilization.
It can significantly reduce the concentration of bacteria and viruses in the air within 0.1 to 5 minutes, achieve a reduction effect of 3log10 or higher, effectively disinfect and sterilize microorganisms in the air.
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Figure CN119677548A_ABST
Abstract
Description
Technical Field
[0001] An air purification product is disclosed, which contains an air purification formulation and a pressurized gas of about 60 psig or more in an aerosol can containing a two-piece mechanical disintegration (MB) nozzle with a vortex chamber. The air purification formulation contains about 10% to about 43% dipropylene glycol by weight of the formulation. The MB nozzle contains two rod holes, each with a diameter of about 0.036 inches [0.91 mm] to about 0.044 inches [1.12 mm]. The disclosed air purification formulation can reduce aerosol bacteria (including Staphylococcus aureus and Klebsiella pneumoniae) and aerosol enveloped viruses (including Phi6) by equal to or greater than 3 log in 0.1 to 5 minutes. 10 , so that for volumes less than or equal to 25m 3 Air disinfection and sterilization. Aerosol non-enveloped viruses (such as MS2) will produce 3log in 10-15 minutes 10 of reduction. Background Art
[0002] Indoor air can be an important vector for the transmission of a wide range of human pathogens, as demonstrated by the recent COVID-19 pandemic associated with severe acute respiratory coronavirus-2 (SARS-CoV-2).
[0003] U.S. Patent No. 2,333,124 to Robertson et al. discloses a method for sterilizing air using ethylene glycol vapor.
[0004] U.S. Pat. No. 2,719,129 to Richardson et al. discloses a liquid room and air deodorant composition comprising 0.5% to 5% of a quaternary morpholinium alkyl sulfate (whose alkyl group contains 8 to 24 carbon atoms) as a deodorant, about 80% to 95% of a liquefied, normally gaseous, low molecular weight halogenated hydrocarbon propellant, and sufficient amounts of polyols and partial esters of higher fatty acids having about 8 to 24 carbon atoms.
[0005] U.S. Patent No. 8,465,728 to SC Johnson & Son discloses an air treatment composition for eliminating malodors in the air and / or disinfecting the air, the composition being combined with a spray valve and actuator and spray performance parameters to maximize dispersion of the composition. Column 3, lines 21 to 23 indicate that the U.S. government has not adopted specific standards or methods for evaluating air disinfectants.
[0006] Various analytical methods and air samplers have been used to characterize airborne pathogens and overcome the challenges of collecting and analyzing these pathogens. See, e.g., Satter et al., Spread of viral infections by aerosols, Crit Rev Environ Control, 1987, 17:89-131; Yates et al., Manual of environmental microbiology, 4th ed., Washington (DC): ASM Press: 2015 p. 3.2.7-1-24; Verreault et al., Design of an environmentally controlled rotating chamber for bioaerosol aging studies, Inhal Toxicol 2014; 26:554-8; Ija et al., Survival characteristics of airborne human coronavirus 229E, J Gen Virol., Dec 1985, 66(Pt 12), 2743-8; and Ijaz et al., Development of methods to study the survival of airborne viruses, J Virol Methods, Nov 1987, 18(2-3), 87-106.
[0007] In DIS / TSS-11, dated September 3, 1980, the U.S. Environmental Protection Agency (EPA) recommended that products containing at least 5% glycols (triethylene glycol, dipropylene glycol and / or propylene glycol) must be quantitatively chemically determined using an air sampling device to demonstrate that glycol vapor saturation reaches or exceeds 50% in an enclosed laboratory room or test chamber.
[0008] The EPA's Office of Chemical Safety and Pollution Prevention (OCSPP) issued guidance OCSPP810.2500 on December 21, 2012, on how to conduct efficacy testing of antimicrobial pesticides used in air treatment to temporarily reduce the number of airborne bacteria. The guidance states that successful test results show that in the test air containing each required test bacteria, after calibration of the deposition rate, the number of viable bacteria is reduced by ≥99.9% (reduced by 3 log) compared to the parallel untreated control. 10 ).
[0009] Both EPA guidelines also note that there are currently no standard testing methods to evaluate the effectiveness of antimicrobial pesticides in temporarily reducing airborne germs.
[0010] In co-UK patent application 2111603.3, filed on August 12, 2021 and claiming priority to U.S. provisional patent application 63 / 217102 filed on June 30, 2022, applicants found that formulations with 28 to 38 wt% dipropylene glycol were effective in terms of bactericidal activity against airborne pathogens. In the examples, formulation D had 15 wt% dipropylene glycol but failed to provide significant bactericidal activity. Applicants initially speculated that the concentration was too low to provide sufficient dipropylene glycol vapor pressure.
[0011] There remains a need to develop germicidal formulations that are effective against airborne pathogens. Summary of the invention
[0012] An air cleaning product is disclosed, comprising an aerosol can comprising (a) a two-piece mechanical disintegration (MB) nozzle having a vortex chamber, (b) an air cleaning formulation, and (c) pressurized liquefied petroleum gas. The air cleaning formulation comprises, or consists essentially of, dipropylene glycol, alcohol, and water in an amount of about 10% to about 43% by weight of the formulation. The pressurized liquefied petroleum gas comprises a mixture of propane and butane sufficient to produce a pressure of at least 60 psig. The MB nozzle comprises two rod holes having a diameter of about 0.036 inches [0.91 mm] to about 0.044 inches [1.12 mm].
[0013] Alternatively, the disclosed air cleaning product comprises an aerosol can comprising (a) a two-piece mechanical disintegration (MB) nozzle having a vortex chamber, (b) an air cleaning formulation, and (c) pressurized liquefied petroleum gas. The air cleaning formulation comprises or consists essentially of: about 10% to about 43% dipropylene glycol by weight of the formulation; about 0.05% to about 0.2% of an odor-neutralizing cationic surfactant by weight of the formulation; about 28% to about 50% alcohol by weight of the formulation; and about 14% to about 33% water by weight of the formulation. The pressurized liquefied petroleum gas comprises a mixture of propane and butane sufficient to produce a pressure of at least 60 psig. The MB nozzle comprises two rod holes having a diameter of about 0.036 inches [0.91 mm] to about 0.044 inches [1.12 mm].
[0014] Alternatively, the air purification formulation contained in the disclosed air purification product consists of: about 10% to about 43% of dipropylene glycol by weight of the formulation; about 0.05% to about 0.2% of a cationic surfactant to neutralize odor by weight of the formulation; about 28% to about 50% of an alcohol, preferably ethanol, by weight of the formulation; about 14% to about 33% of water by weight of the formulation; about 0.043% to about 0.43% of a corrosion inhibitor by weight of the formulation; about 0.043% to about 0.43% of a pH adjuster by weight of the formulation; optionally 0% to about 0.28% of a defoamer by weight of the formulation; and optionally 0% to about 0.43% of a dye and / or fragrance by weight of the formulation.
