JP2021102611A - Full ejection type aerosol agent - Google Patents

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

The present invention relates to a total amount injection type aerosol agent, and more particularly to a total amount injection type aerosol agent which is used by injecting almost the entire amount of the contents of the aerosol agent into a limited space in a short time.

Aerosols, which are made by dissolving active ingredients such as pesticides and deodorants in a small amount of solvent and filling the solution (aerosol stock solution) and propellant in a pressure-resistant container equipped with a sprayer, are pesticides in other dosage forms. For example, it is easier to operate than powders, emulsions, oils, aerosol products, etc., and has advantages such as not causing stains on the surroundings, so it is conveniently used.

Among such aerosols, a full-volume spray type aerosol has been developed that is placed on the floor and the entire contents are sprayed in a short time in order to exterminate pests and deodorize fragrance in a limited space such as a room. The total amount injection type aerosol agent has an advantage that the active ingredient can be treated almost uniformly in a closed space in a short time by a simple operation.

Such a total amount injection type aerosol agent includes, for example, an aerosol stock solution 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. , B / C volume ratio is 1/10 to 1/1, and the average particle size of the sprayed particles is 30 μm or less. An injection-type aerosol product, the content of which contains an inorganic agent (A) having a transition metal, a solvent (B) having a boiling point of 70 to 200 ° C., and an injection agent (C) containing dimethyl ether. However, a total amount injection type aerosol product (see Patent Document 2) in which the mass ratio (B / C) of the solvent (B) to the propellant (C) is 0.1 to 1.0 has been proposed.

JP-A-2002-226301 Japanese Unexamined Patent Publication No. 2014-227369

However, the conventional total amount injection type aerosol agent tends to have a smaller amount of the active ingredient adhered to the ceiling surface and the wall surface as compared with the floor surface. Therefore, in order to enhance the effect of the active ingredient on the ceiling surface and the wall surface, it is necessary to increase the amount of the active ingredient blended in the aerosol stock solution.

Therefore, the present invention provides a total amount injection type aerosol agent capable of improving the amount of the active ingredient adhering to the ceiling surface or the wall surface when the total amount injection type aerosol agent is used in a limited space such as a room. That is the issue.

As a result of diligent research on the above problems, the present inventor has found that the above problems can be solved by containing a powdery substance in the aerosol stock solution and using a total amount injection type aerosol agent that is sprayed at a specific injection amount. The present invention has been completed.

That is, the present invention is characterized by the following (1) to (2).
(1) An aerosol composition composed of a stock solution containing a powdery substance and an active ingredient and a propellant is filled in a pressure-resistant container, and the propellant amount per ^{1 m 3 of the aerosol composition is 0.001 to 1 g / sec.} A total injection type aerosol agent characterized by being in the range.
(2) powder substances and active ingredients from the total amount of injection type aerosols aerosol composition comprising a propellant stock was filled in a pressure vessel containing the said aerosol composition 1 m ³ per 0.001 to 1 g / sec A method for spraying a total amount injection type aerosol agent, which comprises spraying in the range of.

According to the total amount injection type aerosol agent of the present invention, the adhesion of the powdery substance to the treatment surface in the treatment target space is improved, so that when the total amount injection type aerosol agent is sprayed in a closed space such as a room, it is in the form of powder. The amount of the active ingredient retained in the substance attached to the ceiling surface or the wall surface can be improved, and the sustainability of the effect of the active ingredient can also be improved.

It is a figure explaining the test method of the injection test.

In the total amount injection type aerosol agent of the present invention, an aerosol composition composed of a stock solution and an injection agent is filled in a pressure-resistant container equipped with an injection device, and the injection amount per ^{1 m 3 of the aerosol composition is 0.001 to 1 g / g.} It is in the range of seconds.

(Stock solution)
The undiluted solution contains a powdery substance and an active ingredient.
The powdery substance is preferably one that can retain the active ingredient on its surface and inside, and when the entire amount of the aerosol composition, which is the content of the total amount injection type aerosol agent, is injected, the powdery substance retains the active ingredient. The substance adheres to the treated surface in the space to be treated, and the effect of the active ingredient is exhibited on the treated surface.

The powdery substance preferably has an oil absorption amount of 35 mL / 100 g or more. According to the study of the present inventor, when the total amount spray type aerosol agent is used in a space such as a room, the residual effect of the powdery substance on the ceiling surface or the wall surface may differ depending on the oil absorption amount of the powdery substance mixed in the undiluted solution. Do you get it. In the case of a total amount spray type aerosol agent containing a powdery substance having an oil absorption amount of 35 mL / 100 g or more, the amount of the powdery substance remaining on the ceiling surface or the wall surface increases, and the ceiling surface of the active ingredient retained in the powdery substance accordingly. And the amount of adhesion to the wall surface can be improved.

