Total spray aerosol

Abstract

To provide a full ejection type aerosol agent of which attachment amount of an effective component to a ceiling surface or a wall surface is improved, when a full ejection type aerosol agent is used in a limited space such as a chamber or the like.SOLUTION: An aerosol composition comprising a powdery substance and a raw liquid containing an effective component and an injection agent is filled in a pressure proof container, and an ejection amount per 1 m3 of the aerosol composition is in a range of 0.001 to 1 g / sec.SELECTED DRAWING: None

Description

[Technical field]

[0001] The present invention relates to a total-amount-spray type aerosol preparation, and more particularly to a total-amount-spray type aerosol preparation in which almost the entire amount of the contents of the aerosol preparation is sprayed into a limited space in a short period of time. [Background technology]

[0002] Aerosols are made by dissolving the active ingredients of insecticides, deodorants, etc. in a small amount of solvent and filling the resulting solution (aerosol concentrate) and propellant into a pressure-resistant container equipped with an injection device. Aerosols are convenient to use because they have the advantages of being easier to handle than other forms of insecticides, such as powders, emulsions, oils, and smoke products, and do not cause any dirt in the surrounding area.

[0003] Among such aerosol agents, total-volume-spray aerosol agents have been developed that are placed on the floor and the entire contents are sprayed out in a short period of time for the purpose of exterminating pests or deodorizing and creating fragrance in a limited space such as a room. Total-volume-spray aerosol agents have the advantage that they can be easily operated to distribute the active ingredient almost uniformly throughout an enclosed space in a short period of time.

[0004] As such total-spray aerosol agents, for example, a total-spray aerosol agent containing an aerosol concentrate containing A) an active ingredient, B) a high-boiling point solvent having a boiling point of 200°C or higher, C) a lower alcohol having 2 or 3 carbon atoms, and a propellant, in which the volume ratio of B / C is 1 / 10 to 1 / 1 and the average particle size of the sprayed particles is 30 μm or less (see Patent Document 1); a total-spray aerosol product in which contents are filled in a container, the contents containing an inorganic chemical (A) having a transition metal, a solvent (B) having a boiling point of 70 to 200°C, and a propellant (C) containing dimethyl ether, and the mass ratio (B / C) of the solvent (B) to the propellant (C) is 0.1 to 1.0 (see Patent Document 2); and the like have been proposed. [Prior art documents] [Patent documents]

[0005] [Patent Document 1] JP 2002-226301 A [Patent Document 2] JP 2014-227369 A Summary of the Invention [Problem to be solved by the invention]

[0006] However, conventional total-amount aerosols tended to adhere less active ingredient to ceilings and walls compared to floors, and therefore it was necessary to increase the amount of active ingredient in the aerosol concentrate in order to improve the effectiveness of the active ingredient on ceilings and walls.

[0007] Therefore, an object of the present invention is to provide a total-volume-spray aerosol agent that can improve the amount of active ingredient adhered to a ceiling or wall surface when the total-volume-spray aerosol agent is used in a limited space such as a room. [Means for solving the problem]

[0008] As a result of extensive research into the above-mentioned problems, the inventors discovered that the above-mentioned problems could be solved by incorporating a powdery substance into an aerosol concentrate and making it into a total-volume spray-type aerosol that is sprayed at a specific spray volume, thereby completing the present invention.

[0009] That is, the present invention is characterized by the following (1) and (2). (1) An aerosol composition comprising a powdery substance, a concentrate containing an active ingredient, and a propellant is filled in a pressure-resistant container, and 1 m of the aerosol composition is 3 A total-amount-spray type aerosol preparation, characterized in that the amount of spray per unit time is in the range of 0.001 to 1 g / sec. (2) From a total-aerosol formulation in which an aerosol composition consisting of a powdery substance, a concentrate containing an active ingredient, and a propellant is filled in a pressure-resistant container, the aerosol composition is dispensed over 1 m 3 The present invention relates to a method for spraying a total-amount-injection type aerosol agent, the method being characterized in that the agent is sprayed in the range of 0.001 to 1 g / sec per unit time. Effect of the Invention

[0010] According to the total-volume-spray aerosol agent of the present invention, the adhesion of the powdery substance to the treatment surface in the space to be treated is improved, so that when the total-volume-spray aerosol agent is sprayed in an enclosed space such as a room, the amount of active ingredient held in the powdery substance that adheres to the ceiling or wall surfaces can be improved, and the durability of the effect of the active ingredient can also be improved. [Brief description of the drawings]

[0011] [Figure 1] FIG. 13 is a diagram for explaining a test method for an injection test. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS

[0012] The total-amount spray type aerosol agent of the present invention is an aerosol composition comprising a concentrate and a propellant, which is filled in a pressure-resistant container equipped with a spray device, and 1 m of the aerosol composition is sprayed. 3 The amount of spray per second is in the range of 0.001 to 1 g / sec.

[0013] (undiluted) The concentrate contains a powdered substance and an active ingredient. It is preferable that the powdery substance is capable of retaining the active ingredient on its surface and inside, and when the aerosol composition, which is the content of the total-spray type aerosol agent, is sprayed in its entirety, the powdery substance retaining the active ingredient adheres to the treatment surface in the treatment space, and the effect of the active ingredient is exerted on the treatment surface.

