WO2023106385A1 - 定量噴射型エアゾール - Google Patents
定量噴射型エアゾール Download PDFInfo
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- WO2023106385A1 WO2023106385A1 PCT/JP2022/045384 JP2022045384W WO2023106385A1 WO 2023106385 A1 WO2023106385 A1 WO 2023106385A1 JP 2022045384 W JP2022045384 W JP 2022045384W WO 2023106385 A1 WO2023106385 A1 WO 2023106385A1
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- aerosol
- injection
- solvent
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- GRVDJDISBSALJP-UHFFFAOYSA-N methyloxidanyl Chemical group [O]C GRVDJDISBSALJP-UHFFFAOYSA-N 0.000 description 1
- 229960002216 methylparaben Drugs 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000002903 organophosphorus compounds Chemical class 0.000 description 1
- 235000010292 orthophenyl phenol Nutrition 0.000 description 1
- 239000004306 orthophenyl phenol Substances 0.000 description 1
- 150000004866 oxadiazoles Chemical class 0.000 description 1
- 235000020636 oyster Nutrition 0.000 description 1
- 235000019271 petrolatum Nutrition 0.000 description 1
- 150000008048 phenylpyrazoles Chemical class 0.000 description 1
- 239000000419 plant extract Substances 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
- 235000013824 polyphenols Nutrition 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000003755 preservative agent Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000004405 propyl p-hydroxybenzoate Substances 0.000 description 1
- 235000010232 propyl p-hydroxybenzoate Nutrition 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 229960003415 propylparaben Drugs 0.000 description 1
- 239000002728 pyrethroid Substances 0.000 description 1
- NHDHVHZZCFYRSB-UHFFFAOYSA-N pyriproxyfen Chemical compound C=1C=CC=NC=1OC(C)COC(C=C1)=CC=C1OC1=CC=CC=C1 NHDHVHZZCFYRSB-UHFFFAOYSA-N 0.000 description 1
- 230000001846 repelling effect Effects 0.000 description 1
- 229910000030 sodium bicarbonate Inorganic materials 0.000 description 1
- 235000017557 sodium bicarbonate Nutrition 0.000 description 1
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 description 1
- XNRNJIIJLOFJEK-UHFFFAOYSA-N sodium;1-oxidopyridine-2-thione Chemical compound [Na+].[O-]N1C=CC=CC1=S XNRNJIIJLOFJEK-UHFFFAOYSA-N 0.000 description 1
- 229940126589 solid medicine Drugs 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 150000005846 sugar alcohols Polymers 0.000 description 1
- 235000018553 tannin Nutrition 0.000 description 1
- 239000001648 tannin Substances 0.000 description 1
- 229920001864 tannin Polymers 0.000 description 1
- 229960005199 tetramethrin Drugs 0.000 description 1
- CXBMCYHAMVGWJQ-UHFFFAOYSA-N tetramethrin Chemical compound CC1(C)C(C=C(C)C)C1C(=O)OCN1C(=O)C(CCCC2)=C2C1=O CXBMCYHAMVGWJQ-UHFFFAOYSA-N 0.000 description 1
- 239000004308 thiabendazole Substances 0.000 description 1
- WJCNZQLZVWNLKY-UHFFFAOYSA-N thiabendazole Chemical compound S1C=NC(C=2NC3=CC=CC=C3N=2)=C1 WJCNZQLZVWNLKY-UHFFFAOYSA-N 0.000 description 1
- 235000010296 thiabendazole Nutrition 0.000 description 1
- 229960004546 thiabendazole Drugs 0.000 description 1
- 229960000790 thymol Drugs 0.000 description 1
- 229960003500 triclosan Drugs 0.000 description 1
- YFNKIDBQEZZDLK-UHFFFAOYSA-N triglyme Chemical compound COCCOCCOCCOC YFNKIDBQEZZDLK-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 229940043810 zinc pyrithione Drugs 0.000 description 1
- PICXIOQBANWBIZ-UHFFFAOYSA-N zinc;1-oxidopyridine-2-thione Chemical compound [Zn+2].[O-]N1C=CC=CC1=S.[O-]N1C=CC=CC1=S PICXIOQBANWBIZ-UHFFFAOYSA-N 0.000 description 1
- 229930007845 β-thujaplicin Natural products 0.000 description 1
Images
Classifications
-
- 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
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
- A01N25/06—Aerosols
-
- 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
- A01P7/00—Arthropodicides
- A01P7/04—Insecticides
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K3/00—Materials not provided for elsewhere
- C09K3/30—Materials not provided for elsewhere for aerosols
Definitions
- the present invention relates to a metered injection type aerosol.
- Patent Literature 1 describes an aerosol composition that contains an insecticide that is volatile at room temperature as an active ingredient and maintains the concentration of the active ingredient in the air for a long time by spraying a very small amount.
- aerosols general continuous-injection aerosols and fixed-injection aerosols are known.
- the fixed quantity injection type aerosol the amount of medicine ejected by one injection operation is fixed.
- metered injection type aerosols there is room for investigation as to how to treat solid medicines at room temperature over a wider range and to increase their effectiveness.
- the purpose of the present invention is to provide a means that can enhance the effect of a room-temperature solid drug in a treatment using a metered injection type aerosol.
- the present invention relates to the following (1) to (3).