[0015] The disclosed air purification products may include one or more of the following aspects:
[0016] 70% to about 80% by weight of (b) an air cleaning formulation;
[0017] about 20% to about 30% by weight of (c) pressurized liquefied petroleum gas;
[0018] Air purification agents are single-phase liquids;
[0019] The formulation contains alcohol:water in a ratio of about 1:1.3;
[0020] The formulation contains dipropylene glycol: water: alcohol in a ratio of about 1:2:2.3;
[0021] The propellant is a mixture of propane and isobutane;
[0022] The product contains essentially no dimethyl ether propellant;
[0023] The odor neutralizing cationic surfactant is a quaternary morpholinium alkyl sulfate compound;
[0024] The quaternary morpholinium alkyl sulfate compound is selected from the group consisting of soyethylmorpholiniumethosulfate, cetethylmorpholiniumethoxysulfate, N-myristyl-N-methylmorpholiniummethylsulfate and N-oleyl-N-methylmorpholiniummethylsulfate;
[0025] The quaternary morpholinium alkyl sulfate compound is soybean oil ethyl morpholinium ethosulfate and / or cetyl ethyl morpholinium ethosulfate;
[0026] The quaternary morpholinium alkyl sulfate compound is N-myristyl-N-methylmorpholinium methyl sulfate and / or N-oleyl-N-methylmorpholinium methyl sulfate;
[0027] The quaternary morpholinium alkyl sulfate compound is soybean oil ethyl morpholinium ethyl sulfate;
[0028] The quaternary morpholinium alkyl sulfate compound is cetyl ethyl morpholinium ethyl sulfate;
[0029] The quaternary morpholinium alkyl sulfate compound is N-myristyl-N-methylmorpholinium methyl sulfate;
[0030] The quaternary morpholinium alkyl sulfate compound is N-oleyl-N-methylmorpholinium methyl sulfate;
[0031] Air purification formulations also contain corrosion inhibitors;
[0032] The air cleaning formulation further comprises from about 0.043% to about 0.43% by weight of the formulation of a corrosion inhibitor;
[0033] The air cleaning formulation further comprises 0.043% to 0.43% by weight of the formulation of a corrosion inhibitor;
[0034] The air cleaning formulation further comprises from about 0.043% to about 0.43% by weight of the formulation of a pH adjuster;
[0035] The air purification formulation further comprises 0.043% to 0.43% by weight of the formulation of a pH adjuster;
[0036] The air cleaning formulation optionally further comprises 0% to about 0.28% of a defoaming agent by weight of the formulation;
[0037] The air purification formulation optionally further comprises 0% to 0.28% of a defoaming agent by weight of the formulation;
[0038] The air cleaning formulation further comprises from about 0.05% to about 0.43% by weight of the formulation of a dye and / or fragrance;
[0039] The air cleaning formulation further comprises 0.05% to 0.43% by weight of the formulation of a dye and / or fragrance;
[0040] The air purification preparation is substantially free of emulsifiers;
[0041] The air cleaning formulation is substantially free of nonionic surfactants; and / or
[0042] The air purification formulation is substantially free of amphoteric surfactants;
[0043] MB nozzles have an operator orifice with a diameter of about 0.016 inches (0.41 mm) to about 0.022 inches (0.56 mm);
[0044] MB nozzles have operator orifices with diameters from 0.016 inches (0.41 mm) to 0.022 inches (0.56 mm);
[0045] MB nozzles have an operator orifice with a diameter of about 0.017 inches (0.43 mm) to about 0.021 inches (0.53 mm);
[0046] MB nozzles have operator orifices with diameters from 0.017 inches (0.43 mm) to 0.021 inches (0.53 mm);
[0047] MB nozzles have an operator orifice with a diameter of about 0.018 inches (0.46 mm) to about 0.020 inches (0.51 mm);
[0048] MB nozzles have operator orifices with diameters of 0.018 in. (0.46 mm) to 0.020 in. (0.51 mm);
[0049] MB nozzles have stem steam taps with diameters from about 0.016 inches [0.41 mm] to about 0.025 inches [0.64 mm];
[0050] MB nozzles have stem steam taps with diameters from 0.016 in [0.41 mm] to 0.025 in [0.64 mm];
[0051] MB nozzles have stem steam taps with diameters from about 0.017 inches [0.43 mm] to about 0.024 inches [0.61 mm];
[0052] MB nozzles have stem steam taps with diameters from 0.017 in [0.43 mm] to 0.024 in [0.61 mm];
[0053] MB nozzles have stem steam taps with diameters from about 0.018 inches [0.46 mm] to about 0.023 inches [0.58 mm];
[0054] MB nozzles have stem steam taps with diameters from 0.018 in [0.46 mm] to 0.023 in [0.58 mm];
[0055] MB nozzles have stem steam taps with diameters from about 0.019 inches [0.48 mm] to about 0.022 inches [0.56 mm];
[0056] MB nozzles have stem steam taps with diameters from 0.019 in [0.48 mm] to 0.022 in [0.56 mm];
[0057] A two-piece MB nozzle produces a spray having an average particle size of about Dv
[50] =45 microns to about Dv
[50] =90 microns as measured using a laser diffractometer;
[0058] The two-piece MB nozzle produces a spray having an average particle size of Dv
[50] =45 μm to Dv
[50] =90 μm as measured using a laser diffractometer;
[0059] A two-piece MB nozzle produces a spray having an average particle size of about Dv
[50] =50 microns to about Dv
[50] =60 microns as measured using a laser diffractometer;
[0060] The two-piece MB nozzle produces a spray having an average particle size of Dv
[50] =50 μm to Dv
[50] =60 μm as measured using a laser diffractometer;
[0061] A two-piece MB nozzle produces a spray having an average particle size of about Dv
[50] =45 microns to about Dv
[50] =55 microns as measured using a laser diffractometer;
[0062] The two-piece MB nozzle produces a spray having an average particle size of Dv
[50] =45 μm to Dv
[50] =55 μm as measured using a laser diffractometer;
[0063] The two-piece MB nozzle produces a spray having a mean volume moment of Dv[4,3]=55 microns to Dv[4,3]=75 microns, preferably 60-70 microns, as measured using a laser diffractometer;
[0064] • The two-piece MB nozzle produces a spray with a mean volume moment of Dv[4,3]=60 microns to Dv[4,3]=70 as measured using a laser diffractometer.
[0065] Also disclosed is a method for disinfecting and sterilizing air within 0.1 to 5 minutes. The MB nozzle of the air purification product disclosed above is operated to introduce about 1.1 g / sec to about 2.0 g / sec of the air purification formulation into the air for about 10 to about 60 seconds, and the volume occupied by the air is less than or equal to 25 m 3 The air purification formulation may be introduced into the air in one continuous spray of 10 to 60 seconds. Alternatively, the air purification formulation may be introduced into the air in multiple continuous sprays totaling 10 to 60 seconds of spraying over a total time of less than 15 to 40 seconds. The disclosed method may include one or more of the following aspects:
[0066] Introducing the air purification formulation into the air for about 10 to about 45 seconds;
[0067] Introducing the air purification agent into the air for 10 to 45 seconds;
[0068] Introducing the air purification formulation into the air for about 10 to about 30 seconds;
[0069] Introduce the air purification agent into the air for 10 to 30 seconds;
[0070] Also disclosed is a method for disinfecting and sterilizing air within 0.1 to 5 minutes. Dipropylene glycol vapor at about 5 ppm to about 30 ppm, preferably about 9 ppm to about 12 ppm, is introduced into the air for about 10 to about 30 seconds, the volume of the air being less than or equal to 25 m 3 The dipropylene glycol vapor may be introduced in the form of a spray having a particle size of about Dv
[50] =45 micrometers to about Dv
[50] =90 micrometers, preferably about Dv
[50] =50 micrometers to about Dv
[50] =60 micrometers, as measured using a laser diffractometer.
[0071] The above embodiments are exemplary only. Other embodiments described herein are within the scope of the disclosed subject matter. BRIEF DESCRIPTION OF THE DRAWINGS
[0072] For a further understanding of the nature and purpose of the present invention, reference should be made to the following detailed description taken in conjunction with the accompanying drawings, wherein like elements are given the same or similar reference numerals, and wherein:
[0073] Figure 1 is a diagram of a two-piece MB nozzle aerosol valve assembly that can be used in the present invention;
[0074] Figure 2 is a diagram of a liquid electric evaporator that can be used in the present invention;
[0075] Figure 3 is a perspective view of an airborne biological test chamber used in the following examples;
[0076] Figure 4 is a flow chart of the steps performed in the following embodiments;
[0077] Figure 5 is the log of the microorganism being tested 10 Plots of concentration versus time;
[0078] Figure 6 is the log of the microorganism being tested 10 Plots of concentration versus time;
[0079] Figure 7 is a diagram of an OVS-7 sorbent tube used to sample DGP concentration in air;
[0080] Figure 8is an exemplary calibration chromatogram showing the elution times of three (3) different concentrations of DPG standards including DPG isomer peaks;
[0081] Fig. 9 It is a graph of the concentration of DPG in air (ppm) versus time (minutes).
[0082] definition
[0083] As used herein, the term "a" or "an" means one or more.
[0084] As used herein, the term "comprising" is inclusive or open-ended and does not exclude any other elements; the term "consisting of..." excludes any other elements; the term "consisting essentially of..." is intermediate and only allows the addition of elements that do not substantially affect the characteristics of the product or process.
[0085] As used herein, the term "about" or "approximately" means plus or minus 10% of the stated value.
[0086] As used herein, the weight percentage of an ingredient is based on the weight (grams) of the ingredient in the total weight (grams) of the formulation. When an ingredient does not contain close to or equal to 100% active material, two percentages may be provided: one for the weight of the ingredient and the other for the weight of the active agent. For example, 0.2 g of Forestall-LQ-(HM) sold by Croda contains about 35% soya oil base ethylmorpholinium ethosulfate in water, alcohol and / or polypropylene glycol, which is equivalent to about 0.07 g of soya oil base ethylmorpholinium ethosulfate in the formulation. This would be expressed as 0.2 g [0.07 g] of odor neutralizing cationic surfactant.
[0087] As used herein, any and all ranges are inclusive of their endpoints. For example, a formulation having a pH of 10.5 to 11.2 would include a formulation having a pH of 10.5, a formulation having a pH of 11.2, and a formulation having any pH between 10.5 and 11.2.
[0088] As used herein, the term "substantially free" means a concentration of less than 0.2 g / L, preferably less than 0.1 g / L, more preferably less than 0.05 g / L, and most preferably less than 0.001 g / L.
[0089] As used herein, the terms "bacteria" and "microorganism" or "microbial" refer to disease-causing microorganisms, including bacteria and viruses, and "microbicide" refers to an agent that inactivates (or kills) bacteria and microorganisms.
[0090] As used herein, the term "purification" means reducing the concentration of aerosol microorganisms in the air. The terms "disinfection" and "sterilization" mean reducing a volume of less than or equal to 25 m3 within 0.1 to 5 minutes. 3 The reduction of aerosol microorganisms (including Staphylococcus aureus and Klebsiella pneumoniae) and aerosol enveloped viruses (including Phi6) in the air was equal to or greater than 3log 10 .