[0014] The powdery substance preferably has an oil absorption of 35 mL / 100 g or more. The inventors' studies have also found that when a total-spray aerosol agent is used in a space such as a room, the residue effect of the powdery substance on the ceiling or wall surface varies depending on the oil absorption of the powdery substance blended in the concentrate. A total-spray aerosol agent containing a powdery substance with an oil absorption of 35 mL / 100 g or more leaves a large amount of powdery substance residue on the ceiling or wall surface, and therefore the amount of the active ingredient held by the powdery substance adhering to the ceiling or wall surface can be improved.

[0015] The oil absorption of the powdery substance is more preferably 100 mL / 100 g or more, and even more preferably 200 mL / 100 g or more. The upper limit of the oil absorption is not particularly limited, but from the viewpoint of the diffusibility during spraying, it is preferably 500 mL / 100 g or less, more preferably 400 mL / 100 g or less, and even more preferably 350 mL / 100 g or less. The oil absorption of the powdery substance can be measured, for example, by a method in accordance with JIS K5101, ASTM D2414, ISO4656, etc.

[0016] The specific surface area of ​​the powdered material is 50 to 500 m 2 / g, and 100 to 400m 2 / g is more preferable, and 150 to 350m 2 / g. It is more preferable that the specific surface area of ​​the powdery substance is 50 m 2 / g or more, the active ingredient can be sufficiently retained, and the effect of the present invention can be exerted. 2 When the specific surface area is less than 1 / g, the active ingredient is not retained too much. The specific surface area of ​​the powdery substance can be measured, for example, by the BET method, a method in accordance with ISO 5794-1, or the like.

[0017] The average particle size of the powdery substance is preferably 1 to 25 μm, more preferably 1.5 to 20 μm, and even more preferably 2 to 15 μm. If the average particle size of the powdery substance is 1 μm or more, the active ingredient can be sufficiently retained, and if the average particle size is too large, it is likely to fall from the ceiling or wall surface, so it is preferably 25 μm or less. The average particle size of the powdery substance is the volume average particle size, and can be measured, for example, by ISO 13320, the Coulter counter method (Coulter multisizer method), etc.

[0018] Examples of the powdery substance include inorganic compounds and organic compounds. Examples of the inorganic compounds include metal oxides such as silicon dioxide (silica), calcium silicate, magnesium silicate, and alumina. Examples of the organic compounds include polyethylene resins, polystyrene resins, and silicone resins. These may be used alone or in combination of two or more. Among these, from the viewpoint of dispersibility in the aerosol composition, inorganic compounds are preferred, and it is more preferred to use at least one selected from the group consisting of silicon dioxide, calcium silicate, and magnesium silicate.

[0019] A specific example of the powdery substance is a powdery substance having an oil absorption of 35 mL / 100 g or more, such as the commercially available product "Sunsphere NP-200" (product name, manufactured by AGC Si-Tech Co., Ltd., oil absorption of 40 mL / 100 g, specific surface area of ​​100 m 2 / g, average particle size 20μm), "Tokusil NP" (trade name, manufactured by Oriental Silicas Corporation, oil absorption 270mL / 100g, specific surface area 190m) 2 / g, average particle size 10.3 μm), "Adsolider 101" (product name, manufactured by Freund Corporation, oil absorption capacity 310 mL / 100 g, specific surface area 300 m 2 / g, average particle size 3.2 μm.

[0020] The powdery substance is preferably contained in the concentrate at a ratio of 0.01 to 15 weight / volume % (hereinafter referred to as "w / v%"), more preferably 0.05 to 10 w / v%, and even more preferably 0.1 to 5 w / v%. If the content of the powdery substance in the concentrate is 0.01 w / v% or more, the active ingredient that is not retained in the powdery substance and remains can be eliminated, and if it is 15 w / v% or less, there will be no spray trouble such as the powdery substance clogging the nozzle of the aerosol agent and making it impossible to spray the entire amount.

[0021] The content of the powdery substance in the aerosol composition is preferably in the range of 0.001 to 7.5 w / v%, more preferably 0.005 to 6 w / v%, and even more preferably 0.01 to 5 w / v%. When the content of the powdery substance in the aerosol composition is 0.001 w / v% or more, the adhesion of the active ingredient to the treated surface can be improved, and when it is 7.5 w / v% or less, the powdery substance does not cause caking in the aerosol product and can be easily redispersed when used.

[0022] The active ingredient is a substance that exerts some kind of effect when a total-discharge aerosol agent is used. Examples of active ingredients include, but are not limited to, pest control ingredients, fragrance ingredients, deodorizing ingredients, disinfecting and sterilizing ingredients, etc.