- a constant injection type aerosol that has a pressure container and an aerosol composition filled in the pressure container and that injects a fixed amount of the aerosol composition in one injection operation, wherein the aerosol composition comprises a room temperature solid drug, a solvent and a propellant;
- a metered injection aerosol wherein a latent heat of vaporization of a mixture comprising the solvent and the propellant is 10.00 kcal/mol or less.
- the metered-dose aerosol according to (1) wherein the room-temperature solid agent is a room-temperature solid pest control component.
- a metered injection type aerosol that injects a fixed amount of aerosol composition in one injection operation, and the latent heat of vaporization of the injected mixture consisting of the solvent and the propellant is within a specific range.
- the room-temperature solid agent adheres to the treated surface extensively and uniformly. This can enhance the effect of the room-temperature solid drug.
- FIG. 1 is a microscope photograph showing the state of chemical deposition after aerosol injection in Example 1.
- FIG. FIG. 2 is a microscope photograph showing the state of chemical deposition after aerosol injection in Example 2.
- FIG. 3 is a microscope photograph showing the state of chemical deposition after aerosol injection in Example 3.
- FIG. 4 is a microscope photograph showing the state of chemical deposition after aerosol injection in Example 4.
- FIG. 5 is a microscope photograph showing the state of chemical deposition after aerosol injection in Example 5.
- FIG. FIG. 6 is a microscope photograph showing the state of chemical deposition after aerosol injection in Example 6.
- FIG. 7 is a microscope photograph showing the chemical deposition state after the aerosol injection in Example 7.
- FIG. FIG. 8 is a microscope photograph showing the state of chemical deposition after aerosol injection in Example 8.
- FIG. 9 is a microscopic photograph showing the state of chemical deposition after the aerosol injection in Example 9.
- FIG. 10 is a microscope photograph showing the chemical deposition state after the aerosol injection in Example 10.
- FIG. 11 is a microscope photograph showing the state of chemical deposition after application of the chemical solution in Comparative Example 1.
- FIG. 12 is a microscope photograph showing the state of chemical deposition after aerosol injection in Comparative Example 2.
- FIG. 13 is a microscope photograph showing the state of chemical deposition after aerosol injection in Comparative Example 3.
- FIG. FIG. 14 is a microscope photograph showing the state of chemical deposition after application of the chemical solution in Comparative Example 4.
- FIG. 15 is a microscope photograph showing the state of chemical deposition after application of the chemical solution in Comparative Example 5.
- FIG. 10 is a microscope photograph showing the chemical deposition state after the aerosol injection in Example 10.
- FIG. 11 is a microscope photograph showing the state of chemical deposition after application of the chemical solution in Comparative Example 1.
- FIG. FIG. 12 is a microscope photograph showing the state
- the metered-dose aerosol of the present invention comprises a pressure-resistant container and an aerosol composition filled in the pressure-resistant container.
- the aerosol composition contains a room-temperature solid drug (hereinafter also referred to as "medicine") as an active ingredient, a solvent, and a propellant.
- the solid state at room temperature means that it is solid at room temperature, that is, around 25°C, and the vapor pressure at 25°C is preferably 25 mPa or less.
- the room-temperature solid state includes, for example, a crystalline solid state, a powdery solid state, and the like.
- An active ingredient refers to a substance that exerts some action when a metered dose aerosol is used.
- the room-temperature solid drug that is the active ingredient but examples thereof include room-temperature solid pest control ingredients, aromatic ingredients, deodorizing ingredients, and disinfecting/sterilizing ingredients. Each component will be described below.
- the pest control component is a component capable of killing, repelling (including flushing out), or knocking down target pests.
- the type of pest control component is not particularly limited as long as it is solid at room temperature, and preferably has a vapor pressure of 25 mPa or less at 25°C. Also, known compounds can be used.
- room-temperature solid pest control components include pyrethroid compounds such as phthalthrin, etofenprox, bifenthrin, and fenpropathrin; carbamate compounds such as propoxur; Organophosphorus compounds, oxadiazole compounds such as methoxadiazone, neonicotinoid compounds such as dinotefuran, metadiamide compounds such as brofuranilide, phenylpyrazole compounds such as fipronil, and others, pyriproxyfen, diflubenzuron, hydramethylnon, amidoflumet and the like. These may be used individually by 1 type, and may be used in combination of 2 or more type.
- Target pests include, for example, flying pests such as mosquitoes, flies, moths, bees, gadflies, black flies, butterfly flies, midges, and leafhoppers, cockroaches, bedbugs, mites, stink bugs, ants, spiders, pill bugs, lice, centipedes, stink bugs, and ticks. , millipedes, termites, bark beetles, earthworms, earwigs, stains, fleas, triatomine bugs, longhorn beetles, deer beetles, bookworms, burs, and creeping pests, and crawling pests are preferred.
- flying pests such as mosquitoes, flies, moths, bees, gadflies, black flies, butterfly flies, midges, and leafhoppers
- cockroaches bedbugs, mites, stink bugs, ants, spiders, pill bugs, lice, centipedes, stink bugs, and ticks.
- Room-temperature solid deodorant ingredients include sodium hypochlorite, baking soda, catechins (epicatechin gallate, epigallocatechin gallate, etc.), flavonoids, polyphenols, plant extracts (oyster tannin, green tea extract, grapefruit seed extract, yuzu seed extract), metal-based deodorants such as silver, copper and zinc. These may be used individually by 1 type, and may be used in combination of 2 or more type.