[0091] As used herein, the term "vapor" refers to the gaseous state of DPG. Vapor does not include any droplets suspended in the air.
[0092] As used herein, the term "vortex chamber" may also be referred to as a cyclone chamber. DETAILED DESCRIPTION
[0093] Ethylene glycol vapor has been shown to reduce the number of viable airborne bacteria in confined spaces. See, for example, the US EPA's Efficacy Data and Labeling Requirements: Air Sanitizers, DIS / TSS-11, September 3, 1980; Robertson et al., A Study of the Bactericidal Activity invitro of Certain Glycols and Closely Related Compounds, The Journal of Infectious Diseases, Vol. 33, No. 2 (September-October 1948), pp. 124-137. Oust by SC Johnson TM Product labels for surface disinfectants and air sanitizers list 6.0% triethylene glycol as one of their active ingredients. As the examples below show, this concentration of triethylene glycol is unlikely to function as an air disinfectant as defined herein.
[0094] Triethylene glycol (TEG) is a colorless, odorless, viscous liquid. TEG has a boiling point of 285°C and a density of 1.1255 g / mL. TEG has a vapor pressure of 0.02 Pa at 20°C. TEG is soluble in ethanol and miscible in water. PCT Publication WO2007 / 117534 ('534 Publication) by SC Johnson discloses that ethanol must be added to TEG-based aerosol compositions to increase their solubility in hydrocarbon propellants. The '534 Publication further discloses that 12%-15% triethylene glycol will produce a two-phase system that consumers need to shake vigorously before use.
[0095] Dipropylene glycol (DPG) is a colorless, nearly odorless liquid. The boiling point of DPG is 227°C, the density at 20°C is 1.1255 g / mL, and the viscosity at 25°C is 75.0 cPs. The vapor pressure of DPG at 20°C is 2.7 Pa. At just below 100°C, the vapor pressure of DPG increases to about 250 Pa. DPG is soluble in ethanol and water. DPG is a mixture of three isomeric compounds: 4-oxa-2,6-heptanediol, 2-(2-hydroxypropoxy)propan-1-ol, and 2-(2-hydroxy-1-methylethoxy)propanol. Those skilled in the art will recognize that different isomers may have different properties. Applicants have found that DPG produced by non-catalyzed hydration of propylene oxide with water and subsequent vacuum distillation has consistent isomeric characteristics.
[0096] Initially, applicants believed that an air cleaning formulation containing about 28 wt % to about 43 wt % dipropylene glycol (DPG), about 0.12 wt % to about 0.43 wt % of a cationic surfactant to neutralize odor, about 28 wt % to about 50 wt % alcohol, and about 14 wt % to about 33 wt % water was needed to disinfect the air. The original theory was that "more is better", and higher concentrations of DPG were necessary to achieve sterilization.
[0097] Thereafter, the applicant discovered that the initial concentration of DPG vapor in the air is more important than the DPG concentration in the formulation. More particularly, as shown in the following examples, sterilization is achieved when the DPG vapor concentration in the air is about 5 to about 30 ppm, preferably about 9 to about 12 ppm. This concentration is much higher than the theoretical saturation of 2-3 ppm expected for DPG vapor, and significantly higher than 50% (i.e., 1-1.5 ppm) of the 50% theoretical saturation recommended by the EPA in DIS / TSS-11 of September 3, 1980. Therefore, the DPG vapor concentration in the air purification formulation can be as low as about 10% by weight, as long as the delivery mechanism produces about 5 to about 30 ppm of DPG in vapor form. In the following examples, this concentration is achieved by increasing the size of the rod hole in the aerosol nozzle to produce larger spray particles of about Dv
[50] =45 microns to about Dv
[50] 90 microns, preferably about Dv
[50] 45 microns to about Dv
[50] 55 microns or about Dv
[50] 50 microns to about Dv
[50] 60 microns. Alternative delivery mechanisms, such as piezoelectric vaporizers or nebulizers, may also be used as long as a DPG concentration in air of about 5 to about 30 ppm is achieved.
[0098] The disclosed air cleaning formulations contain about 10 wt % to about 43 wt %, preferably about 11 wt % to about 38 wt %, more preferably about 12 wt % to about 30 wt %, more preferably about 13 wt % to about 25 wt %, and most preferably about 14 wt % to about 20 wt % of dipropylene glycol.
[0099] Alternatively, the disclosed air purification formulations contain 10 wt % to 43 wt %, preferably 11 wt % to 38 wt %, more preferably 12 wt % to 30 wt %, more preferably 13 wt % to 25 wt %, and most preferably 14 wt % to 20 wt % of dipropylene glycol.
[0100] The disclosed air purification formulation comprises about 0.05 wt % to about 0.2 wt %, preferably about 0.6 wt % to about 0.15 wt % of a cationic surfactant for neutralizing odor. Alternatively, the disclosed air purification formulation comprises 0.05 wt % to 0.2 wt %, preferably 0.6 wt % to 0.15 wt % of a cationic surfactant for neutralizing odor. Exemplary cationic surfactants for neutralizing odor include, but are not limited to, quaternary morpholinium alkyl sulfate compounds, such as soybean oil base ethyl morpholinium ethyl sulfate, cetyl ethyl morpholinium ethyl sulfate, N-myristyl-N methyl morpholinium methyl sulfate, N-oleyl-N methyl morpholinium methyl sulfate or a combination thereof. Soybean oil base ethyl morpholinium ethyl sulfate and / or cetyl ethyl morpholinium ethyl sulfate are particularly preferred cationic surfactants for neutralizing odor. Exemplary commercial sources of soya ethyl morpholinium ethosulfate include the product sold by Croda under the trade name Forestall-LQ-(HM).Exemplary commercial sources of cetyl ethyl morpholinium ethosulfate include the product sold by Lonza under the trade name Barquat cme-A.
[0101] As described above, DPG is soluble in water and ethanol. The percentage of water and alcohol in the disclosed air purification formulation is very important for obtaining the best vaporization of DPG and cationic surfactants that neutralize odors. The air purification formulation comprises (a) a combination of about 33% to about 55% by weight of alcohol and about 38% to about 19% of water; and (b) a suitable dispensing device. In aerosol distribution applications using hydrocarbon gases, a combination of about 45% to about 55% by weight of alcohol and about 29% to about 38% of water is particularly preferred, and a combination of about 45% to about 50% by weight of alcohol and about 32% to about 37% by weight of water is more preferred. Preferably, for aerosol applications, the formulation comprises alcohol: water in a weight ratio of about 1.3: 1. Preferably, for aerosol applications, the formulation comprises dipropylene glycol: water: alcohol in a weight ratio of about 1: 2: 2.3. Those skilled in the art will recognize that the propellant helps to dry the distributed droplets and aerosolize the formulation. Non-aerosol applications will need to be formulated to compensate for the low vapor pressure of DPG and eliminate the drying effect provided by aerosols. Thus, a combination of about 7% to about 12% alcohol by weight and about 0.5% to about 4% water can be provided for any dispensing device that does not utilize a propellant. For non-aerosol applications, the formulation preferably contains dipropylene glycol:water:alcohol in a ratio of about 10:1 to about 3:1.
[0102] Ethanol is a preferred alcohol due to its safety features. However, the combination of C1-C6 alcohols can be used for disclosed air purification formulations without departing from the teachings of this article. For example, the amount of alcohol in the formulation can include 95% ethanol and 5% tert-butyl alcohol, or 98% ethanol and 2% isopropanol (e.g., about 14% by formulation weight to about 47% ethanol by formulation weight, and about 1% by formulation weight to about 3% tert-butyl alcohol by formulation weight). Those skilled in the art will recognize that alcohol and propellant are volatile organic compounds (VOCs), so the concentrations of the two are also selected to remain within any government's VOC limits.
[0103] The disclosed formulation is a single liquid phase, so consumers do not need to shake it before use. Compared with two-phase formulations, single-phase formulations are also generally easier to manufacture, vaporize, and exhibit fewer stability issues. The order of addition of the disclosed formulation ingredients is not critical. Specifically, the raw materials for producing the disclosed air purification formulation can be mixed in one pot to reduce manufacturing complexity. The resulting formulation has a viscosity similar to that of water (i.e., 0.89 mPa·s at 25°C).
[0104] The disclosed air purification formulation does not require any emulsifier or amphoteric or nonionic surfactant, because these ingredients will combine to form a single liquid phase. Emulsifiers may also produce foam, which is disadvantageous. For example, the disclosed air purification formulation is substantially free of partial esters of polyacids, alcohols or ethers, such as glyceryl monostearate, mannitol monostearate, propylene glycol monostearate or diethylene glycol monostearate. The disclosed air purification formulation is substantially free of glyceryl dilaurate, ethylene glycol monopalmitate, propylene glycol monolaurate, ethylene glycol monostearate or propylene glycol monopalmitate. Those skilled in the art will recognize that fragrances may contain trace amounts of these ingredients. However, any trace ingredients contained in any fragrance are used as fragrances themselves and will not provide an amount sufficient to affect the properties of the disclosed air purification formulation. Therefore, the disclosed formulation may contain 0% to about 0.1% by weight, more preferably 0% to about 0.075% by weight, and most preferably 0% to about 0.05% by weight of any emulsifier and a combination of amphoteric and nonionic surfactants.