The oil absorption of the powdery substance is more preferably 100 mL / 100 g or more, and further preferably 200 mL / 100 g or more. The upper limit of the oil absorption amount is not particularly limited, but from the viewpoint of diffusivity at the time of injection, it is preferably 500 mL / 100 g or less, more preferably 400 mL / 100 g or less, still more preferably 350 mL / 100 g or less. The oil absorption of the powdery substance can be measured by, for example, a method based on JIS K5101, ASTM D2414, ISO4656, or the like.

The specific surface area of powdery material is preferably 50 to 500 m ² / g, more preferably 100 to 400 m ² / g, more preferably 150~350m ² / g. When the specific surface area of the powdery substance is 50 m ² / g or more, the active ingredient can be sufficiently retained, so that the effect of the present invention can be exhibited, and when it is 500 m ² / g or less, the active ingredient is retained. It's never too much. The specific surface area of the powdery substance can be measured by, for example, a method based on the BET method, ISO 5794-1 or the like.

The average particle size of the powdery substance is preferably 1 to 25 μm, more preferably 1.5 to 20 μm, still 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 easily falls from the ceiling surface or the wall surface, so that the average particle size is 25 μm or less. Is preferable. The average particle size of the powdery substance is the volume average particle size, and can be measured by, for example, ISO 13320, the Coulter counter method (Coulter multisizer method), or the like.

Examples of the powdery substance include inorganic compounds and organic compounds. Examples of the inorganic compound include metal oxides such as silicon dioxide (silica), calcium silicate, magnesium silicate, and alumina. Examples of the organic compound include polyethylene resin, polystyrene resin, silicone resin and the like. One of these may be used alone, or two or more thereof may be used in combination. Among these, an inorganic compound is preferable from the viewpoint of dispersibility in the aerosol composition, and it is more preferable to use at least one selected from the group consisting of silicon dioxide, calcium silicate and magnesium silicate.

As a specific example of the powdery substance, as a powdery substance having an oil absorption amount of 35 mL / 100 g or more, for example, a commercially available product "Sunsphere NP-200" (trade name, manufactured by AGC Si-Tech Co., Ltd., oil absorption amount 40 mL / 100 g). , Specific surface area 100 m ² / g, average particle size 20 μm), “Tokuseal NP” (trade name, manufactured by Oriental Silicon Corporation, oil absorption 270 mL / 100 g, specific surface area 190 m ² / g, average particle size 10.3 μm), “Adsorber” 101 ”(trade name, manufactured by Freund Sangyo Co., Ltd., oil absorption amount 310 mL / 100 g, specific surface area 300 m ² / g, average particle size 3.2 μm) and the like can be mentioned.

The powdery substance is preferably contained in the stock solution at a ratio of 0.01 to 15% by weight / volume% (hereinafter referred to as "w / v%"), more preferably 0.05 to 10 w / v%. , 0.1 to 5 w / v% is more preferable. When the content of the powdery substance in the stock solution is 0.01 w / v% or more, the active ingredient which is not retained by the powdery substance and exists can be eliminated, and when it is 15 w / v% or less, the aerosol agent. It does not cause injection troubles such as clogging of the powdery substance at the injection port and the inability to inject the entire amount.

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 0.01 to 5 w / v%. Is even more preferable. When the content of the powdery substance in the aerosol composition is 0.001 w / v% or more, the adhesiveness of the active ingredient on the treated surface can be improved, and when it is 7.5 w / v% or less, it is said. Powdery substances do not cause caking in aerosol products and are easily redispersed during use.

The active ingredient refers to one that exerts some action when a total amount injection type aerosol agent is used. The active ingredient is not particularly limited, and examples thereof include a pest control component, an aromatic component, a deodorant component, a sterilization / bactericidal component, and the like.