- Normal-temperature solid disinfecting/sterilizing ingredients are ingredients that remove or kill microorganisms, molds, and bacteria.
- disinfecting/sterilizing components include isopropylmethylphenol, chlorinated isocyanurate, cetylpyridinium chloride, thymol, hinokitiol, triclosan, methylparaben, ethylparaben, propylparaben, butylparaben, 4-chloro-3,5-dimethylphenol.
- the above drugs can be used by combining ingredients with different effects.
- the content of the drug is preferably 0.01 to 90% by mass/volume in terms of the total amount of the drug and solvent (hereinafter also referred to as "stock solution").
- stock solution solvent
- the lower limit of the drug content is more preferably 0.1% by mass/volume or more, still more preferably 0.3% by mass/volume or more, particularly preferably 0.5% by mass/volume or more, and 1% by mass/volume.
- % by volume is most preferable, and the upper limit is more preferably 80% by mass/volume or less, further preferably 65% by mass/volume or less, particularly preferably 50% by mass/volume or less, and most preferably 15% by mass/volume.
- the drug is solid at room temperature, it is preferably dissolved or dispersed in a solvent in the stock solution from the viewpoint of handling.
- a volatile solvent is particularly preferred because it is required to dissolve or disperse the drug in the aerosol composition and to gradually volatilize after the aerosol composition is jetted to deposit the drug.
- volatile solvents include organic solvents such as glycol ether solvents, hydrocarbon solvents, alcohol solvents, aromatic solvents, ester solvents, and water.
- the volatile solvent is not particularly limited as long as it is volatile at room temperature, but the vapor pressure at 25° C. is preferably 50 Pa or more, more preferably 100 Pa or more, and particularly 1000 Pa or more. preferable.
- a surfactant may also be used.
- glycol ether solvents include propylene glycol monopropyl ether, propylene glycol monobutyl ether, dipropylene glycol monopropyl ether, dipropylene glycol monobutyl ether, dipropylene glycol dimethyl ether, ethylene glycol monoisobutyl ether, diethylene glycol monoisobutyl ether, and diethylene glycol. dibutyl ether, diethylene glycol dimethyl ether, triethylene glycol dimethyl ether and the like.
- hydrocarbon-based solvents include aliphatic hydrocarbons such as paraffinic hydrocarbons and naphthenic hydrocarbons, and alicyclic hydrocarbons, and kerosene such as JIS No.
- 1 kerosene is preferred.
- Specific examples include normal paraffin and isoparaffin.
- Typical normal paraffins have 8 to 16 carbon atoms, and examples thereof include Neothiosol manufactured by Sanko Kagaku Kogyo Co., Ltd. and normal paraffin MA manufactured by ENEOS Corporation.
- Isoparaffins typically have 8 to 16 carbon atoms, such as IP Clean LX manufactured by Idemitsu Kosan Co., Ltd., and the like.
- alcohol solvents include lower alcohols such as ethanol, normal propanol and isopropanol, and polyhydric alcohols such as ethylene glycol.
- aromatic solvents include toluene and xylene.
- ester solvents examples include isopropyl myristate, hexyl laurate, isopropyl palmitate and the like.
- alcoholic solvents are preferable, and lower alcohols such as ethanol, normal propanol, and isopropanol are more preferable because they are excellent in the solubility or dispersibility of the normal-temperature solid drug.
- One of the above solvents may be used alone, or two or more thereof may be used in combination.
- the stock solution can contain other ingredients as long as the effects of the present invention are not impaired.
- Other components include, for example, preservatives, pH adjusters, ultraviolet absorbers, inorganic substances, surfactants, dissolution aids, and the like.
- the content of the stock solution in the aerosol composition can be appropriately changed according to the purpose of use of the metered injection type aerosol and the combination with the propellant, and is not particularly limited. can be When the content of the stock solution in the aerosol composition is 1% by volume or more, the surface area of the drug remaining on the treated surface increases, so that the amount of pest insects that take up the drug and the frequency of contact with the drug can be increased. A good pest control effect can be obtained. In addition, when the content of the stock solution in the aerosol composition is 90% by volume or less, the stock solution can be sprayed as sprayed particles, so that, for example, the drug can be sufficiently and uniformly attached to the target site.
- the lower limit is more preferably 5% by volume or more, and the upper limit is more preferably 70% by volume or less in the aerosol composition.
- the propellant is a medium for injecting the undiluted liquid consisting of the drug and the solvent, and is pressure-filled into the pressure-resistant container together with the drug and the solvent.
- the propellant include liquefied petroleum gas (LPG) such as propane, propylene, n-butane and isobutane, liquefied gas such as dimethyl ether (DME), compressed gas such as carbon dioxide, nitrogen gas, and compressed air, and HFC-152a. , HFC-134a, HFO-1234yf, HFO-1234ze, and other halogenated carbon gases.
- LPG liquefied petroleum gas
- DME dimethyl ether
- the content of the propellant in the aerosol composition can be appropriately changed according to the purpose of use of the metered dose aerosol and the combination with the stock solution, and is not particularly limited.
- the lower limit of the propellant content in the aerosol composition is more preferably 30% by volume or more, and the upper limit is more preferably 95% by volume or less.