[0105] The disclosed air purification formulation also includes a pH regulator that maintains a pH at about 10.0 to about 11.2. Exemplary pH regulators include, but are not limited to, inorganic bases, alkanolamines, or combinations thereof. Exemplary inorganic bases include hydroxides, such as sodium hydroxide, potassium hydroxide, magnesium hydroxide, ammonium hydroxide, or combinations thereof. Exemplary alkanolamines include monoethanolamine, diethanolamine, triethanolamine, methylethylhydroxypropylhydroxylamine, or combinations thereof. Buffers may also be used as pH regulators, such as glycine and sodium hydroxide, ammonia and ammonium chloride, sodium dihydrogen phosphate and sodium hydroxide, or combinations thereof.
[0106] When disposed in a metal or alloy container, the disclosed air purification formulation may also optionally include a corrosion inhibitor. The corrosion inhibitor reduces the reaction between the air purification formulation and the metal or alloy container. The same ingredient can provide the formulation with buffering and corrosion inhibition capabilities. The disclosed air purification formulation may optionally include about 0.03 wt % to about 0.3 wt % of a corrosion inhibitor. Exemplary corrosion inhibitors include, but are not limited to, sodium hydroxide, sodium benzoate, sodium nitrite, sodium silicate, sodium lauryl sarcosinate, borates, or combinations thereof. An exemplary borate corrosion inhibitor may include a mixture of monoethanolamine (MEA) borate and monoisopropanolamine (MIPA) borate. An exemplary suitable commercial source of MEA / MIPA borate corrosion inhibitors is available from Croda under the trade name Crodacor. TM BE sales.
[0107] Alternatively, the metal or alloy container may include an internal coating that prevents reaction between the metal or alloy container and its contents. Exemplary coatings include, but are not limited to, silicon oxide coatings.
[0108] Aerosol formulations typically contain defoamers to prevent foaming. Defoamers can also be used to solubilize other ingredients (e.g., fragrances). The disclosed formulations do not produce a large amount of foam, so defoamers are not mandatory unless required for a specific fragrance. The disclosed air purification formulations may optionally contain 0% to about 0.28% by weight of defoamers. Exemplary defoamers include, but are not limited to, PEG-12 polydimethylsiloxane. An exemplary suitable commercial source of PEG-12 polydimethylsiloxane is available from Dow under the trade name Xiameter TM OFX-0193Fluid for sale.
[0109] The disclosed air cleaning formulations may optionally further comprise dyes and / or fragrances.
[0110] A particularly preferred air cleaning formulation consists of: 10% to about 43% by weight of the formulation of dipropylene glycol; about 0.05% to about 0.2% by weight of the formulation of a cationic surfactant to neutralize odor; about 28% to about 50% by weight of the formulation of an alcohol, preferably ethanol; about 14% to about 33% by weight of the formulation of water; optionally 0% to about 0.43% by weight of the formulation of a corrosion inhibitor; optionally 0% to about 0.43% by weight of the formulation of a pH adjuster; optionally 0% to about 0.29% by weight of the formulation of a defoamer; and optionally 0% to about 0.43% by weight of the formulation of a dye and / or fragrance.
[0111] The disclosed air cleaning formulations can be packaged in single-use or multiple-use aerosol cans. Alternatively, the disclosed air cleaning formulations can be packaged in non-aerosol containers and vaporized using a mechanical device (e.g., a piezoelectric evaporator or a nebulizer). As described above, due to the lower vapor pressure of DPG and the drying effect provided by the aerosol, the concentrations of alcohol and water in the disclosed air cleaning formulations need to be adjusted for non-aerosol applications.
[0112] The disclosed air cleaning product comprises about 70 wt % to about 80 wt % of an air cleaning formulation and about 20 wt % to about 30 wt % of pressurized liquefied petroleum gas. The concentration of the pressurized liquefied petroleum gas helps to obtain a desired DPG concentration in the air.
[0113] The disclosed air purification formulation reduces the concentration of bacteria in the air and can disinfect and sterilize the air. For testing purposes, the air can be contained in an area of less than or equal to 25m 3The air volume is used for comparative testing purposes only and the disclosed formulations may be used for larger areas without departing from the teachings herein. About 1.1 g / sec to about 2.0 g / sec of the above disclosed aerosol air cleaning formulation is introduced into the air for about 10 to about 60 seconds, preferably about 10 to about 45 seconds, and more preferably about 10 to about 30 seconds. The air cleaning formulation may be introduced into the air by one (1) spray or multiple, sequential, shorter sprays.
[0114] As shown in the following examples, the disclosed air purification formulations reduced Staphylococcus aureus, Klebsiella pneumoniae, and Phi6 by 3 log in 0.1 to 5 minutes. 10 . Staphylococcus aureus is one of the most difficult bacteria to eliminate. Klebsiella pneumoniae is one of the easiest bacteria to eliminate. Phi6 is a bacteriophage that serves as a test surrogate for enveloped viruses (such as SARS-CoV-2, coronaviruses, and influenza viruses). The disclosed air purification formulations can also be used to reduce the concentration of small non-enveloped viruses, as shown in the example below for MS2 bacteriophage. Those skilled in the art will recognize that non-enveloped viruses are more difficult to inactivate than bacteria and enveloped viruses. Therefore, the disclosed air purification formulations require longer time to inactivate MS2 than Staphylococcus aureus, Klebsiella pneumoniae, and Phi6.
[0115] The disclosed air cleaning product comprises an aerosol can containing an air cleaning formulation and a propellant. The aerosol container is filled with a liquid air cleaning formulation and a propellant at a pressure approximately equal to or slightly greater than the vapor pressure of the propellant. The air cleaning product comprises about 70% to about 80% by weight of the air cleaning formulation and about 20% to about 30% by weight of the propellant.
[0116] The propellant is a pressurized liquefied petroleum gas (LPG). The propellant is not dimethyl ether (DME). DME is not compatible with a variety of packaging components (such as plastics and rubber). LPG comprises a mixture of propane and butane, which is enough to produce a pressure of at least 60psig, preferably about 70psig to about 80psig. For example, the pressurized liquefied petroleum gas can include about 40% by weight to about 60% by weight of propane gas and about 40% by weight to about 60% by weight of isobutane gas. An exemplary gas suitable for the teachings of this paper has 42.89% by weight of propane and 57.11% by weight of isobutane. The gas can be purchased from multiple suppliers as an A-70 hydrocarbon mixture with a pressure of 70psig.
[0117] The aerosol can includes a two-piece mechanical disintegration (MB) nozzle with a vortex chamber. The MB nozzle includes two rod holes, each with a diameter of about 0.036 inches [0.91 mm] to about 0.044 inches [1.12 mm]. The size of each of the two rod holes in the disclosed air purification product increases the discharge rate of the air purification formulation. The size of the rod hole also increases the particle size of the resulting spray.
[0118] The particle size of the resulting spray is from about Dv
[50] =45 microns to about Dv
[50] =90 microns, preferably from about Dv
[50] =50 microns to about Dv
[50] =60 microns or from about Dv
[50] =45 microns to about Dv
[50] =55 microns. Those skilled in the art will recognize that Dv
[50] is the maximum particle size at which 50% of the sample volume exists. A wide range of commercially available particle size measurement equipment is available, including but not limited to laser diffraction, dynamic light scattering, electrophoretic light scattering, automated imaging, sedimentation, electrostatic sensing and sieving, which are preferred techniques for the disclosed particle sizes, with laser diffraction being particularly preferred.
[0119] The average volume moment of the obtained spray measured by laser diffractometer is Dv[4,3]=55 μm to Dv[4,3]=75 μm, preferably Dv[4,3]=60 μm to Dv[4,3]=70 μm. The volume moment reflects the size of most particles in the sample.
[0120] As described in the following examples, tests were conducted using two or four rod holes. Although four rod holes helped increase the flow rate of the disclosed air cleaning formulation, the particle size in the resulting spray was inconsistent and irregular. The size of the two rod holes in the disclosed air cleaning product produced less turbulence of the desired volume and a smaller spray size of the air cleaning formulation than four rod holes.
[0121] Applicants were surprised by the rod hole and spray particle size required. One skilled in the art would not expect these parameters to successfully produce vaporized glycol. One skilled in the art would expect to use a spray of smaller particles for better vaporization to occur. The increased discharge rate caused by the rod hole size fills the air with vaporized material, producing about 5ppm to about 30ppm of DPG vapor in the air, preferably about 9 to about 12ppm of DPG vapor. This air saturation creates an environment that allows glycol to decompose rapidly on bacterial surfaces. DPG creates a liquid film on the surface of any bacteria in the air, resulting in osmotic imbalance and subsequent inactivation of the bacteria. Applicants believe that DPG prevents viral particles from replicating.