[0023] The type of pest control component is not particularly limited, and any known compound can be used. Examples of pest control components include pyrethroid compounds such as permethrin, pyrethrin, allethrin, phthalthrin, resmethrin, furamethrin, fenothrin, empenthrin, prallethrin, cyphenothrin, cyfluthrin, imiprothrin, transfluthrin, metofluthrin, dimefluthrin, mepafluthrin, profluthrin, and momfluorothrin; fenitrothion, dichlorvos, chlorpyrifos-methyl, diazinon, and fenthi. organic phosphorus compounds such as carbaryl and propoxur; carbamate compounds such as methoprene, pyriproxyfen, methoxadiazone, fipronil, amidoflumet, and broflanilide; peppermint oil, orange oil, fennel oil, cinnamon oil, clove oil, turpentine oil, eucalyptus oil, Japanese cypress oil, jasmine oil, neroli oil, peppermint oil, bergamot oil, butiglen oil, lemon oil, lemongrass oil, cinnamon oil, citronella oil, and geranium Oil, citral, l-menthol, citronellyl acetate, cinnamic aldehyde, terpineol, nonyl alcohol, cis-jasmone, limonene, linalool, 1,8-cineole, geraniol, α-pinene, p-menthane-3,8-diol, eugenol, menthyl acetate, thymol, benzyl benzoate, benzyl salicylate, and other essential oil components; glycol ethers such as 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, diethylene glycol dibutyl ether, diethylene glycol dimethyl ether, and triethylene glycol dimethyl ether; dibasic acid esters such as dibutyl adipate, etc. These may be used alone or in combination of two or more.

[0024] The pest control component may be appropriately selected according to the type of target pest, such as mosquitoes, flies, moths, bees, stink bugs, bedbugs, cockroaches, ants, spiders, pillbugs, mites, ticks, lice, centipedes, caterpillars, millipedes, spiders, horseflies, blackflies, moths, termites, midges, leafhoppers, wood beetles, ground beetles, earwigs, silverfish, longhorn beetles, dermestid beetles, booklice, burrs, and rice moths. For flying pests such as mosquitoes, flies, moths, bees, horseflies, blackflies, midges, leafhoppers, moths, burrs, and rice moths, transfluthrin, metofluthrin, profluthrin, phthalthrin, prallethrin, momfluorothrin, methoxadiazone, broflanilide, etc. are suitable. For crawling pests such as cockroaches, stink bugs, bedbugs, ants, spiders, pillbugs, mites, lice, centipedes, caterpillars, millipedes, spiders, termites, wood beetles, ground beetles, earwigs, and silverfish, cyphenothrin, cyfluthrin, fenothrin, phthalthrin, prallethrin, imiprothrin, permethrin, propoxur, methoxadiazone, amidoflumet, broflanilide, etc. are suitable.

[0025] Examples of the aromatic components include, in addition to the essential oil components described above, anise oil, lavender oil, rose oil, rosemary oil, grapefruit oil, camphene, p-cymene, citronellol, nerol, benzyl alcohol, n-butyraldehyde, isobutyraldehyde, coumarin, cineol, etc. These may be used alone or in combination of two or more.

[0026] Examples of deodorizing components include components that adsorb odorous components such as green tea extract, persimmon tannin, lauric acid methacrylate, methyl benzoate, methyl phenylacetate, geranyl crotolate, acetophenone myristate, benzyl acetate, benzyl propionate, and silver, and components that mask odorous components such as the above-mentioned aromatic components. These may be used alone or in combination of two or more.

[0027] Examples of disinfecting and sterilizing components include environmental disinfectants such as thiabendazole, 4-isopropyl-3-methylphenol (IPMP), 3-iodo-2-propynyl butylcarbamate (IPBC), and p-chlorophenyl-3-iodopropargyl formal (IF-1000); agricultural disinfectants such as isophthalonitrile, procymidone, bayleton, and morestan; and silver compounds such as silver alone, silver oxide, inorganic silver salts (e.g., silver chloride, silver nitrate, silver sulfate, silver carbonate, silver sulfonate, etc.), and organic silver salts (e.g., silver formate, silver acetate, etc.). These may be used alone or in combination of two or more.

[0028] The active ingredients may be used in combination with ingredients having different effects, for example, a pest control ingredient may be used in combination with a fragrance ingredient, or a fragrance ingredient may be used in combination with a deodorizing ingredient other than a fragrance ingredient.

[0029] The content of the active ingredient may be appropriately adjusted depending on the type of active ingredient, the purpose, the size of the application space, the use environment, etc., and specifically, in the undiluted solution, it is preferably 0.01 to 30 w / v%, more preferably 0.1 to 25 w / v%, and even more preferably 0.5 to 20 w / v%. If the content of the active ingredient in the undiluted solution is 0.01 w / v% or more, a sufficient effect of the active ingredient can be obtained, and if it is 30 w / v% or less, production suitability is improved.

[0030] The content of the active ingredient in the aerosol composition may be appropriately adjusted depending on the type of active ingredient, the purpose, the size of the application space, the use environment, etc., and specifically, the range of 0.001 to 15 w / v% is preferable, 0.005 to 12.5 w / v% is more preferable, and 0.01 to 10 w / v% is even more preferable. If the content of the active ingredient in the aerosol composition is 0.001 w / v% or more, a sufficient effect of the active ingredient can be obtained, and if it is 15 w / v% or less, production suitability is improved.