- the volume ratio of the stock solution to the propellant in the aerosol composition is preferably 1:99 to 90:10, more preferably 3:97 to 80:20, even more preferably 5:95 to 70:30. . By setting it as such a volume ratio, the effect of a sufficient chemical
- the latent heat of vaporization of the mixture of solvent and propellant is 10.00 kcal/mol or less, preferably 9.80 kcal/mol or less. It is preferable that the latent heat of vaporization of the mixture of the solvent and the propellant is 10.00 kcal/mol or less, because the drug in the composition is unlikely to aggregate on the treated surface. Also, the latent heat of vaporization of the mixture of solvent and propellant is preferably 1.00 kcal/mol or more. When it is 1.00 kcal/mol or more, the drug in the composition spreads sufficiently on the treated surface, which is preferable.
- the above latent heat of vaporization is a numerical value at 0° C. (273.15 K).
- polar liquids refer to liquids composed of polar molecules, such as ethanol, isopropanol, isopropyl myristate, water, and dimethyl ether.
- nonpolar liquids refer to liquids composed of molecules that do not have polarity, such as normal paraffin, isoparaffin, propane, butane, and ethane.
- the metered-dose aerosol of the present invention comprises a pressure-resistant container and the aerosol composition filled in the pressure-resistant container.
- the pressure container has its opening closed by an aerosol valve.
- a fixed quantity injection type aerosol is an aerosol that injects a fixed amount of an aerosol composition in one injection operation.
- a fixed quantity injection type aerosol is a spray member attached to an aerosol valve (hereinafter also referred to as a spray button) that is operated by the user to pass through the aerosol valve and spray a fixed amount of the aerosol composition in a pressure container.
- the stock solution is granulated by a propellant and sprayed as spray particles.
- the aerosol valve includes an opening/closing member for switching between communication and disconnection between the inside and the outside of the pressure vessel when the injection member is operated by the user, a housing to which the opening/closing member is attached, and the housing at a predetermined position in the pressure vessel.
- a mounting member is provided for holding.
- the opening/closing member includes a stem that slides up and down in conjunction with the injection member. By sliding the stem, communication (injection state) and blocking (non-injection state) of the aerosol composition are switched.
- the aerosol valve is formed with a housing hole for taking in the aerosol composition from the pressure container and a stem hole for sending the taken in aerosol composition to the injection member.
- the path from the housing bore to the stem bore constitutes an internal passageway through which the aerosol composition passes.
- the aerosol valve is a fixed quantity type aerosol valve that performs a fixed quantity injection by operating the injection member once.
- the injection amount of the aerosol valve can be set in the range of 0.1 mL or more in one injection operation, preferably in the range of 0.2 to 5 mL, more preferably in the range of 0.2 to 3 mL. It is By setting the injection amount within the above range, it is possible to efficiently spread the chemical agent on the surface to be treated while keeping the amount of the chemical agent to be injected to a very small amount. If the injection amount of the aerosol valve is within the above range, a predetermined injection amount can be appropriately set.
- injection member is a member attached to the pressure container via the aerosol valve.
- the injection button is formed with a passage in the operation part through which the aerosol composition taken in from the pressure container passes through the stem hole of the aerosol valve, and a nozzle hole through which the aerosol composition is injected.
- the injection button may be a button type that is pressed from above, or may be a trigger type from the viewpoint of operability.
- the inner diameter of the injection hole of the injection button is preferably ⁇ 0.45 to 3.0 mm, more preferably ⁇ 0.5 to 2.0 mm, and ⁇ 0. 6 to 1.6 mm is more preferred.
- the injection button may have one or more injection holes having such an inner diameter.
- the aerosol pressure container is filled with the aerosol composition as described above, and the injection member is operated to inject a fixed amount of the aerosol composition in one operation.
- the ejection force of the aerosol composition at 25° C. at a position 20 cm away from the nozzle is preferably 1 to 60 gf, more preferably 5 to 40 gf.
- the injection force was measured at a room temperature of 25° C. from a distance of 20 cm from the nozzle of the metered injection type aerosol, and a digital force gauge (for example, manufactured by Imada Co., Ltd., model number: DS2-2N). It can be determined by measuring the maximum value when the aerosol composition is injected once toward the center of the flat plate.
- the aerosol composition ejected in the form of particles by injection adheres to the treated surface, aggregates while the solvent volatilizes, and precipitates the normal-temperature solid drug.
- a drug precipitate can be observed under the following conditions.
- the aerosol composition is sprayed toward the center of a vinyl chloride plate of 15 cm ⁇ 15 cm from a distance of 15 cm under conditions of about 15° C., and then air-dried for 1 hour.
- An arbitrary section is set at a position 2.5 to 10 cm from the center of the plate, and the state of the crystal in the section is photographed. Crystals are photographed using a digital microscope (for example, Digital Microscope VHX-900 manufactured by KEYENCE).
- the aerosol of the present invention preferably has an average particle diameter (D50) of 3 to 300 ⁇ m at an injection distance of 50 cm under conditions of about 25° C., from the viewpoint of the volatility of the injected particles.
- the average particle size of the aerosol composition can be measured with a laser beam diffraction particle size analyzer (for example, "LDSA-1400A” manufactured by Microtrack Bell Co., Ltd.). Also, the average particle size of the aerosol composition can be adjusted by adjusting the internal pressure, the nozzle hole diameter, and the like.
- the metered-volume aerosol of the present invention allows the drug to adhere uniformly over a wide area of the treatment surface.
- the particle size distribution of the chemical deposit should be within a narrow range, and the difference between the maximum and minimum particle sizes of the chemical deposit should be small. That is, it is characterized in that the sizes of the drug deposits are uniform, and that the drug deposits can be evenly adhered without unevenness or gaps.