[0122] Figure 11 is a diagram of an exemplary two-piece MB nozzle aerosol valve assembly 100 that can be used to dispense the disclosed air purification formulation. The valve assembly 100 is connected to the mounting cup 101. The mounting cup 101 is crimped onto the aerosol can (not shown) in an airtight manner. The gasket 102 seals the joint between the top of the valve assembly housing 104, the mounting cup 101 and the rod 103. The rod 103 extends from the valve assembly housing 104 through the gasket 102 and the mounting cup 101 to the operator 105. The valve assembly housing 104 includes a housing hole 107, a steam tap 108 and a spring 109. The spring 109 holds the valve assembly housing 104 in a closed position. The rod 103 includes a rod hole 110 and an expansion chamber 111. Figure 1 The single rod hole 110 in the disclosed product is for illustration purposes only. The two rod holes 110 in the disclosed product are located on both sides of the rod 103. However, the location of the two rod holes 110 should not affect the resulting particle spray rate and size. The operator 105 includes a vortex chamber 114 that is fluidly connected to the operator hole 112. Figure 1 The operator 105 in the valve assembly is at right angles to the rod 103 and the operator hole 112. Those skilled in the art will recognize that a straight path may also be used without departing from the teachings herein. The dip tube 106 is connected to the bottom of the valve assembly housing 104.
[0123] When the operator 105 is depressed, the stem 103 moves downward, thereby opening the seal between the gasket 102 and the stem hole 110. The propellant forces the disclosed air purifying formulation into the dip tube 106 and into the valve assembly housing 104 through the housing hole 107. The propellant enters the valve assembly housing 104 through the steam tap 108 and mixes with the disclosed air purifying formulation inside the valve assembly housing 104. The propellant both dries the air purifying formulation and initiates the formation of aerosol droplets and subsequent glycol vapor. The generation of glycol vapor is absolutely critical to the denaturation of airborne microorganisms. Applicants have discovered that the propellant must have a pressure of at least 60 psig to vaporize the disclosed air purifying formulation. The air purifying formulation / propellant blend enters the expansion chamber 111 from the valve assembly housing 104 through the stem hole 110. From the expansion chamber 111, the formulation enters the vortex chamber 114 through the operator 105 and then is ejected from the operator hole 112 as an aerosol spray.
[0124] Many swirl chambers 114 are commercially available. For example, see U.S. Patent No. 3,583,642 of SC Johnson & Son, the contents of which are incorporated herein by reference in their entirety. The swirl chamber 114 is one of the factors that produce aerosol particles of the desired size. The result of the initial R&D tests conducted without the swirl chamber 114 was that visible spray appeared on the floor below the nozzle. Those skilled in the art will recognize that pinholes can also produce aerosol particles of the appropriate size.
[0125] The size of the operator hole 112 in the disclosed air purification product and the combination of the propellant provide the projection of the spray. The aerosol spray travels from the operator hole about 7 feet (2.1m) to about 9 feet (2.7m). The combination allows the aerosol of larger size to shrink over time due to evaporation. The combination also allows the aerosol to cover a larger area than the standard fine mist spray. The diameter of the operator hole is about 0.016 inches (0.41mm) to about 0.022 inches (0.56mm), preferably about 0.017 inches (0.43mm) to about 0.021 inches (0.53mm), and more preferably about 0.018 inches (0.46mm) to about 0.020 inches (0.51mm). Alternatively, the diameter of the operator hole is 0.016 inches (0.41 mm) to 0.022 inches (0.56 mm), preferably 0.017 inches (0.43 mm) to 0.021 inches (0.53 mm), and more preferably 0.018 inches (0.46 mm) to 0.020 inches (0.51 mm).
[0126] The size of the steam tap 108 is another factor that helps determine the size of the aerosol particles. Reducing the size of the steam tap 108 reduces the ratio of propellant to air purification formulation and reduces the retention of formulation in the tank. However, reducing the size of the steam tap 108 also increases the size of the aerosol particles, which may prevent the aerosolization of the formulation due to the lower vapor pressure of the DPG. In other words, as shown in some of the following examples, the aerosol particle size of the disclosed air purification formulation is too large to cause visible liquid to appear on the floor below the tank nozzle. The liquid on the floor cannot provide effective air disinfection. As described above, the increase in the pressure of the propellant allows a larger size of the aerosol spray to have the ability to shrink with distance and time. Therefore, the pressure of the disclosed air purification product is above 60psig. This difference is most significant in the comparison of Examples D and N.
[0127] The size of the housing aperture 107 also affects the size of the aerosol particles. A reduction in the size of the housing aperture 107 reduces the size of the aerosol particles.
[0128] The size of the rod hole 110 also affects the size of the aerosol particles. A reduction in the size of the rod hole 110 reduces the size of the aerosol particles.
[0129] The two-piece MB nozzle aerosol valve assembly 100 includes an operator hole 112 having a diameter of about 16 μm to about 22 μm, a steam tap 108 having a diameter of about 0.016 inches [0.41 mm] to about 0.025 inches [0.64 mm], and two stem holes 110 each having a diameter of about 0.036 inches [0.91 mm] to about 0.044 inches [1.12 mm].
[0130] Alternatively, the two-piece MB nozzle aerosol valve assembly 100 includes an operator hole 112 having a diameter of 16 μm to 22 μm, a steam tap 108 having a diameter of 0.016 inches [0.41 mm] to 0.025 inches [0.64 mm], and two stem holes 110 each having a diameter of 0.036 inches [0.91 mm] to 0.044 inches [1.12 mm].
[0131] In another alternative, the two-piece MB nozzle aerosol valve assembly 100 includes an operator hole 112 having a diameter of about 17 μm to about 21 μm, a steam tap 108 having a diameter of about 0.017 inches [0.43 mm] to about 0.024 inches [0.61 mm], and two stem holes 110 each having a diameter of about 0.037 inches [0.94 mm] to about 0.043 inches [1.09 mm].
[0132] In another alternative, the two-piece MB nozzle aerosol valve assembly 100 includes an operator hole 112 having a diameter of 17 μm to 21 μm, a steam tap 108 having a diameter of 0.017 inches [0.43 mm] to 0.024 inches [0.61 mm], and two stem holes 110 each having a diameter of 0.037 inches [0.94 mm] to 0.043 inches [1.09 mm].
[0133] In another alternative, the two-piece MB nozzle aerosol valve assembly 100 includes an operator hole 112 having a diameter of about 18 μm to about 20 μm, a steam tap 108 having a diameter of about 0.018 inches [0.43 mm] to about 0.023 inches [0.61 mm], and two stem holes 110 each having a diameter of about 0.038 inches [0.97 mm] to about 0.042 inches [1.07 mm].
[0134] In another alternative, the two-piece MB nozzle aerosol valve assembly 100 includes an operator hole 112 having a diameter of 18 μm to 20 μm, a steam tap 108 having a diameter of 0.018 inches [0.43 mm] to 0.023 inches [0.61 mm], and two stem holes 110 each having a diameter of 0.038 inches [0.97 mm] to 0.042 inches [1.07 mm].
[0135] In another alternative, the two-piece MB nozzle aerosol valve assembly 100 includes an operator hole 112 having a diameter of about 18 μm to about 20 μm, a steam tap 108 having a diameter of about 0.019 inches [0.48 mm] to about 0.022 inches [0.56 mm], and two stem holes 110 each having a diameter of about 0.038 inches [0.97 mm] to about 0.042 inches [1.07 mm].
[0136] In another alternative, the two-piece MB nozzle aerosol valve assembly 100 includes an operator hole 112 having a diameter of 18 μm to 20 μm, a steam tap 108 having a diameter of 0.019 inches [0.48 mm] to 0.022 inches [0.56 mm], and two stem holes 110 each having a diameter of 0.038 inches [0.97 mm] to 0.042 inches [1.07 mm].
[0137] As shown in the following examples, the disclosed air purification formulation is used in combination with the two-piece MB nozzle aerosol valve assembly 100 to sterilize the air within 0.1 to 5 minutes. The operator 105 is pressed for about 10 to about 60 seconds to introduce about 1.1 g / second to about 2 g / second of the air purification formulation into the area less than or equal to 25 m 3 The operator 105 can be manually pressed. Alternatively, the operator 105 can automatically remain pressed for the desired dispensing duration. For example, the valve assembly 100 can include a solenoid switch disclosed in PCT Publication Nos. WO2007 / 045826, WO2007 / 045827, and WO2007 / 045828, the contents of which are incorporated herein by reference. More particularly, the valve assembly 100 can include a movable magnetic rod 103 surrounded by a copper coil (not shown), and an iron bracket (not shown) surrounding the copper coil. The current applied to the copper coil can move the magnetic rod 103 to an open or closed position.