The type of pest control component is not particularly limited, and known compounds can be used.
Pest control ingredients include, for example, permethrin, pyrethrin, alesulin, phthalthrin, resmethrin, flamethrin, phenothrin, empentrin, praretrin, ciphenothrin, sifluthrin, imiprothrin, transfluthrin, metoflutrin, dimefurthrin, mepafurthrin, profluthrin, Pyrethroid compounds; organic phosphorus compounds such as fenitrothione, dichlorovos, chlorpyriphosmethyl, diazinone, fenthion; carbamate compounds such as carbalyl and propoxul; compounds such as metoprene, pyriproxyfen, methoxadiazone, fipronil, amidoflumeth, brofuranilide; Orange oil, uikyo oil, kehi oil, butterfly oil, television oil, eucalyptus oil, hiba oil, jasmine oil, neroli oil, peppermint oil, bergamot oil, butiglen oil, lemon oil, lemongrass oil, cinnamon oil, citronella oil, geranium oil , Citral, l-menthol, citronellyl acetate, synamic aldehyde, terpineol, nonyl alcohol, cis-jasmon, limonene, linalol, 1,8-cineole, geraniol, α-pinene, p-menthan-3,8-diol, eugenol , Various essential oil components such as menthyl acetate, timole, benzyl benzoate, benzyl salicylate; propylene glycol monopropyl ether, propylene glycol monobutyl ether, dipropylene glycol monopropyl ether, dipropylene glycol monobutyl ether, dipropylene glycol dimethyl ether, ethylene glycol mono Glycol ethers such as isobutyl 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 and the like can be mentioned. These may be used individually by 1 type, and may be used in combination of 2 or more type.

The pest control component may be appropriately selected according to the type of target pest. Target pests include, for example, mosquitoes, flies, moths, bees, turtles, tokojirami, cockroaches, ants, spiders, dung beetles, mites, ticks, sardines, centipedes, gnats, yasde, spiders, abs, gnats, butterfly flies, termites, and chironomids. , Yokobai, Kikuimushi, Garbage beetle, Scissors, Stain, Kamikirimushi, Katsuobushimushi, Chatatemushi, Iga, Koiga and the like.
For flying pests such as mosquitoes, flies, moths, bees, abs, gnats, midges, yokobai, butterfly flies, clothes moths, clothes moths, transfluthrin, metoflutrin, profluthrin, phthalthrin, praretrin, monfluorotrin, metoxadiazone, brofuranilide, etc. Is preferable. In addition, for cockroaches, bedbugs, bed bugs, ants, spiders, mite, mites, sardines, mud, termites, yasde, spiders, termites, bedbugs, bedbugs, bedbugs, stains, etc. , Phthalthrin, Praletrin, Imiprothrin, Permethrin, Propoxul, Metoxadiazone, Amidoflumeth, Brofuranilide and the like are suitable.

Examples of aromatic components include anis oil, lavender oil, rose oil, rosemary oil, grapefruit oil, camphen, p-simene, citronellol, nerol, benzyl alcohol, n-butylaldehyde, and isobutyl, in addition to the above-mentioned essential oil components. Examples include aldehyde, coumarin, cineole and the like. These may be used individually by 1 type, and may be used in combination of 2 or more type.

Deodorant components include, for example, green tea extract, persimmon tannin, methacrylate laurate, methyl benzoate, methyl phenylacetate, geranyl crotolate, acetophenone myristate, benzyl acetate, benzyl propionate, silver and other odor components. Or, a component that masks an odor component such as the above-mentioned fragrance component can be mentioned. These may be used individually by 1 type, and may be used in combination of 2 or more type.

Examples of the sterilizing / sterilizing component include siabendazole, 4-isopropyl-3-methylphenol (IPMP), 3-iodo-2-propynylbutylcarbamate (IPBC), and p-chlorophenyl-3-iodopropagilformal (IPBC). Environmental hygiene bactericides such as IF-1000); Agricultural chemical sterilizers such as isophthalonitrile, procymidone, bileton, morestan; silver alone, silver oxide, inorganic silver salts (eg, silver chloride, silver nitrate, silver sulfate, silver carbonate) , Sulfonic acid silver salt, etc.), organic silver salts (for example, silver nitrate, silver acetate, etc.) and other silver compounds. These may be used individually by 1 type, and may be used in combination of 2 or more type.

As the active ingredient, ingredients having different effects can be used in combination. For example, the pest control component and the fragrance component can be used in combination, or the fragrance component and the deodorant component other than the fragrance component can be used in combination.

The content of the active ingredient may be appropriately adjusted according to the type of active ingredient, application, size of application space, usage environment, etc., and specifically, it should be 0.01 to 30 w / v% in the undiluted solution. Is preferable, 0.1 to 25 w / v% is more preferable, and 0.5 to 20 w / v% is further preferable. When the content of the active ingredient in the stock solution is 0.01 w / v% or more, a sufficient effect of the active ingredient can be obtained, and when it is 30 w / v% or less, the production suitability is improved.

Further, the content of the active ingredient in the aerosol composition may be appropriately adjusted according to the type of active ingredient, application, size of application space, usage environment, etc., and specifically, 0.001 to 15 w / v%. The range is preferably 0.005 to 12.5 w / v%, more preferably 0.01 to 10 w / v%. When 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 when it is 15 w / v% or less, the production suitability is improved.