[0031] The concentrate may contain a solvent for the purpose of improving the viscosity of the concentrate, suitability for production, exerting the effect of the active ingredient (for example, when the active ingredient is a pest control agent, increasing the penetration of the agent into pests), etc. Examples of such solvents include organic solvents such as glycol ethers, hydrocarbon solvents, alcohol solvents, aromatic solvents, and ester solvents, as well as water.

[0032] Examples of the hydrocarbon solvent include aliphatic hydrocarbons and alicyclic hydrocarbons such as paraffinic hydrocarbons and naphthenic hydrocarbons, and specifically include normal paraffin, isoparaffin, etc. Normal paraffin is preferably one having a carbon number of 8 to 16, and examples thereof include Neothiosol manufactured by Chuo Kasei Co., Ltd. and normal paraffin MA manufactured by JXTG Nippon Oil & Energy Corporation. Isoparaffin is preferably one having a carbon number of 8 to 16, and examples thereof include IP Clean LX and Supersol FP25 manufactured by Idemitsu Kosan Co., Ltd. Examples of the alcohol-based solvent include lower alcohols such as ethanol and propanol (normal and iso), and polyhydric alcohols such as glycerin and ethylene glycol. Examples of aromatic solvents include toluene and xylene. Examples of ester-based solvents include isopropyl myristate, hexyl laurate, and isopropyl palmitate. Examples of water include tap water, distilled water, purified water, and ion-exchanged water.

[0033] The content of the solvent varies depending on the specific gravity of the solvent, but is preferably in the range of 50 to 99.98 w / v% in the original solution, more preferably 60 to 99.9 w / v%, and even more preferably 70 to 99.5 w / v%. If the content of the solvent is 50 w / v% or more, the productivity can be improved, and if it is 99.98 w / v% or less, the effect of the active ingredient can be sufficiently obtained.

[0034] The concentrate is obtained by dissolving / dispersing a powdery substance and an active ingredient in, for example, a solvent. The active ingredient is supported by the powdery substance in the concentrate, and when sprayed with a propellant, the active ingredient is sprayed in a state supported by the powdery substance, and the powdery substance supporting the active ingredient adheres to the treatment surface.

[0035] The method for making the powder substance support the active ingredient is not particularly limited. For example, there may be mentioned a method in which the liquid active ingredient is dropped or sprayed onto the powder substance to bring them into contact with each other, or the powder substance is immersed in the liquid active ingredient to bring them into contact with each other, and the powder substance is supported with the active ingredient, and then the resultant is added to a solvent, or a method in which the powder substance and the active ingredient are added separately to a solvent, and the powder substance is supported with the active ingredient in the original solution by stirring as necessary, etc.

[0036] The concentrate may contain other ingredients, such as preservatives, pH adjusters, UV absorbers, surfactants, dissolution aids, etc., within the scope of not impairing the effects of the present invention. The content of these ingredients may be appropriately adjusted.

[0037] The content of the concentrate in the aerosol composition can be appropriately changed depending on the purpose of use of the total-spray type aerosol agent and the combination with the propellant, and is not particularly limited, but can be, for example, 1 to 50% by volume in the aerosol composition. When the concentrate is 1% by volume or more in the aerosol composition, a sufficient effect of the active ingredient can be obtained, and when it is 50% by volume or less, the concentrate can be sprayed as spray particles, so that when used indoors, for example, the contamination of furniture, floors, walls, etc. by the concentrate can be reduced. The content of the concentrate in the aerosol composition is more preferably 5% by volume or more at the lower limit, more preferably 10% by volume or more, and more preferably 40% by volume or less at the upper limit, more preferably 35% by volume or less.

[0038] (Propellant) The propellant is a medium for spraying the concentrate, and is filled under pressure together with the concentrate into a pressure-resistant container. As the propellant, for example, one or more of liquefied gases such as liquefied petroleum gases (LPG) such as propane, propylene, n-butane, isobutane, etc., dimethyl ether (DME), etc., compressed gases such as carbon dioxide gas, nitrogen gas, compressed air, etc., halogenated carbon gases such as HFC-152a, HFC-134a, HFO-1234yf, HFO-1234ze, etc. can be used. The propellant to be used may be appropriately selected according to the compatibility with the concentrate and the container components such as an aerosol valve.

[0039] The content of the propellant in the aerosol composition can be appropriately changed depending on the purpose of use of the total-spray type aerosol agent and the combination with the concentrate, and is not particularly limited, but can be, for example, 50 to 99% by volume in the aerosol composition. When the propellant is 50% by volume or more in the aerosol composition, the concentrate can be sprayed as spray particles, so that the active ingredient is more easily diffused and the effect of the active ingredient is more likely to be sustained. When the propellant is 99% by volume or less, the effect of the active ingredient can be sufficiently obtained. The content of the propellant in the aerosol composition is more preferably 60% by volume or more at the lower limit, more preferably 65% ​​by volume or more, and more preferably 95% by volume or less at the upper limit, more preferably 90% by volume or less.

[0040] The volume ratio of the concentrate to the propellant in the aerosol composition is preferably 1:99 to 50:50, more preferably 3:97 to 40:60, and even more preferably 5:95 to 30:70. By setting the volume ratio in this range, the effect of the active ingredient can be sufficiently obtained.