[0138] Alternatively, the disclosed non-aerosol air-purifying formulation can also be evaporated using an elevated temperature delivered by a liquid electric vaporizer. The non-aerosol air-purifying formulation comprises or consists essentially of about 84 wt % to about 92.5 wt % of dipropylene glycol, about 7 wt % to about 12 wt % of alcohol, and about 0.5 wt % to about 4 wt % of water. An exemplary liquid electric vaporizer 201 is shown in FIG. Figure 2 As shown, the PCT publication No. WO2019 / 038529 of Reckitt Benckiser (Brand) Co., Ltd. is borrowed. Figure 2, the contents of which are incorporated herein by reference in their entirety. The liquid electric vaporizer 201 is generally composed of a housing 203 having an electrical plug 208 and a heater 202, and a removable refill bottle 204 having a wick 205 or other liquid transfer mechanism (e.g., a ceramic coil). The wick 205 may form a portion of the refill bottle 204. The removable refill bottle 204 contains the disclosed air purification preparation 213. The removable refill bottle 204 may generally hold about 20 mL to about 25 mL of the air purification preparation 213, but those skilled in the art may easily adjust it to hold about 100 mL to about 500 mL to achieve the purposes disclosed herein. Those skilled in the art will recognize that the single-phase nature of the disclosed air purification preparation and the stability associated therewith make it particularly suitable for liquid electric evaporation. After the refill bottle 204 is inserted into the housing 203, the wick 205 or the ceramic coil is located near the heater 202. When the liquid electric vaporizer 201 is plugged into an electrical outlet, the heater 202 is activated, thereby distributing the air purification preparation. Figure 2 The liquid electric vaporizer 201 in the embodiment also includes a chimney 206. The chimney 206 has an opening 207 through which the vaporized active substance leaves the evaporator 201. As described above, when about 1.1 g / sec to about 2 g / sec of an aerosol air purification formulation is introduced into the air for about 10 seconds to about 60 seconds, the air can be disinfected and sterilized. In the absence of an aerosol, when about 0.825 g / sec to about 1.125 g / sec of a non-aerosol purification formulation is introduced into the air for about 30 seconds to about 60 seconds, air disinfection and sterilization are expected to occur. Non-aerosol applications need to be formulated to compensate for the low vapor pressure of DPG and remove the need for drying (provided by aerosol). Therefore, the disclosed formulation can be provided for any dispensing device that does not use a propellant. For non-aerosol applications, the formulation preferably contains alcohol: water in a ratio of about 10:1 to 3:1.
[0139] Those skilled in the art will recognize that there are a variety of liquid electric vaporizers and can be used with the disclosed air purification formulations without departing from the teachings of this article. For example, the chimney 206 of the liquid vaporizer 201 may include a chimney extension that extends farther on the distal side than the proximal side to help guide the flow of the vaporized material away from the wall and into the room. The liquid vaporizer 201 may also or alternatively include an electronic control device to increase the power applied to the heater 202, and thus increase the emission rate of the vaporized air purification formulation, as disclosed in PCT Publication No. WO2011 / 045615 of Reckitt & Colman (Overseas) Co., Ltd., the contents of which are incorporated herein by reference in their entirety. The electronic control device can also be programmed to provide sufficient heat for vaporization for about 30 seconds to about 60 seconds at intermittent time intervals (e.g., every 4, 8, 12 or 24 hours).
[0140] The following examples list exemplary embodiments of the present invention. It should be understood that these examples are only for illustration, and more examples can be generated based on the teachings of the present invention.
[0141] Example
[0142] The following examples are Figure 3 The volume of the aerobiological testing chamber 1 is about 24 m 3 About 25m 3 . Chamber 1 is located in a clean room with negative pressure and controlled access (not shown). The ceiling, floor and walls of chamber 1 are made of wipeable white corrugated plastic sheets 3, which are fixed to the frame 4 of chamber 1 to maintain an airtight seal and prevent air exchange between chamber 1 and the clean room. Although other colors can also be used without departing from the teachings of this document, the white corrugated plastic sheet provides better visibility to any residual product stains. The wipeable corrugated plastic sheet 3 used in the following examples is 0.0157 inches (0.4 cm) thick and was purchased from Coroplast Fritz Müller GmbH & Co. at Home Depot under the name Coroplast TM Brand sales. The walls should be grounded to dissipate static electricity that may accumulate. Static discharge wires (not shown) can help discharge the accumulated static electricity. Chamber 1 can also include transparent plastic windows, sealable access doors, and inlets and outlets for HEPA filtration systems. A more detailed description of some exemplary chambers 1 can be found in Sattar et al., Spread of viral infections by aerosols, Crit Rev Environ Control, 1987, 17: 89-131; Sattar et al., Decontamination of indoor air to reduce the risk of airborne infections: Studies on survival and inactivation of airborne pathogens using an aerobiology chamber, American Journal of Infection Control, 44 (2016) e177-e182, the contents of both of which are incorporated herein by reference in their entirety.
[0143] Muffin fan 5, also known as axial flow fan, is placed on the floor in chamber 1, directly below the 3.8 cm diameter inlet pipe 6 leading to 6 nozzle atomizer 7. 6 nozzle collision atomizer 7 produces microbial aerosol with a respirable range of 0.5 μm to 5.0 μm. The atomizer 7 used in the following examples is the MRE CN24 / 25 type purchased from CHTechnologies in New Jersey, USA. Atomizer 7 is connected to a cylinder of ultra-dry compressed air with a pressure regulator and a backflow preventer (not shown). The fan 5 used is Nidec Alpha V, TA300, A31022-20 type provided by Nidec Corp of Braintree, Massachusetts, USA, part number 933314 3.0 inches / 7.62m diameter, output 30CFM. Data logger (not shown) records the relative humidity and air temperature of the chamber. The following examples use the wireless data logger of RTR-503L type of CASData Loggers in Chesterland, Ohio, USA. A magnetometer (not shown) records the pressure differential between the inside and outside of chamber 1. The following examples used a magnetometer purchased from ITM Instrument, Ontario, Canada.
[0144] An externally placed slit-to-agar airsample with a built-in vacuum pump 10 was used to sample the sample at a rate of 1 ft. 3 The air in chamber 1 was sampled at a rate of (28.3 L) / min. The sampler 10 used in the examples was purchased from PinPoint Scientific of Bridgend, Wales. The air flowing out of the sampler 10 was either captured by a HEPA filter in the device 10 or discharged directly to the facility's HEPA filtered exhaust system (not shown). The sampler 10 drew an air sample from the center of chamber 1 through an outlet tube 11 having a diameter of 5.0 cm.
[0145] As discussed by Zargar et al. on page S136, when fan 5 is placed at a 45° angle at the bottom of one side of chamber 1 and operated at a speed of 2800 RPM, a uniform distribution of aerosol particles in the air within chamber 1 can be achieved. Mathematical modeling and simulation of bacterial distribution in an aerobiology chamber using computational fluid dynamics, American Journal of Infection Control 44 (2016) S127-S137, the contents of which are incorporated herein by reference in their entirety. Zargar et al. further disclosed that a post-nebulization time of 5 minutes is sufficient to evenly distribute the introduced bacterial aerosol throughout the chamber. As above, Zargar et al. further disclosed that an air sample collected from the center of chamber 1 is sufficient to provide a representative overview of the concentration of airborne bacteria present in chamber 1. As above.
[0146] Figure 4 is a flow chart of the steps performed in the following example. In step 1, the fan 5 is turned on to start air circulation in chamber 1. In step 2, the environmental parameters in chamber 1 are checked and adjusted as needed. In step 3, the slit to agar sampler 10 is activated for 2 minutes to obtain a sample of any background contamination in chamber 1. After closing the sampler 10, the bacteria, virus or bacteriophage to be tested enters chamber 1 through the nebulizer 7 and the air inlet pipe 6. In this step 4, the nebulizer 7 is operated for 10 minutes. The nebulizer 7 is then turned off and the bacteria, virus or bacteriophage is allowed to stabilize in chamber 1 for 5 minutes. The concentration of bacteria, virus or bacteriophage produced in chamber 1 in step 4 should be a minimum of 4.2log 10 / m 3 Up to 5.0log 10 CFU / m 3 between.
[0147] Any meaningful air purification assessment requires that the aerosolized challenge microorganisms remain viable in the air long enough so that their biological decay or physical deposition can be properly distinguished from inactivation or removal by the technology being evaluated. In step 4, the test microorganisms (i.e., bacteria and bacteriophages) are aerosolized into chamber 1. Steps 5a and 5b are initially skipped, providing a comparative baseline reading of biological decay or physical deposition. In step 6, samples are collected at predetermined intervals over a specified time using a slit-to-agar sampler 10, for example every 2 minutes for 8 hours. The plates are incubated at 36°C ± 1°C, colony forming units (CFU) or plaque forming units (PFU) are recorded, and the data is analyzed to determine the biological decay rate. The results are as follows: Figure 5Then in step 7, chamber 1 is flushed with fresh air for one hour to eliminate contamination, and the process then starts again from step 1.