The undiluted solution may contain a solvent for purposes such as the viscosity of the undiluted solution, production suitability, and the effect of the active ingredient (for example, when the active ingredient is a pest control agent, the permeability of the drug to pests is increased). Good. Examples of such a solvent include glycol ethers, organic solvents such as hydrocarbon solvents, alcohol solvents, aromatic solvents, ester solvents, and water.

Examples of the hydrocarbon solvent include aliphatic hydrocarbons such as paraffin-based hydrocarbons and naphthen-based hydrocarbons, and alicyclic hydrocarbons, and specific examples thereof include normal paraffin and isoparaffin. The normal paraffin preferably has 8 to 16 carbon atoms, and examples thereof include neothiosol manufactured by Chuo Kasei Co., Ltd. and normal paraffin MA manufactured by JXTG Energy Co., Ltd. The isoparaffin preferably has 8 to 16 carbon atoms, and examples thereof include IP Clean LX and Supersol FP25 manufactured by Idemitsu Kosan Co., Ltd.
Examples of the alcohol solvent include lower alcohols such as ethanol and propanol (normal, iso), and polyhydric alcohols such as glycerin and ethylene glycol.
Examples of the aromatic solvent include toluene, xylene and the like.
Examples of the ester solvent include isopropyl myristate, hexyl laurate, isopropyl palmitate and the like.
Examples of water include tap water, distilled water, purified water, ion-exchanged water and the like.

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%, more preferably 60 to 99.9 w / v%, and 70 to 99.5 w / v% in the stock solution. v% is more preferred. When the content of the solvent is 50 w / v% or more, the production suitability can be improved, and when it is 99.98 w / v% or less, a sufficient effect of the active ingredient can be obtained.

The stock solution is obtained by dissolving / dispersing the powdery substance and the active ingredient in, for example, a solvent. The active ingredient is supported on the powder substance in the undiluted solution, and when injected by the propellant, the active ingredient is injected while being supported on the powder substance, and the powder substance carrying the active ingredient is treated. Adheres to the surface.

The method for supporting the active ingredient on the powder substance is not particularly limited. For example, the liquid active ingredient is dropped or sprayed onto the powder material to bring them into contact with each other, or the powder material is immersed in the liquid active ingredient to bring them into contact with each other, which is effective for the powder material. A method of adding a substance carrying an ingredient to a solvent, a method of adding a powder substance and an active ingredient to the solvent separately, and a method of supporting the active ingredient in the powder substance in a stock solution by stirring if necessary, etc. Can be mentioned.

The undiluted solution may contain other components as long as the effects of the present invention are not impaired. Examples of other components include preservatives, pH adjusters, ultraviolet absorbers, surfactants, solubilizing agents and the like, and the content can be appropriately adjusted.

The content of the undiluted solution in the aerosol composition can be appropriately changed according to the purpose of use of the total amount injection type aerosol agent and the combination with the injection agent, and is not particularly limited. For example, 1 to 50 volumes in the aerosol composition. Can be%. When the undiluted solution 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 undiluted solution can be sprayed as spray particles. When used, it can reduce the contamination of furniture, floors, walls, etc. by the undiluted solution. The lower limit of the content of the stock solution in the aerosol composition is more preferably 5% by volume or more, further preferably 10% by volume or more, and the upper limit is more preferably 40% by volume or less, and 35% by volume. The following is more preferable.

(Injector)
The propellant is a medium for injecting the undiluted solution, and is pressure-filled in a pressure-resistant container together with the undiluted solution.
Examples of 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 gas, nitrogen gas and compressed air, and HFC-152a. , HFC-134a, HFO-1234yf, HFO-1234ze and the like halogenated carbon gas and the like, or two or more kinds can be used. The propellant to be used may be appropriately selected according to the compatibility with the undiluted solution and the container member such as the aerosol valve.

The content of the propellant in the aerosol composition can be appropriately changed according to the purpose of use of the total amount propellant aerosol and the combination with the stock solution, and is not particularly limited. For example, 50 to 99 volumes in the aerosol composition. Can be%. When the propellant is 50% by volume or more in the aerosol composition, the stock solution 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. Further, when the propellant is 99% by volume or less, a sufficient effect of the active ingredient can be obtained. The lower limit of the content of the propellant in the aerosol composition is more preferably 60% by volume or more, further preferably 65% by volume or more, and the upper limit is more preferably 95% by volume or less, and 90% by volume or less. More preferred.