[0041] (Total volume spray aerosol) The total-amount-spraying aerosol agent of the present invention is constructed by filling the concentrate and propellant described above into a pressure-resistant container for aerosols, and closing the opening of the pressure-resistant container with an aerosol valve. The total-amount-spraying aerosol agent is configured such that, when a user operates a spray member (hereinafter also referred to as a spray button) attached to the aerosol valve once, the entire amount of the aerosol composition (concentrate and propellant) in the pressure-resistant container is pushed out of the pressure-resistant container through the aerosol valve, at which point the aerosol composition is sprayed in particulate form.

[0042] (Aerosol valve) The aerosol valve comprises an opening / closing member for switching between communication and cut-off between the inside and outside of the pressure-resistant container by the user operating the ejection member, a housing to which the opening / closing member is attached, and a mounting member for holding the housing at a predetermined position on the pressure-resistant container. The opening / closing member also includes a stem that slides up and down in conjunction with the ejection member. The sliding of the stem switches between communication (ejection state) and cut-off (non-ejection state) of the aerosol composition. The housing is formed with a housing hole for taking in the aerosol composition from the pressure-resistant container. The stem is formed with a stem hole for sending the aerosol composition taken in the housing to the ejection member. The path from the housing hole to the stem hole constitutes an internal passage through which the aerosol composition passes.

[0043] The shape of the stem hole of the stem may be circular or polygonal. When the stem hole is circular, the size of the stem hole is preferably 0.1 to 4.5 mm in diameter, more preferably 0.3 to 4.2 mm in diameter, and even more preferably 0.6 to 4 mm in diameter. When the stem hole is polygonal, the size of the stem hole may be the same as that of a circular stem hole. When the undertap hole of the stem is circular, it is preferable that the diameter of the undertap hole is 0.5 to 3 mm, more preferably 0.7 to 2.5 mm, and even more preferably 1 to 2.2 mm. The shape of the undertap hole may be circular or polygonal, and if it is polygonal, the size of the undertap hole may be the same as that of a circle. The stem may or may not have a vapor tap hole, but if it does have a vapor tap hole, the size of the hole is preferably 0.1 to 3 mm in diameter, more preferably 0.2 to 2.5 mm in diameter, and even more preferably 0.3 to 2.2 mm in diameter, if circular. The shape of the vapor tap hole may be circular or polygonal, and if polygonal, the size of the vapor tap hole may be the same as that of the circular one. The number of stem holes and vapor tap holes may be one or more. When there are multiple stem holes and vapor tap holes, the size of the stem hole and vapor tap hole is the total size of the multiple stem holes and vapor tap holes.

[0044] (Injection member) The spray member (spray button) is a member attached to the pressure-resistant container via the aerosol valve. The spray button is formed with a passage in the operating part through which the aerosol composition taken in from the pressure-resistant container via the stem hole of the aerosol valve passes, and with a nozzle through which the aerosol composition is sprayed. When pressure is applied to the spray button of the spray member used for a total spray type aerosol agent, the spray button is fixed in a position pressing down on the stem of the aerosol valve, and the aerosol composition passes through the pressed-down stem and is sprayed continuously (total spray) from the nozzle of the spray button.

[0045] The shape of the nozzle of the injection button may be circular or polygonal. When the nozzle is circular, its inner diameter (diameter of the nozzle hole) may be adjusted appropriately according to the design of the injection amount and injection time, and is preferably 0.1 to 2 mm in diameter, more preferably 0.3 to 1.5 mm in diameter, and even more preferably 0.6 to 1.2 mm in diameter. When the nozzle is polygonal in shape, the size of the nozzle may be the same as that of a circle. In addition, there is no problem in having multiple nozzles with the same area as these.

[0046] (Aerosol internal pressure) The internal pressure of the total-amount-spraying aerosol at 25°C is preferably 0.2 to 0.8 MPa. When the internal pressure is 0.2 MPa or more, the aerosol composition can be sprayed in its entirety while ensuring the diffusibility of the powdery substance in the space of use. When the internal pressure is 0.8 MPa or less, the aerosol composition can be prevented from being sprayed too forcefully, causing the powdery substance to hit the ceiling constituting the space of use and fall without adhering. The internal pressure of the total-amount-spraying aerosol is more preferably 0.25 to 0.6 MPa, and even more preferably 0.3 to 0.5 MPa.

[0047] (Injection pressure) The spray pressure of the total-amount spray aerosol agent is preferably 1 to 15 gf, more preferably 3 to 10 gf, as measured at a position 20 cm away from the nozzle. By having the spray pressure within the above range, the aerosol composition can be sprayed up to the ceiling surface when used in a space inside a general building. The spray pressure can be measured by placing a circular plate with a diameter of 60 mm attached to a digital force gauge (e.g., Imada Co., Ltd., model number: DS2-2N) at a vertical distance of 20 cm from the nozzle of the total-spray aerosol agent, spraying the aerosol composition toward the center of the plate at room temperature of 25°C, and calculating the average of the maximum value as the spray load.