- the chemical is an insect pest control component
- the probability of contact between the insect pests adhering to the treated surface and the pest control component can be increased, and the pest control effect is likely to be exhibited.
- An injection button having an injection hole diameter and the number of injection holes shown in Tables 1 and 2 was attached to an aerosol valve, and the injection amount per operation and the treatment amount of the pest control component were shown in Table 1.
- Examples 1 to 13 A metered injection type aerosol of Comparative Examples 2 and 3 was obtained.
- the drug solutions of Comparative Examples 1, 4, and 5 were dropped onto the center of one surface of a vinyl chloride plate measuring 15 cm long and 15 cm wide using a Pipetman (manufactured by Gilson).
- the amount of the chemical solution dropped was such that the chemical treatment amount on the plate surface was the same as in the corresponding example.
- the liquid was spread over the entire plate. After 1 hour at room temperature, the appearance of the drug deposit deposited on the surface of the vinyl chloride plate was observed using a microscope.
- a plastic cup (diameter 13 cm, height 10 cm) was placed upside down on the vinyl chloride plate, and 10 German cockroaches were released into the cup and brought into contact with the vinyl chloride plate for a predetermined time. After standing for a certain period of time, the test insects were transferred to a clean cup, and the knockdown rate after 3 hours and the mortality rate after 24 hours were measured.
- a vinyl chloride plate measuring 15 cm long and 15 cm wide was coated with petroleum jelly on its outer edge to prevent the escape of test insects, and was treated with a chemical agent by the following method.
- a chemical treatment method in the case of the metered injection aerosol of Examples 7, 10, 11 to 13 a plate placed at an angle of 45° was sprayed from a distance of 75 cm toward the center of the plate. was operated once (1 push) and air-dried for 1 hour.
- a trigger product number T-95 (manufactured by Canyon Co., Ltd.) was operated once with a hand pump to air-dry for 1 hour.
- Adjusted fatality rate (%) (lethal rate in drug-treated area - lethal rate in drug-untreated area) / (1-lethal rate in drug-untreated area) x 100
- Example 3 and Comparative Example 2 and between Example 8 and Comparative Example 4 even when the amount of pest control component treated is small, the knockdown rate and At least one of the lethality rates improved.
- Example 2 and Comparative Example 2 comparison between Examples 3 and 4 and Comparative Example 3, comparison between Example 5 and Comparative Example 1, comparison between Example 7 and Comparative Example 4