The volume ratio of the stock solution to the propellant in the aerosol composition is preferably 1:99 to 50:50 for the stock solution: propellant, more preferably 3:97 to 40:60, and 5:95 to 30. : 70 is more preferable. With such a volume ratio, a sufficient effect of the active ingredient can be obtained.

(Total amount injection type aerosol agent)
The total amount injection type aerosol agent of the present invention is configured by filling the pressure-resistant container for aerosol with the above-mentioned stock solution and the propellant, and closing the opening of the pressure-resistant container with an aerosol valve. The total amount injection type aerosol agent is an aerosol composition (undiluted solution and injection agent) in a pressure-resistant container in which an injection member (hereinafter, also referred to as an injection button) attached to an aerosol valve is operated once by a user. The entire amount is extruded out of the pressure vessel through the aerosol valve, at which time the aerosol composition is injected in the form of particles.

(Aerosol valve)
The aerosol valve has an opening / closing member for switching communication and blocking between the inside and the outside of the pressure-resistant container when the injection member is operated by the user, a housing to which the opening / closing member is attached, and a housing at a predetermined position of the pressure-resistant container. A mounting member for holding is provided. Further, the opening / closing member includes a stem that slides up and down in conjunction with the injection member. The sliding of the stem switches between communication (injection state) and cutoff (non-injection 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 incorporated in the housing to the injection member. The path from the housing hole to the stem hole constitutes an internal passage through which the aerosol composition passes.

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 shape of the stem hole is polygonal, the size of the stem hole may be the same as that in the case of a circle.
When the under tap hole of the stem is circular, the size thereof is preferably 0.5 to 3 mm in diameter, more preferably 0.7 to 2.5 mm in diameter, and further preferably 1 to 2.2 mm in diameter. The shape of the undertap hole may be circular or polygonal, and in the case of a polygon, the size of the undertap hole may be the same as that in the case of a circular shape.
The stem may or may not have a vapor tap hole, but if it has a vapor tap hole, its size is preferably 0.1 to 3 mm in diameter when it is circular, and the diameter is 0.2. ~ 2.5 mm is more preferable, and a diameter of 0.3 to 2.2 mm is further preferable. The shape of the vapor tap hole may be circular or polygonal, and in the case of a polygon, the size of the vapor tap hole may be the same as that in the case of a circle.
The stem hole and the vapor tap hole may be one or have a plurality of holes. The size of the stem hole and the vapor tap hole is the total size of a plurality of them, if any.

(Injection member)
The injection member (injection button) is a member attached to the pressure-resistant container via an aerosol valve. The injection button is formed with a passage in the operation unit through which the aerosol composition taken in from the pressure-resistant container passes through the stem hole of the aerosol valve and a nozzle into which the aerosol composition is injected.
When the injection member used for the total amount injection type aerosol agent is pressed against the injection button, the injection button is fixed in a state where the stem of the aerosol valve is pressed down, and the aerosol composition is passed through the pressed stem to the injection button. Continuously ejects (total amount injection) from the nozzle of.

The shape of the injection button injection button may be circular or polygonal. When the injection port is circular, the inner diameter (injection hole diameter) may be appropriately adjusted according to the design of the injection amount and the injection time, but for example, the diameter is preferably 0.1 to 2 mm, and the diameter is 0.3. ~ 1.5 mm is more preferable, and a diameter of 0.6 to 1.2 mm is further preferable. When the shape of the nozzle is polygonal, the size of the nozzle may be the same as that of the circular shape. Further, there is no problem even if a plurality of nozzles having the same area as these are provided.

(Aerosol internal pressure)
The internal pressure of the total amount injection type aerosol agent at 25 ° C. is preferably 0.2 to 0.8 MPa. When the internal pressure is 0.2 MPa or more, the entire amount of the aerosol composition can be injected while ensuring the diffusibility of the powdery substance into the space used. Further, when the internal pressure is 0.8 MPa or less, it is possible to prevent the aerosol composition from coming out too vigorously at the time of injection and the powdery substance hitting the ceiling constituting the use space and falling without adhering. The internal pressure of the total amount injection type aerosol agent is more preferably 0.25 to 0.6 MPa, further preferably 0.3 to 0.5 MPa.

(Injection pressure)
The injection pressure of the total amount injection type aerosol agent is preferably 1 to 15 gf, more preferably 3 to 10 gf, as measured at a position 20 cm away from the injection port. When the injection pressure is within the above range, the aerosol composition can be scattered to the ceiling surface when used in a space in a general building.
The injection pressure is a circle with a diameter of 60 mm mounted on a digital force gauge (for example, manufactured by Imada Co., Ltd., model number: DS2-2N) at a distance of 20 cm in the vertical direction from the injection port of the total injection type aerosol agent. It can be measured by setting a flat plate in the shape of a plate and using the maximum value when the aerosol composition is sprayed toward the center of the flat plate at room temperature of 25 ° C. as the injection load and calculating the average.