[0148] Repeat steps 1 to 4 for different product samples. In step 5a, the slit-to-agar sampler 10 is run for 2 minutes to determine the initial concentration of the challenge microorganism. In step 5b, the decontaminated product to be tested may enter chamber 1 through an inlet 12 in the wall 2 of chamber 1. Alternatively, the decontaminated sample may be placed in chamber 1 prior to step 1, and the sample may be approached and activated in step 5b using a glove 13 secured to the wall 2 of chamber 1. In step 6, the slit-to-agar sampler 10 is used to collect samples at predetermined intervals over a specified time, for example, every 2 minutes for 8 hours. The intervals and time periods for determining biological decay and physical sedimentation should match the intervals and time periods for determining inactivation using the test product. The culture plates are incubated at 36°C ± 1°C, the colony forming units (CFU) or plaque forming units (PFU) are recorded, and the data is analyzed to determine the inactivation rate. The results are as shown in FIG. Figure 5 Chamber 1 is then flushed with fresh air for one hour in step 7 to eliminate contamination, and the process is restarted with a new sample in step 1.
[0149] Figure 5 is the log of the microorganism being tested 10 Concentration versus time. The black line shows the biodegradation rate of the challenge strain. The red line shows the inactivation rate of the challenge strain by the test product. Since the initial titers of the two experiments may be different, the biodegradation data must be converted so that its initial titer is equal to the initial titer of the inactivation test. This conversion step is easily accomplished by a person skilled in the art. The modified biodegradation is shown in blue. The logarithm of natural or biodegradation to inactivation in contact times of less than 5 minutes is shown in Figure 1. 10 Reduction value equal to or greater than 3log 10 Successful disinfection results can be obtained.
[0150] The lyophilized test microorganisms were obtained from a reputable source, such as the American Type Culture Collection (ATCC). The microorganisms were isolated using standard techniques. The bacteria were cultured to provide approximately 1.6 × 10 4 CFU / m 3 About 1.0×10 5 CFU / m 3 The nebulizer solution was prepared by adding 50 μL of cultured bacteria, 0.75 mL of bovine serum albumin (BSA), 1.05 mL of yeast extract, 3.0 mL of mucin, and 10 μL of antifoam A (from Sigma-Aldrich, catalog number A-5633) to 10.14 mL of Dulbecco's phosphate buffered saline (PBS).
[0151] The formulations in the following examples were prepared using the ingredients shown in Table A:
[0152] Table A:
[0153]
[0154] The formulations in the following examples were tested using the aerosol nozzles shown in Table B, all of which used a two-piece mechanical breakaway operator with a swirl chamber ("Two-piece MB").
[0155] Table B:
[0156]
[0157] Example 1: Staphylococcus aureus
[0158] R&D samples of the following formulations were tested against Staphylococcus aureus (ATCC 6538).
[0159] Table 1 lists the formulations and aerosol nozzles used in the tests:
[0160] Table 1:
[0161]
[0162] The particle size produced by Formulation N was measured using a Malvern laser diffractometer with a 300 mm lens at 6 inches from the beam. The average Dv(50) of 3 separate measurements was 54.83 microns. The average volume moment D[4,3] of 3 separate measurements was 63.88 microns.
[0163] Staphylococcus aureus reduced by 3 log 10 , demonstrating the efficacy of the spray. Table 2 lists the spray time, temperature, relative humidity percentage (%RH) and results, if any:
[0164] Table 2:
[0165]
[0166] N / A - This data is currently unavailable
[0167] *There are small droplets under the tank, but not on the floor, probably condensation
[0168] **Average of 3 tests
[0169] Table 2 provides (a) specific log reduction of Staphylococcus aureus 10 The time required to (b) reduce S. aureus by 3 log 10 Time required (if S. aureus is indeed reduced by 3 log 10). When the formulation reduces Staphylococcus aureus by 3 log in 5 minutes or less 10 When the air disinfectant is effective, it can be considered a successful air disinfectant.
[0170] Those skilled in the art will recognize that microbiological test results are not as consistent as chemical test results. Microbiological test results may vary from test to test, even if all other parameters remain constant. In an R&D testing environment, greater variability in microbiological test results is also expected. Those skilled in the art will further recognize that airborne bacteria concentrations can fluctuate over time. In addition, real-time air samples may contain residual bacteria when product concentrations are suboptimal / not efficient enough to quickly kill all bacteria. In other words, Formulation I was able to reduce the number of Staphylococcus aureus by 3 log in 5.75 minutes after 25 seconds of spraying. 10 , but after 120 minutes the reduction dropped to 2.86 log 10 , multiple factors may have contributed to this result.
[0171] It can be seen that despite the high concentration of ethanol, the combination of low concentration DPG and low pressure of formulations B, C and D does not produce sufficient vapor pressure to achieve sterilization. Formulation E shows that increasing the concentration of DPG is not enough to overcome the limitations of the low pressure NP-46 propellant. Initially, the best results were obtained with an aerosol formulation containing dipropylene glycol, water, and alcohol in a ratio of about 1.25:1:1.5.
[0172] Formulation D, which was about 2:1 alcohol:water, produced a noticeable spray on the floor. Applicants believe that the propellant may have caused the higher concentration of ethanol to evaporate more quickly. For aerosol formulations containing alcohol:water ratios of about 1.3:1 to 1.5:1, no spray was visible on the floor.
[0173] The 30-second spray of formulations F, I, and N and the 60-second spray of formulation F successfully achieved air disinfection and sterilization. The 15-second spray of formulation F showed that it could sometimes produce 3 log 10 In contrast, Formulations I and N produced more consistent results in repeated tests at 30 seconds. Formulation N was also tested against Klebsiella pneumoniae (ATCC 4352). In the presence of stain load, ≥3 log was achieved in 1.17 minutes 10 This result is expected, since Klebsiella pneumoniae is more easily inactivated than S. aureus.
[0174] Table 2 further shows that increasing the spray time (e.g., 60 seconds for Formulations B and D) or increasing the percentage of DPG in the formulation (e.g., 35% in Formulations J and K) alone is not sufficient to provide suitable microbicidal results. The viscosity of Formulations J and K is too high to convert DPG into the gas phase even at a pressure of 70 psig.
[0175] Figure 6 is a plot of the log 10 concentration of S. aureus versus time for Formulation L. It can be seen that both 20 and 30 second nebulization times provide a rapid reduction in the concentration of S. aureus.
[0176] Those skilled in the art will recognize that a spray time of 20 to 30 seconds is longer than the average consumer would expect to press a spray button. Applicants expect to achieve similar efficacy after multiple but shorter consecutive spray times. For example, ten (10) consecutive 2 to 3 second sprays, or four (4) to six (6) consecutive 5 second sprays with <1- to 2 second pauses between sprays, are expected to produce similar results.
[0177] Example 2: Phi6 and MS2
[0178] 3 log reduction of Phi6 or MS2 after 30 s nebulization time 10 The spraying time, temperature, relative humidity percentage (%RH) and results are shown in Table 3:
[0179] Table 3:
[0180]
[0181] As mentioned above, Table 3 demonstrates that non-enveloped viruses like MS2 are more difficult to inactivate than bacteria and enveloped viruses like Phi6. Nevertheless, formulations J and N, nebulized for 30 seconds, were still able to provide 3 log 10 The concentration decreases.
[0182] Example 3: DPG vs TEG
[0183] Four (4) formulations in Table 4 were tested against S. epidermidis to evaluate the efficacy of DPG relative to TEG: TEG alone, DPG alone, TEG-DPG blend, and TEG based. S. epidermidis is a safer bacteria, equally related to S. aureus, and an alternative to multiple nosocomial vegetative pathogens with airborne potential. Approximately 200 g of product was placed in chamber 1 (i.e., the entire can).
[0184] Table 4:
[0185] TEG only DPG only TEG-DPG blends Based on TEG <![CDATA[H2O]]> 36.8 36.8 33.8 49.03 DPG 0 3 3 0 TEG 3 0 3 5.4 CI 0.2 0.2 0.2 0.1 EtOH 40 40 40 20.42 Quat 0 0 0 0.15 Prop 20 20 20 24.9
[0186] The DPG and TEG-DPG only formulations showed a 4.56 log 10 Mean baseline titer decreased by ≥3 log 10 The TEG-only formulation showed a mean log 10 at 10 minutes of 1.33 compared to a mean baseline low of 4.83 log 10. 10 Reduced, average log of 2.35 at 60 minutes 10 The TEG-based formulation showed a 4.36 log decrease from the mean baseline 10 In comparison, the average log at 10 minutes was 1.59 10 The average log of 2.93 at 60 minutes 10 The data indicate that DPG is a more effective airborne microbicide than TEG.
[0187] Example 4 DPG concentration in air
[0188] The DPG concentration in air of Formulation N was determined using capillary gas chromatography (GC) with a FID detector.