[0048] (Injection amount) The total amount spray type aerosol agent of the present invention is a total amount spray type aerosol agent. 3 The amount of spray per 1 m of the aerosol composition is in the range of 0.001 to 1 g / sec. 3 When the amount of spray per unit area is 0.001 g / sec or more, the force of the spray is sufficient to disperse the aerosol composition throughout the entire space of use, and when the amount of spray per unit area is 1 g / sec or less, the safety of the aerosol composition can be ensured. 3 The amount of spray per second is preferably 0.005 to 0.7 g / sec, and more preferably 0.01 to 0.5 g / sec.

[0049] (injection time) The spray time until the entire amount of the total-amount-spraying aerosol agent of the present invention is sprayed is preferably 5 to 150 seconds. If the spray time is 5 seconds or more, the active ingredient can be sprayed throughout the entire space in which it is used, and if it is 150 seconds or less, the amount of the aerosol agent sprayed per unit time can be increased, so that the scattering of the aerosol composition in the space in which it is used can be improved, and thus the amount of the active ingredient attached to the ceiling surface or wall surface can be increased. The spray time is more preferably 7 to 120 seconds, and even more preferably 10 to 100 seconds.

[0050] Methods for adjusting the spray amount and spray time include, for example, adjusting the size of the nozzle of the spray button, adjusting the spray pressure of a total-spray type aerosol agent, adjusting the stem hole diameter of the aerosol valve, adjusting the pressure of the propellant, and combinations of these.

[0051] In the present invention, the total-amount-spraying aerosol agent of the present invention is used, and an aerosol composition is sprayed from the total-amount-spraying aerosol agent to a volume of 1 m. 3 The aerosol composition is sprayed in the range of 0.001 to 1 g / sec per unit time. By spraying the aerosol composition in an amount within the above range, it is possible to improve the adhesion of the powdery substance to the treatment surface in the space to be treated, and when a total-amount spray type aerosol agent is sprayed in an enclosed space such as a room, it is possible to improve the amount of the active ingredient held in the powdery substance that adheres to the ceiling or wall surface, and therefore it is possible to improve the duration of the effect of the active ingredient. 1m 3 The amount of spray per second is preferably 0.005 to 0.7 g / sec, and more preferably 0.01 to 0.5 g / sec.

[0052] In the present invention, a total-amount-spray type aerosol agent in which a concentrate and a propellant are filled in a pressure-resistant container contains a powdery substance in the concentrate, and 1 m of the aerosol composition is added to the concentrate. 3 The present invention also provides a method for enhancing the effectiveness of a total-amount-spray type aerosol agent by setting the amount of spray per second in the range of 0.001 to 1 g / sec. As described above, when the powdery substance is contained in a total-amount-spraying aerosol agent, the amount of residue on the ceiling and wall surfaces of a room, etc. increases. Therefore, by containing the powdery substance in a concentrate and spraying it so that the spray amount falls within the above range, the active ingredient held in the powdery substance also remains on the ceiling and wall surfaces, improving the amount of adhesion of the active ingredient on the treated surface. Therefore, the effectiveness of the total-amount-spraying aerosol agent can be enhanced. EXAMPLES

[0053] The present invention will be further explained by the following test examples, but the present invention is not limited to the following test examples in any way.

[0054] The powder substances used in the following test examples are as shown in Table 1.

[0055] [Table 1]

[0056] (Test Example 1) 1. Preparation of Stock Solutions According to the formulation shown in Table 2, the active ingredient and / or powdery substance was measured out, and absolute ethanol (specific gravity 0.797 (15° C.)) was added to make up to 100 mL, to prepare stock solutions 1 to 4.

[0057] [Table 2]

[0058] 2. Preparation of total-volume aerosol (Sample 1) 30 mL of concentrate 1 was filled into an aerosol pressure can (volume 100 mL), and the aerosol pressure can was closed with an aerosol valve (stem hole diameter 1.2 mm × 3, undertap hole diameter 1.85 mm). Then, 70 mL of dimethyl ether was filled under pressure as a propellant. The volume ratio of concentrate to propellant in the aerosol composition was 30:70 (concentrate:propellant). A total-amount spray button (nozzle hole diameter: 0.6 mm) was attached to the aerosol valve to obtain a total-amount spray type aerosol preparation.

[0059] (Samples 2-4) Total-emission aerosol preparations of Samples 2 to 4 were prepared in the same manner as Sample 1, except that Stock Solution 1 was replaced with Stock Solutions 2 to 4.

[0060] 3.Measurement of injection volume The total-volume-spray aerosol formulation prepared above was used for a 1m 3 The amount of the aerosol composition sprayed per unit was measured. A test room (length 3.6m x width 3.6m x height 2.5m: volume 32.4m) set at 25℃ 3 The total amount of sprayed aerosol was placed in the approximate center of the floor of the test chamber, and the spray button was operated to confirm that the aerosol composition had been sprayed, after which the test chamber was sealed. The weight (amount sprayed) and time when the total amount of the aerosol composition had been sprayed were measured, and the mass per 1 m was calculated using the following formula (1). 3 The amount of the aerosol composition sprayed per unit was determined. The sprayed weight was calculated by subtracting the weight of the aerosol after spraying from the weight of the aerosol before spraying. 1m 3 Amount injected per second (g / sec) = weight injected (g) ÷ time required to inject the entire amount (sec) ÷ volume of test chamber (m 3 ) ···(1) The results are shown in Table 3.