(Injection amount)
In the total amount injection type aerosol agent of the present invention, ^{the injection amount per 1 m 3 of the} aerosol composition is in the range of 0.001 to 1 g / sec. ^{When the injection amount per 1 m 3} of the aerosol composition is 0.001 g / sec or more, the momentum of the injection can be obtained, so that the aerosol composition can be scattered over the entire use space, and it is 1 g / sec or less. , The safety as an aerosol agent can be guaranteed. The injection amount per 1 m ³ is preferably 0.005 to 0.7 g / sec, more preferably 0.01 to 0.5 g / sec.

(Injection time)
The injection time until the entire amount of the total amount injection type aerosol agent of the present invention is injected is preferably 5 to 150 seconds. When the injection time is 5 seconds or more, the active ingredient can be injected into the entire space to be used, and when the injection time is 150 seconds or less, the injection amount of the aerosol agent per unit time can be increased. It is possible to increase the scattering property of the active ingredient, thereby increasing the amount of the active ingredient adhering to the ceiling surface and the wall surface. The injection time is more preferably 7 to 120 seconds, even more preferably 10 to 100 seconds.

Examples of the method of adjusting the injection amount and the injection time include a method of adjusting the size of the injection port of the injection button, a method of adjusting the injection pressure of the total amount injection type aerosol agent, a method of adjusting the stem hole diameter of the aerosol valve, and an injection. Examples thereof include a method of adjusting the pressure of the agent and a combination thereof.

In the present invention, with reference to the total amount injected aerosol dose of the present invention described above, the aerosol composition from the total amount of injection aerosol dose, is injected in the range of 1 m ³ per 0.001 to 1 g / sec. By injecting the aerosol composition so as to have an injection amount within the above range, it is possible to improve the adhesion of the powdery substance to the treatment surface in the treatment target space, and the total amount injection type aerosol agent in a closed space such as a room. It is possible to improve the amount of the active ingredient retained in the powdery substance adhering to the ceiling surface and the wall surface when the powder is sprayed, and thus the sustainability of the effect of the active ingredient can also be improved.
The injection amount per 1 m ³ is preferably 0.005 to 0.7 g / sec, more preferably 0.01 to 0.5 g / sec.

In the present invention, the undiluted solution of the total amount injection type aerosol agent in which the aerosol composition composed of the undiluted solution and the propellant is filled in a pressure-resistant container contains a powdery substance, and the aerosol composition is sprayed per ^{1 m 3.} Also provided is a method of enhancing the efficacy of a total volume injection aerosol agent by setting the amount in the range of 0.001 to 1 g / sec.
As described above, when the powdery substance is contained in the total amount of the injection type aerosol agent, the amount of residue on the ceiling surface or wall surface of the room or the like increases. Therefore, by incorporating the powdery substance in the undiluted solution and injecting it so that the injection amount is within the above range, the active ingredient retained in the powdery substance also remains on the ceiling surface and the wall surface, so that it is effective on the treated surface. The amount of components adhered is improved. Therefore, the efficacy of the total amount injection type aerosol agent can be enhanced.

The present invention will be further described with reference to the following test examples, but the present invention is not limited to the following test examples.

The powdery substances used in the following test examples are as shown in Table 1.

(Test Example 1)
1. 1. Preparation of undiluted solution According to the formulation shown in Table 2, the active ingredient and / or powdery substance is measured, and absolute ethanol (specific gravity 0.797 (15 ° C.)) is added to make up to 100 mL, and the undiluted solution 1 to 1 4 was prepared.

2. Preparation of full-volume spray aerosol agent (Sample 1)
An aerosol pressure can (capacity 100 mL) was filled with 30 mL of undiluted solution 1, and the aerosol pressure can was closed with an aerosol valve (stem hole diameter 1.2 mm × 3, undertap hole diameter 1.85 mm). Subsequently, 70 mL of dimethyl ether was pressure-filled as a propellant. The volume ratio of the stock solution to the propellant in the aerosol composition was 30:70 for the stock solution: propellant.
An injection button (injection hole diameter 0.6 mm) for total injection was attached to the aerosol valve to obtain a total injection type aerosol agent.

(Samples 2-4)
A total amount injection type aerosol agent for Samples 2 to 4 was prepared in the same manner as Sample 1 except that Stock Solution 1 was replaced with Stock Solutions 2 to 4.