[0189] exist Figure 3 The slit of the agar air sampler 10 is connected to the agar air sampler 10 by using a pump (not shown) and Figure 7 Custom Occupational Safety and Health Administration (OSHA) Multipurpose Sampler (OVS) sorbent tubes (specifically Configuration 7 (OVS-7)) are shown to collect air samples. The pump is calibrated to within ±5% of the recommended flow rate.
[0190] The custom adsorbent tube has two sections: a 5.0 cm long section with an inner diameter of 11 mm and an outer diameter (od) of 13 mm gradually narrows to a 2.5 cm long section with an od of 6 mm. A foam plug is set in the 13 mm od section until it reaches the junction with the 6 mmo.d. section. 140 mg of a hydrophobic organic porous polymer adsorbent sold by Rohm and Haas under the trade name XADTM-7 is added to the 13 mm od section to form a layer between the foam plugs, and a second foam plug is added. An additional 270 mg of polymer adsorbent is added to the 13 mmo.d. section, followed by a glass fiber filler and finally a polytetrafluoroethylene (PTFE) container. These tubes are currently available as custom products from SKC Inc. (Article No. 226-57), Supelco and Forest Biomedical.
[0191] The 6 mm od end of the custom tube is attached to the pump with flexible tubing. The custom tube can be positioned vertically with the 13 mmo.d. end of the tube pointing outward at an angle, 76 to 101.6 cm from the ground.
[0192] Measure the initial weight of the aerosol can containing Formulation N and record it as t 0 , keep two decimal places. Using gloves 13, spray the aerosol into the test chamber 1 in a sweeping motion towards the center of the chamber for 30 seconds. Turn on the sampling pump and sample at the intervals specified in the table below.
[0193] Record room temperature, pressure, relative humidity, aerosol can final weight, and sample volume (liters of air) for each sample and blank test run.
[0194] Dissolve the test sample, blank control sample and standard sample in 2mL of isopropyl alcohol (IPA). Immediately seal the sample tube and extract / desorb it by shaking manually or using a sonicator for 30 minutes. Transfer a portion of the extracted IPA solution to a 4mL vial suitable for the GC autosampler. Run at least 2 injections for each sample. Calibrate the GC using a three-point external standard curve and quantify in the range of 5 to 300ppm. Figure 8 is an exemplary calibration chromatogram showing the elution times of 3 different concentrations of DPG standards including the DPG isomer peaks.
[0195] The DPG concentration of the sample (in ppm) is calculated as (YC) / M, where Y is the DPG peak area in the GC chromatogram, C is the y-intercept in the GC chromatogram, and M is the slope of the 3-point original standard curve. The PPM of total DPG is the sum of the DPG from the absorbent layers in the front and back of the sample tube. The replicate analysis acceptance criterion (RAAC) is [result of injection 1 / result of injection 2)-1]*100 and must be within ±10% to be acceptable. The DPG concentration in the air sample is calculated as:
[0196]
[0197] in:
[0198] Total ppmDPG = Concentration of DPG in the sample
[0199] DV = Desorption Volume = 2 mL Isopropanol
[0200] 24.46 = molar volume at 25°C and 760 mm HG (liters / mole)
[0201] Liters = number of liters of air sample
[0202] DE = desorption efficiency = 1
[0203] MW = molecular weight (g / mole) = 134.17
[0204] 5.488 = MwDPG / 24.45 (unit conversion factor)
[0205] The results are summarized in Table 5 and Fig. 9 middle.
[0206] Table 5:
[0207]
[0208] *Time is defined as the midpoint of the measurement (e.g., 0-2 minutes = 1, 4-6 minutes = 5, etc.)
[0209] From Table 5 and Fig. 9 It can be seen that the initial concentration of DPG in the air measured 0-2 minutes after stopping the spray aerosol is about 12ppm. Those skilled in the art will recognize that the DPG concentration in the air will be higher than 12ppm during the spraying process, especially at the end of the spraying process. About 10-15 minutes after the spraying is completed, the DPG concentration in the air reaches an almost stable state of 2-4ppm, consistent with the expectation based on the vapor pressure of DPG. This data emphasizes that DPG must be applied in a state of almost supersaturated steam, causing the steam to remain at this concentration unstably. This scenario causes the steam to decompose quickly on the external structure of the microorganism, helping to destroy it. Lower concentrations of DPG tend to bind and settle on the vertical surface of the treatment area instead of decomposing on the microorganism.
[0210] Example 4: Piezoelectric delivery
[0211] A formulation containing 18.667 wt % DPG, 34.253 wt % deionized water and 47.08 wt % ethanol was prepared. The mixture produced a single phase clear solution. The solution was placed in a 100% ethanol solution manufactured by Reckitt under the brand Air Wick TM In the EssentialMist Diffuser sold by , details of which are disclosed in PCT Publication No. WO2017 / 216548 of Reckitt Benckiser (Brand) Ltd. More specifically, the solution is placed in a refill bottle containing a core formed of polypropylene. The bottle is placed in an atomizer and sprayed successfully without any spray being visible on the atomizer or on the surface supporting the atomizer. The formulation has been successfully tested in gravity-fed piezoelectric devices. Testing is being conducted with these devices to determine DPG concentrations in air.
[0212] The above description of various aspects of the present invention is for the purpose of illustration and description. The embodiments and / or features therein may be freely combined with each other. This is not intended to be exhaustive or to limit the present invention to the precise form disclosed, and it is obvious that many modifications and variations may be made. Modifications and variations obvious to those skilled in the art should be included within the scope of the present invention as defined by the appended claims.
Claims
1. An air purification product, comprising an aerosol can, wherein the aerosol can comprises: (a) Two-piece mechanical disintegration (MB) nozzle with swirl chamber or disintegration strip, (b) an air purification preparation, the air purification preparation comprising: (i) from about 10% to about 43%, preferably from about 11% to about 38%, by weight of the formulation, of dipropylene glycol; (ii) alcohol; and (iii) water; and (c) pressurized liquefied petroleum gas comprising a blend of propane and butane sufficient to produce a pressure of at least 60 psig; The MB nozzle includes two rod holes, each having a diameter of about 0.036 inches [0.91 mm] to about 0.044 inches [1.12 mm].
2. The air purification product according to claim 1, wherein: The air cleaning formulation is a single-phase liquid.
3. The air purification product according to claim 1 or 2, wherein: The air cleaning formulation also comprises an odor neutralizing cationic surfactant, preferably a quaternary morpholinium alkyl sulfate compound.
4. The air purification product according to any one of claims 1 to 3, wherein: The air purification preparation comprises: (iii) from about 35% to about 55%, by weight of the formulation, of ethanol; and (iv) from about 29% to about 38% water, by weight of the formulation.
5. The air purification product according to any one of claims 1 to 4, wherein: The formulation contained dipropylene glycol:water:alcohol in a ratio of about 1:2:2.
3.
6. The air cleaning product of any one of claims 1 to 5, comprising about 70% to about 80% by weight of (b) the air cleaning formulation and about 20% to about 30% by weight of (c) the pressurized liquefied petroleum gas.
7. An air purification product as described in any one of claims 1 to 6, wherein the MB nozzle further comprises an actuator hole, wherein the diameter of the actuator hole is from about 0.016 inches [0.41 mm] to about 0.022 inches [0.56 mm], preferably from about 0.017 inches [0.43 mm] to about 0.021 inches [0.53 mm], and more preferably from about 0.018 inches [0.46 mm] to about 0.020 inches [0.51 mm].
8. The air purification product of any one of claims 1 to 7, wherein the MB nozzle further comprises a stem steam tap having a diameter of about 0.016 inches [0.41 mm] to about 0.020 inches [0.51 mm].
9. The air purification product according to any one of claims 1 to 8, wherein: The MB nozzle produces a spray having a particle size of about Dv[50]=45 to about Dv[50]=90 microns, preferably about Dv[50]=50 to about Dv[50]=60 microns or about Dv[50]=45 to about Dv[50]=55 microns.
10. The air purification product according to any one of claims 1 to 9, wherein: The MB nozzle produces a spray having a mean volume moment of about Dv[4,3]=55 to about Dv[4,3]=75 microns, preferably about Dv[4,3]=60 to about Dv[4,3]=70 microns.
11. A method of sterilizing air in 0.1 to 5 minutes, the method comprising generating about 5 ppm to about 30 ppm of dipropylene glycol in vapor form.
12. A method of reducing the concentration of viruses in air within 0.1 to 5 minutes, the method comprising producing about 5 ppm to about 30 ppm of dipropylene glycol in vapor form.
13. The method according to claim 11 or 12, wherein: The virus was an enveloped virus and a 3 log10 reduction was achieved in less than 5 minutes.
14. The method according to claim 11 or 12, wherein: The virus is non-enveloped and achieved a 3 log10 reduction in less than 15 minutes.
15. The method according to any one of claims 11 to 14, wherein: The dipropylene glycol in vapor form is produced by operating the MB nozzle of the air purification product according to any one of claims 1 to 10.
Citation Information
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