[0061] 4. Injection test As shown in Figure 1, an 8-tatami room (length 3.6m x width 3.6m x height 2.5m: volume 32.4m) 3 ) in the corner of the ceiling of the test room 10, and 10 cm on the bottom 2 Two plastic cups 2 (cup height 9.8 cm) with filter paper of the same size attached were placed with the cup openings facing the floor. A total-aerosol formulation 1 was placed in the approximate center of the floor of the test chamber 10, and the spray button was operated to confirm that the aerosol composition had been sprayed, after which the test chamber was sealed. After one hour, the plastic cups 2 were collected, and 10 adult female German cockroaches were placed in each of the collected plastic cups 2 as test insects. A plastic lid (with an air hole opened with tweezers) was then placed over the cups to ensure continuous contact between the filter paper and the susceptible German cockroaches. The number of knocked down (KD) susceptible German cockroaches (the number of cockroaches that fell over and were unable to move) 10 hours after the start of observation and the number of dead susceptible German cockroaches 24 hours after the start of observation were counted, and the KD rate and mortality rate for each plastic cup were calculated and their average values ​​were calculated. The above test was performed twice, and the KD rate and mortality rate at each time point are shown in Table 3.

[0062] [Table 3]

[0063] As shown in Table 3, samples 2 to 4 had significantly higher KD rates after 10 hours and mortality rates after 24 hours than sample 1, demonstrating that the KD effect and mortality effect in a plastic cup placed on the ceiling surface can be improved by adding a powdered substance to the raw materials of a total-spray aerosol agent. Among them, samples 2 and 3, which have a higher oil absorption rate of the powdered substance than sample 4, had better KD rates after 10 hours and mortality rates after 24 hours.

[0064] (Test Example 2) A test similar to Test Example 1 was carried out, except that the active ingredient was changed to methoxadiazone.

[0065] 1. Preparation of Stock Solutions According to the formulation shown in Table 4, the active ingredient and / or powdery substance was measured out, and absolute ethanol (specific gravity 0.797 (15°C)) was added to make up to 100 mL, to prepare stock solutions 5 to 8.

[0066] [Table 4]

[0067] 2. Preparation of total-volume aerosol (Specimen 5) 30 mL of concentrate 5 was filled into an aerosol pressure can (volume 100 mL), and the aerosol pressure can was closed with an aerosol valve (stem hole diameter 1.2 mm × 3, undertap hole diameter 1.85 mm). Then, 70 mL of dimethyl ether was filled under pressure as a propellant. The volume ratio of concentrate to propellant in the aerosol composition was 30:70 (concentrate:propellant). A total-amount spray button (nozzle hole diameter: 0.6 mm) was attached to the aerosol valve to obtain a total-amount spray type aerosol preparation.

[0068] (Samples 6-8) Total-emission aerosol preparations of Samples 6 to 8 were prepared in the same manner as Sample 5, except that Stock Solution 5 was replaced with Stock Solutions 6 to 8.

[0069] 3.Measurement of injection volume In the same manner as in "3. Measurement of the amount sprayed" in Test Example 1, the total amount spray type aerosol preparations of Samples 5 to 8 were used, and the amount sprayed was measured by 1 m 3 The amount of the aerosol composition sprayed per unit was measured. The results are shown in Table 5.

[0070] 4. Injection test In the same manner as in "4. Spray test" in Test Example 1, the KD rate and mortality rate of the susceptible German cockroach were determined using the total-spray type aerosol preparations of Samples 5 to 8. The results are shown in Table 5.

[0071] [Table 5]

[0072] As shown in Table 5, samples 6 to 8 had the same or higher KD rate of the test insects after 10 hours and significantly higher mortality rate after 24 hours than sample 5. It was found that the effect of the present invention can be obtained regardless of the type of active ingredient by blending a powdery substance in the raw material of a total-spray aerosol agent. Among them, samples 6 and 7, which have a higher oil absorption of the powdery substance than sample 8, had better KD rate of the test insects after 10 hours and mortality rate after 24 hours.

[0073] (Test Example 3) 1. Preparation of Stock Solutions According to the formulation shown in Table 6, the active ingredient and / or powdery substance was measured out, and absolute ethanol (specific gravity 0.797 (15°C)) was added to make up to 100 mL, to prepare stock solutions 9 to 12. In addition, stock solutions 9 to 12 have the same formulation as stock solutions 1 to 4 in Test Example 1.

[0074] [Table 6]

[0075] 2. Preparation of total-volume aerosol (Specimen 9) 30 mL of concentrate 9 was filled into an aerosol pressure can (volume 100 mL), and the aerosol pressure can was closed with an aerosol valve (stem hole diameter 0.6 mm × 2, undertap hole diameter 1.85 mm). Then, 70 mL of dimethyl ether was filled under pressure as a propellant. The volume ratio of concentrate to propellant in the aerosol composition was 30:70 (concentrate:propellant). A total-amount spray button (nozzle hole diameter: 0.6 mm) was attached to the aerosol valve to obtain a total-amount spray type aerosol preparation.