3. 3. Measurement of Injection Amount The injection amount of the aerosol composition per ^{1 m 3} was measured using the total amount injection type aerosol agent prepared above.
Place the total amount of spray-type aerosol in the center of the floor of the test room (length 3.6 m x width 3.6 m x height 2.5 m: volume 32.4 m ^{3) set at 25 ° C, and operate the spray button.} After confirming that the aerosol composition had been sprayed, the test room was sealed. The weight (injection amount) and time when the entire amount of the aerosol composition was injected were measured, and the injection amount of the aerosol composition per ^{1 m 3 was determined by the following formula (1).} The injected weight is a value obtained by subtracting the weight of the aerosol agent after injection from the weight of the aerosol agent before injection.
Injection amount per 1 m ³ (g / sec) = weight injected (g) ÷ time required for total injection (seconds) ÷ volume of test room (m ³ ) ... (1)
The results are shown in Table 3.

4. Injection test As shown in Fig. 1, in the corner of the ceiling of the test room 10 in an 8 tatami space (length 3.6 m x width 3.6 m x height 2.5 m: volume 32.4 m ^{3 ), 10 cm 2} on the bottom. Two plastic cups 2 (cup height 9.8 cm) to which a filter paper of a size was attached were installed so that the cup openings faced the floor. A total amount injection type aerosol agent 1 was placed substantially in the center of the floor surface of the test room 10, and the test room was sealed after confirming that the aerosol composition had been sprayed by operating the injection button.
One hour later, the plastic cup 2 was collected, and 10 adult female German cockroaches were placed in each of the collected plastic cups 2 as test insects, covered with a plastic lid (with a vent hole made with tweezers), and sensitive to filter paper. Continuous contact with the German cockroach was made.
The number of knockdowns (KD) of sensitive German cockroaches 10 hours after the start of observation (the number of cockroaches that fell and became stuck) and the number of lethal numbers of sensitive German cockroaches 24 hours after the start of observation were counted, and KD for each plastic cup. The rate and lethality were calculated, and their average values were calculated.
The above test was performed twice, and the KD rate and mortality rate at each elapsed time in each test are shown in Table 3.

As shown in Table 3, Specimens 2 to 4 have a significantly higher KD rate after 10 hours and a lethality rate after 24 hours than Specimen 1, and are powdery in the raw material of the total spray type aerosol agent. It was found that the KD effect and the lethal effect of the plastic cup installed on the ceiling surface were improved by blending the substance. Among them, the samples 2 and 3 having a higher oil absorption of the powder substance than the sample 4 were more excellent in the KD rate after 10 hours and the mortality rate after 24 hours.

(Test Example 2)
The active ingredient was changed to methoxadiazone, and the same test as in Test Example 1 was conducted.

1. 1. Preparation of undiluted solution According to the formulation shown in Table 4, the active ingredient and / or powdery substance is measured, and absolute ethanol (specific gravity 0.797 (15 ° C.)) is added to make up to 100 mL, and the undiluted solution 5 to 5 8 was prepared.

2. Preparation of full-volume spray aerosol agent (Sample 5)
An aerosol pressure can (capacity 100 mL) was filled with 30 mL of the stock solution 5, and the aerosol pressure can was closed with an aerosol valve (stem hole diameter 1.2 mm × 3, under tap hole diameter 1.85 mm). Subsequently, 70 mL of dimethyl ether was pressure-filled as a propellant. The volume ratio of the stock solution to the propellant in the aerosol composition was 30:70 for the stock solution: propellant.
An injection button (injection hole diameter 0.6 mm) for total injection was attached to the aerosol valve to obtain a total injection type aerosol agent.

(Samples 6-8)
A total amount injection type aerosol agent for Samples 6 to 8 was prepared in the same manner as for Specimen 5 except that the stock solution 5 was replaced with the stock solutions 6 to 8.

3. 3. Measurement of injection amount In the same manner as in the method described in "3. Measurement of injection amount" of Test Example 1, the injection amount of the aerosol composition per ^{1 m 3 is measured by using the total amount injection type aerosol agent of the samples 5 to 8.} did.
The results are shown in Table 5.

4. Injection test Similar to the method described in "4. Injection test" of Test Example 1, the KD rate and the mortality rate of the sensitive German cockroach were determined by using the total amount injection type aerosol agent of the samples 5 to 8.
The results are shown in Table 5.

As shown in Table 5, the KD rate of the specimens 6 to 8 after 10 hours was equal to or higher than that of the sample 5, and the mortality rate after 24 hours was remarkably high. It was found that the effect of the present invention can be obtained regardless of the type of the active ingredient by blending the powdery substance in the raw material of the total amount injection type aerosol agent. Among them, the samples 6 and 7, which had a higher oil absorption of the powder substance than the sample 8, had a more excellent KD rate after 10 hours and a mortality rate after 24 hours.