- the Example improved at least one of the knockdown rate and the lethality rate more than the Comparative Example.
- Example 11 In the case of Dermatophagoides farinae, a comparison between Example 11 and Comparative Example 6 shows that when the type of pest control component and the treatment amount per operation are the same, the corrected lethality rate is higher in the example than in the comparative example. In addition, from the comparison between Examples 11 to 13 and Comparative Example 6, the corrected fatality rate was improved in the Examples compared to the Comparative Examples, regardless of the treatment amount of the pest control component, the average particle size, and the jetting force. Furthermore, from the results of Examples 7, 10 and 11, the Examples showed high corrected lethality regardless of the type of pest control component.
- Example 1 (FIG. 1) and Example 2 (FIG. 2) with Comparative Example 2 (FIG. 12), Example 3 (FIG. 3) and Example 4 ( 4) and Comparative Example 3 (FIG. 13), Example 5 (FIG. 5) and Comparative Example 1 (FIG. 11), Example 7 (FIG. 7) and Comparative Example 4 (FIG. 14)
- Example 10 (FIG. 10) and Comparative Example 5 (FIG. 15)
- Comparative Example 5 (FIG. 15)
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Abstract
Description
一方、有効成分となる薬剤が常温固体状である場合、常温で揮散せず処理面で析出するため、付着時の状態が効果に直接影響する。
このように、常温固体状の薬剤を効果的に処理する手段には検討の余地があった。
(1)耐圧容器と、前記耐圧容器に充填されたエアゾール組成物とを有し、1回の噴射操作で一定量のエアゾール組成物を噴射する定量噴射型エアゾールであって、
前記エアゾール組成物が常温固体状薬剤と溶剤と噴射剤とを含み、
前記溶剤及び前記噴射剤からなる混合物の蒸発潜熱が10.00kcal/mol以下である、定量噴射型エアゾール。
(2)前記常温固体状薬剤が常温固体状害虫防除成分である、(1)に記載の定量噴射型エアゾール。
(3)前記溶剤が揮散性溶剤である、(1)または(2)に記載の定量噴射型エアゾール。
本発明の定量噴射型エアゾールは、耐圧容器と、前記耐圧容器に充填されたエアゾール組成物とを有する。
エアゾール組成物は、有効成分である常温固体状薬剤(以下「薬剤」とも記載する。)と溶剤と噴射剤とを含む。常温固体状とは、常温すなわち25℃付近において固体状であることを意味し、25℃における蒸気圧が25mPa以下であることが好ましい。常温固体状とは、例えば結晶性固体状、粉体固体状であること等が挙げられる。有効成分とは、定量噴射型エアゾールを使用した時に、何らかの作用を発揮するものを指す。有効成分である常温固体状薬剤としては、特に限定されないが、例えば、常温固体状の、害虫防除成分、芳香成分、消臭成分、除菌・殺菌成分等が挙げられる。
以下、各成分について説明する。
常温固体状害虫防除成分としては、具体的には、フタルスリン、エトフェンプロックス、ビフェントリン、フェンプロパトリン等のピレスロイド系化合物、プロポクスル等のカーバメート系化合物、トリクロルホン、ブロモホス、カルクロホス、ピリダフェンチオン、クロルピリホスメチル等の有機リン系化合物、メトキサジアゾン等のオキサジアゾール系化合物、ジノテフラン等のネオニコチノイド系化合物、ブロフラニリド等のメタジアミド系化合物、フィプロニル等のフェニルピラゾール系化合物、その他、ピリプロキシフェン、ジフルベンズロン、ヒドラメチルノン、アミドフルメト等が挙げられる。これらは、1種を単独で使用してもよく、2種以上を組み合わせて使用してもよい。
揮散性溶剤としては、具体的にはグリコールエーテル系溶剤、炭化水素系溶剤、アルコール系溶剤、芳香族系溶剤、エステル系溶剤等の有機溶剤や、水が挙げられる。揮散性溶剤は、常温で揮散性を有するものであれば特に限定されないが、25℃における蒸気圧が50Pa以上であることが好ましく、100Pa以上であることがより好ましく、1000Pa以上であることが特に好ましい。また界面活性剤を用いてもよい。
炭化水素系溶剤としては、例えば、パラフィン系炭化水素やナフテン系炭化水素等の脂肪族炭化水素及び脂環式炭化水素が挙げられ、JIS 1号灯油等の灯油が好ましい。具体的にはノルマルパラフィン、イソパラフィン等が挙げられる。ノルマルパラフィンとしては、炭素数が8~16のものが代表的で、例えば、三光化学工業株式会社製のネオチオゾール、ENEOS株式会社製のノルマルパラフィンMA等が挙げられる。イソパラフィンとしては、炭素数が8~16のものが代表的で、例えば、出光興産株式会社製のIPクリーンLX等が挙げられる。
アルコール系溶剤としては、例えば、エタノール、ノルマルプロパノール、イソプロパノール等の低級アルコール、エチレングリコール等の多価アルコール等が挙げられる。
芳香族系溶剤としては、例えば、トルエン、キシレン等が挙げられる。