[0076] (Samples 10-12) Total-emission aerosol preparations of Samples 10 to 12 were prepared in the same manner as Sample 9, except that Stock Solution 9 was replaced with Stock Solutions 10 to 12.

[0077] (Sample 13) 30 mL of the concentrate 9 was filled into an aerosol pressure can (volume 100 mL), and the aerosol pressure can was closed with an aerosol valve (stem hole diameter 0.3 mm, undertap hole diameter 2.2 mm). Then, 70 mL of dimethyl ether was filled under pressure as a propellant. The volume ratio of the concentrate to the propellant in the aerosol composition was 30:70 (concentrate:propellant). A total-amount spray button (nozzle hole diameter: 0.6 mm) was attached to the aerosol valve to obtain a total-amount spray type aerosol preparation.

[0078] (Sample 14) A total-emission aerosol formulation of Sample 14 was prepared in the same manner as Sample 13, except that Stock Solution 9 was replaced with Stock Solution 10.

[0079] 3.Measurement of injection volume In the same manner as in "3. Measurement of the amount sprayed" in Test Example 1, the total amount spray type aerosol preparations of Samples 9 to 14 were used, and the amount sprayed was measured by 1 m 3 The amount of the aerosol composition sprayed per unit was measured. The results are shown in Table 7.

[0080] 4. Injection test In the same manner as in "4. Spray test" of Test Example 1, the KD rate and mortality rate of the susceptible German cockroach were determined using the total-spray type aerosol preparations of Samples 9 to 14. The results are shown in Table 7.

[0081] [Table 7]

[0082] As shown in Table 7, a comparison between sample 9 and samples 10 to 12, and a comparison between sample 13 and sample 14 shows that the sample is 1 m shorter than the test examples 1 and 2. 3 It was found that even under conditions where the amount of sprayed onto a target object was low, the KD effect and lethal effect in a plastic cup placed on the ceiling were improved by adding a powdered substance to the raw materials of a total-volume spray aerosol agent.

[0083] (Test Example 4) 1. Preparation of Stock Solutions According to the formulation shown in Table 8, the active ingredient and / or powdery substance was measured out, and absolute ethanol (specific gravity 0.797 (15°C)) was added to make up to 100 mL to prepare stock solutions 13 and 14.

[0084] [Table 8]

[0085] 2. Preparation of total-volume aerosol (Sample 15) 10 mL of the concentrate 13 was filled into an aerosol pressure can (volume 100 mL), and the aerosol pressure can was closed with an aerosol valve (stem hole diameter 1.2 mm × 3, undertap hole diameter 1.85 mm). Then, 90 mL of dimethyl ether was filled under pressure as a propellant. The volume ratio of the concentrate to the propellant in the aerosol composition was 10:90 (concentrate:propellant). A total-amount spray button (nozzle hole diameter: 0.6 mm) was attached to the aerosol valve to obtain a total-amount spray type aerosol preparation.

[0086] (Sample 16) A total-emission aerosol formulation of Sample 16 was prepared in the same manner as Sample 15, except that Stock Solution 13 was replaced with Stock Solution 14.

[0087] 3.Measurement of injection volume In the same manner as in "3. Measurement of the amount sprayed" in Test Example 1, the total amount spray type aerosol preparations of Samples 15 to 16 were used, and the amount sprayed was measured by 1 m 3 The amount of the aerosol composition sprayed per unit was measured. The results are shown in Table 9.

[0088] 4. Injection test In the same manner as in "4. Spray test" of Test Example 1, the KD rate and lethality rate of the susceptible German cockroach were determined using the total-spray type aerosol preparations of Samples 15 to 16. The results are shown in Table 9.

[0089] [Table 9]

[0090] As shown in Table 9, even when the ratio (volume ratio) of concentrate to propellant was 10:90, it was found that the KD effect and lethal effect in a plastic cup placed on the ceiling were improved by adding a powder substance to the raw materials of the total-volume aerosol agent. [Explanation of symbols]

[0091] 1. Total volume spray aerosol 2 plastic cups 10. Test Room

Claims

1. An aerosol composition comprising a powdery substance, a concentrate containing an active ingredient, and a propellant is filled in a pressure-resistant container, the active ingredient is a pest control ingredient, the powdery substance is at least one selected from the group consisting of silicon dioxide, calcium silicate, and magnesium silicate, and the powdery substance has an oil absorption of 35 mL / 100 g or more; 1 m of the aerosol composition ３ The total amount of spraying aerosol preparation is characterized in that the amount of spraying per unit time is in the range of 0.001 to 1 g / sec.

2. The aerosol composition is filled in a pressure-resistant container and comprises a concentrate containing a powdery substance and an active ingredient, and a propellant, the active ingredient being a pest control ingredient, the powdery substance being at least one selected from the group consisting of silicon dioxide, calcium silicate, and magnesium silicate, and the aerosol composition is dispensed from a total-spray aerosol agent having an oil absorption of 35 mL / 100 g or more. ３ The spray treatment method of the total amount spray type aerosol agent is characterized in that the spray rate is in the range of 0.001 to 1 g / sec per unit time.

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