エステル系溶剤としては、例えば、ミリスチン酸イソプロピル、ラウリン酸ヘキシル、パルミチン酸イソプロピル等が挙げられる。
これらの中でも、常温固体状薬剤の溶解性または分散性に優れる点から、アルコール系溶剤が好ましく、エタノール、ノルマルプロパノール、イソプロパノール等の低級アルコールがより好ましい。
上記溶剤は、1種を単独で使用してもよく、2種以上を組み合わせて使用してもよい。
噴射剤としては、例えば、プロパン、プロピレン、n-ブタン、イソブタン等の液化石油ガス(LPG)やジメチルエーテル(DME)等の液化ガス、炭酸ガス、窒素ガス、圧縮空気等の圧縮ガス、HFC-152a、HFC-134a、HFO-1234yf、HFO-1234ze等のハロゲン化炭素ガス等の1種又は2種以上を用いることができる。使用する噴射剤は、原液との相溶性やエアゾールバルブ等の容器部材に合わせて適宜選択すればよい。
なお、上記蒸発潜熱は0℃(273.15K)における数値である。
また、上記蒸発潜熱は、以下の式1~3によって算出できる。式1~3において、極性液体とは極性を持つ分子からなる液体を指し、例えばエタノールやイソプロパノール、ミリスチン酸イソプロピル、水、ジメチルエーテルなどが挙げられる。一方で、無極性液体とは極性を持たない分子からなる液体を指し、例えば、ノルマルパラフィンやイソパラフィン、プロパン、ブタン、エタンなどが挙げられる。
※式1:溶剤及び噴射剤からなる混合物の蒸発潜熱(kcal/mol)=溶剤の蒸発潜熱(kcal/mol)×溶剤のモル比率(mol%)+噴射剤の蒸発潜熱(kcal/mol)×噴射剤のモル比率(mol%)
※式2:溶剤または噴射剤が極性液体である場合
溶剤または噴射剤の蒸発潜熱(kcal/mol)=温度(K)×27.98×(溶剤または噴射剤の温度(K)における蒸気圧(mmHg)/温度(K))-0.105
※式3:溶剤または噴射剤が無極性液体である場合
溶剤または噴射剤の蒸発潜熱(kcal/mol)=温度(K)×23.61×(溶剤または噴射剤の温度(K)における蒸気圧(mmHg)/温度(K))-0.119
なお、上記式1~3において、ヒルデブランドの法則に基づき蒸気圧から蒸発潜熱を計算した。また、アントワン式またはカリンゲール・デーヴィス式に基づき蒸気圧を計算した。
蒸発潜熱は、溶剤および噴射剤の種類と量、及び配合比を変更することにより調整可能である。
本発明の定量噴射型エアゾールは、耐圧容器と、耐圧容器に充填された上記エアゾール組成物とを有する。耐圧容器はエアゾールバルブによりその開口を閉止される。
定量噴射型エアゾールとは、1回の噴射操作で一定量のエアゾール組成物を噴射するエアゾールである。定量噴射型エアゾールは、エアゾールバルブに取り付けられた噴射部材(以下、噴射ボタンともいう。)が使用者に操作されることにより、エアゾールバルブを通って耐圧容器内のエアゾール組成物の一定量が噴射され、原液は噴射剤によって粒子状とされ噴霧粒子として噴射される。
エアゾールバルブは、噴射部材が使用者に操作されることにより耐圧容器内と外部との連通および遮断を切り替えるための開閉部材と、開閉部材が取り付けられるハウジングと、ハウジングを耐圧容器の所定の位置に保持するためのマウント部材を備える。また、開閉部材は、噴射部材と連動して上下に摺動するステムを含む。ステムの摺動によりエアゾール組成物の連通(噴射状態)および遮断(非噴射状態)が切り替えられる。エアゾールバルブには、耐圧容器からエアゾール組成物を取り込むためのハウジング孔と、取り込まれたエアゾール組成物を噴射部材に送るためのステム孔とが形成されている。ハウジング孔からステム孔までの経路は、エアゾール組成物が通過する内部通路を構成する。
噴射部材(噴射ボタン)は、エアゾールバルブを介して耐圧容器に取り付けられる部材である。噴射ボタンには、エアゾールバルブのステム孔を介して耐圧容器から取り込まれるエアゾール組成物が通過する操作部内通路とエアゾール組成物が噴射される噴口が形成されている。なお、噴射ボタンは、上から押圧するボタンタイプでもよく、操作性の観点から、トリガータイプでもよい。
また、噴射ボタンは、かかる内径を有する噴口を1以上有していてもよい。
本発明のエアゾールは、上記したようにエアゾール用耐圧容器にエアゾール組成物が充填され、噴射部材を操作することにより、1回の操作によって一定量のエアゾール組成物が噴射される。
噴口から20cm離れた位置におけるエアゾール組成物の25℃における噴射力は、1~60gfであることが好ましく、5~40gfがより好ましい。噴射力が前記範囲であることで、噴射時間を所望の範囲とすることができる。
本発明において、噴射により粒子状に吐出されたエアゾール組成物は処理面に付着し、溶剤が揮散しながら凝集し、常温固体状薬剤が析出する。薬剤析出体は下記条件に基づき観察できる。
条件:15cm×15cmの塩化ビニル板の中央に向けて、15cmの距離からエアゾール組成物を約15℃の条件下で噴射し、その後1時間風乾させる。板の中央から2.5~10cmの位置において、任意の区画を設定し、区画内にある結晶の様子を撮影する。結晶の撮影は、デジタルマイクロスコープ(例えば、KEYENCE製デジタルマイクロスコープVHX-900)を用いて行う。
本発明のエアゾールはまた、噴射粒子の揮散性の観点から、約25℃の条件下での噴射距離50cmにおけるエアゾール組成物の平均粒子径(D50)が、3~300μmであることが好ましい。エアゾール組成物の平均粒子径はレーザー光回析式粒度測定装置(例えば、マイクロトラック・ベル株式会社製「LDSA-1400A」)により測定できる。また、エアゾール組成物の平均粒子径は内圧、噴口孔径などにより調整できる。
下記表1、2に示す各常温固体状害虫防除成分と溶剤を混合し、害虫防除成分濃度が下記表1、2に示す値となるように原液を調製した。
エアゾール用耐圧缶(容量220mL)に、下記表1、2に示す量の各原液を充填し、1操作当たりの噴射量が表1、2に示す量のエアゾールバルブでエアゾール用耐圧缶を閉止した。続いて、下記表1、2に示す量の噴射剤を加圧充填した。
エアゾールバルブに、表1、2に示す噴口孔径と噴口数を備えた噴射ボタンを取り付け、1操作当たりの噴射量および害虫防除成分の処理量が表1に示す量の、実施例1~13、比較例2、3の各定量噴射型エアゾールを得た。
下記表2に示す常温固体状害虫防除成分と溶剤を混合し、害虫防除成分濃度が下記表2に示す値となるように薬剤溶液を調製した。
下記表2に示す常温固体状害虫防除成分と溶剤を混合し、害虫防除成分濃度が下記表2に示す値となるように薬剤溶液を調製し、ハンドポンプ組成物を製造した。ポリプロピレン製ハンドポンプ用容器(容量400mL)に下記表2に示す原液を充填し、1操作当たりの噴射量が表2に示す量のハンドポンプ用トリガーで閉止した。
約25℃の条件下で、噴射距離50cmにおけるエアゾール組成物及びハンドポンプ組成物の平均粒子径を、マイクロトラック・ベル株式会社製「LDSA-1400A」を用いて測定した。
実施例1~10、比較例2、3で製造した各定量噴射型エアゾールについて薬剤析出体の観察を行った。定量噴射型エアゾールの噴口から噴射方向(水平方向)に直線で15cm離れた位置に設置した、縦15cm、横15cmの塩化ビニル板の中央に向けて、噴射ボタンを1回操作して下記表1、2に示す噴射量のエアゾール組成物を約15℃の条件下にて噴射した。1時間経過後、塩化ビニル板表面に析出した薬剤析出体の様子をマイクロスコープを用いて観察した。
縦15cm、横15cmの塩化ビニル板に、下記方法により薬剤を処理した。
実施例及び比較例の定量噴射型エアゾールの場合の薬剤処理方法としては、15cmの距離から板の中央部に向けて、定量噴射型エアゾールを1回操作(1プッシュ)し1時間風乾させた。
比較例の薬剤溶液の場合の薬剤処理方法としては、薬剤溶液0.3mLを、板の一方の表面中央部にピペットマン(ギルソン社製)を用いて滴下した。滴下直後に板を傾けることで板全体に液を広げ、1時間風乾させた。
次に、塩化ビニル板の上にプラスチックカップ(直径13cm、高さ10cm)を逆さに置き、その中にチャバネゴキブリ10頭を放虫して、所定時間塩化ビニル板と接触させた。
一定時間静置した後、清潔なカップに供試虫を移し、3時間後のノックダウン率および24時間後の致死率を計測した。
チャバネゴキブリ10頭に替えてクロゴキブリ10頭を用いたこと以外は、チャバネゴキブリに対する殺虫効力確認試験と同様に試験を行った。
チャバネゴキブリ10頭に替えてトコジラミ5頭を用いたこと、プラスチックカップに替えてガラス瓶(直径6cm、高さ9cm)を用いたこと以外は、チャバネゴキブリに対する殺虫効力確認試験と同様に試験を行った。
縦15cm、横15cmの塩化ビニル板の外縁に、供試虫の逃亡防止のためワセリンを塗布したものを用意し、下記方法により薬剤を処理した。
実施例7、10、11~13の定量噴射型エアゾールの場合の薬剤処理方法としては、45°の角度で設置した板に対し、75cmの距離から板の中央部に向けて、定量噴射型エアゾールを1回操作(1プッシュ)し1時間風乾させた。
比較例6の場合の薬剤処理方法としては、45°の角度で設置した板に対し、75cmの距離から板の中央部に向けて、1操作当たりの噴射量が1.0mLであるトリガー(品番T-95、キャニヨン株式会社製)を取り付けたハンドポンプを1回操作し、1時間風乾させた。
次に、塩化ビニル板の中央にヤケヒョウヒダニ30~300頭を供試し、一晩塩化ビニル板と接触させた。
また、薬剤を処理しない塩化ビニル板を用いて同じ操作を行った。
一晩経過後、供試したヤケヒョウヒダニ全頭を回収した。実体顕微鏡(オリンパス株式会社製)を用いて回収したヤケヒョウヒダニ全頭を観察し、生存頭数と致死頭数を計数し、薬剤処理区における致死率を算出した。また、薬剤を処理しない塩化ビニル板を用いて同じ操作を行い、薬剤無処理区における致死率を算出し、下記の式から補正致死率(%)を算出した。
補正致死率(%)
=(薬剤処理区の致死率-薬剤無処理区の致死率)/(1-薬剤無処理区の致死率)×100
また、マイクロスコープによる薬剤析出体の状態を示す写真を図1~15に示す。
IPA:イソプロパノール
DME:ジメチルエーテル
LPG0.20MPa:液化石油ガス
エアゾール組成物の蒸発潜熱:上述の式1~3に基づき算出した。
クロゴキブリに対しては、実施例2と比較例2との対比から、害虫防除成分の種類と1操作当たりの処理量が同一の場合、比較例よりも実施例の方がノックダウン率及び致死率の少なくとも一方が向上した。また、実施例3と比較例2との対比、実施例8と比較例4との対比から、害虫防除成分の処理量が少ない場合でも、比較例よりも実施例の方が、ノックダウン率及び致死率の少なくとも一方が向上した。
トコジラミに対しては、実施例2と比較例2との対比、実施例3、4と比較例3との対比、実施例5と比較例1との対比、実施例7と比較例4との対比から、害虫防除成分の種類と1操作当たりの処理量が同一の場合、比較例よりも実施例の方が、ノックダウン率及び致死率の少なくとも一方が向上した。また、実施例8と比較例4との対比から、害虫防除成分の処理量が少ない場合でも、比較例よりも実施例の方が、ノックダウン率及び致死率の少なくとも一方が向上した。
ヤケヒョウヒダニの場合、実施例11と比較例6との対比から、害虫防除成分の種類と1操作当たりの処理量が同一の場合、比較例よりも実施例の方が、補正致死率が向上した。また、実施例11~13と比較例6との対比から、害虫防除成分の処理量や平均粒子径、噴射力によらず、比較例よりも実施例の方が、補正致死率が向上した。さらに、実施例7、10と実施例11の結果から、害虫防除成分の種類によらず、実施例は高い補正致死率を示した。
したがって、混合物の蒸発潜熱が特定の範囲である定量噴射型エアゾールとすることで、種々の害虫に対して、害虫防除成分である常温固体状薬剤の効力を高めることができたことが分かる。
これらのことから、溶剤及び噴射剤からなる混合物の蒸発潜熱が特定の範囲である定量噴射型エアゾールとすることで、薬剤結晶が、均一な大きさで、偏りや隙間がなく、均等に、板表面全体を覆う状態で、板表面に付着するため、種々の害虫に対して、害虫防除成分である常温固体状薬剤の効力を高めることができたと推察される。
Claims (3)
- 耐圧容器と、前記耐圧容器に充填されたエアゾール組成物とを有し、1回の噴射操作で一定量のエアゾール組成物を噴射する定量噴射型エアゾールであって、
前記エアゾール組成物が常温固体状薬剤と溶剤と噴射剤とを含み、
前記溶剤及び前記噴射剤からなる混合物の蒸発潜熱が10.00kcal/mol以下である、定量噴射型エアゾール。 - 前記常温固体状薬剤が常温固体状害虫防除成分である、請求項1に記載の定量噴射型エアゾール。
- 前記溶剤が揮散性溶剤である、請求項1または2に記載の定量噴射型エアゾール。
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