(Test Example 3)
1. 1. Preparation of undiluted solution According to the formulation shown in Table 6, the active ingredient and / or powdery substance is measured, and absolute ethanol (specific gravity 0.797 (15 ° C.)) is added to make up to 100 mL, and the undiluted solution 9 to 9 to 12 was prepared.
The stock solutions 9 to 12 have the same formulation as the stock solutions 1 to 4 of Test Example 1.

2. Preparation of full-volume spray aerosol agent (Sample 9)
An aerosol pressure can (capacity 100 mL) was filled with 30 mL of the undiluted solution 9, and the aerosol pressure can was closed with an aerosol valve (stem hole diameter 0.6 mm × 2, undertap hole diameter 1.85 mm). Subsequently, 70 mL of dimethyl ether was pressure-filled as a propellant. The volume ratio of the stock solution to the propellant in the aerosol composition was 30:70 for the stock solution: propellant.
An injection button (injection hole diameter 0.6 mm) for total injection was attached to the aerosol valve to obtain a total injection type aerosol agent.

(Samples 10 to 12)
A total amount injection type aerosol agent for samples 10 to 12 was prepared in the same manner as for sample 9 except that the stock solution 9 was replaced with the stock solution 10-12.

(Sample 13)
An aerosol pressure can (capacity 100 mL) was filled with 30 mL of the undiluted solution 9, and the aerosol pressure can was closed with an aerosol valve (stem hole diameter 0.3 mm, undertap hole diameter 2.2 mm). Subsequently, 70 mL of dimethyl ether was pressure-filled as a propellant. The volume ratio of the stock solution to the propellant in the aerosol composition was 30:70 for the stock solution: propellant.
An injection button (injection hole diameter 0.6 mm) for total injection was attached to the aerosol valve to obtain a total injection type aerosol agent.

(Sample 14)
A total amount injection type aerosol agent of sample 14 was prepared in the same manner as sample 13 except that the stock solution 9 was replaced with the stock solution 10.

3. 3. Measurement of injection amount In the same manner as in the method described in "3. Measurement of injection amount" of Test Example 1, the injection amount of the aerosol composition per ^{1 m 3 is measured by using the total amount injection type aerosol agent of the samples 9 to 14.} did.
The results are shown in Table 7.

4. Injection test Similar to the method described in "4. Injection test" of Test Example 1, the KD rate and the mortality rate of the sensitive German cockroach were determined by using the total amount injection type aerosol agent of the samples 9 to 14.
The results are shown in Table 7.

As shown in Table 7, even under the condition that the injection amount per ^{1 m 3} is lower than that of Test Examples 1 and 2 as compared with the comparison between the sample 9 and the sample 10 to 12 and the comparison between the sample 13 and the sample 14, the total amount injection type aerosol is used. It was found that the KD effect and the lethal effect in the plastic cup installed on the ceiling surface were improved by blending the powdery substance in the raw material of the agent.

(Test Example 4)
1. 1. Preparation of undiluted solution According to the formulation shown in Table 8, the active ingredient and / or powdery substance is measured, and absolute ethanol (specific gravity 0.797 (15 ° C.)) is added to make up to 100 mL, and the undiluted solution 13 to 13 to 14 was prepared.

2. Preparation of full-volume spray aerosol agent (Sample 15)
An aerosol pressure can (capacity 100 mL) was filled with 10 mL of the undiluted solution 13, and the aerosol pressure can was closed with an aerosol valve (stem hole diameter 1.2 mm × 3, under tap hole diameter 1.85 mm). Subsequently, 90 mL of dimethyl ether was pressure-filled as a propellant. The volume ratio of the stock solution to the propellant in the aerosol composition was 10:90 for the stock solution: propellant.
An injection button (injection hole diameter 0.6 mm) for total injection was attached to the aerosol valve to obtain a total injection type aerosol agent.

(Sample 16)
A total amount injection type aerosol agent of the sample 16 was prepared in the same manner as the sample 15 except that the stock solution 13 was replaced with the stock solution 14.

3. 3. Measurement of injection amount In the same manner as in the method described in "3. Measurement of injection amount" of Test Example 1, the injection amount of the aerosol composition per ^{1 m 3 is measured by using the total amount injection type aerosol agent of the samples 15 to 16.} did.
The results are shown in Table 9.

4. Injection test Similar to the method described in "4. Injection test" of Test Example 1, the KD rate and mortality rate of the sensitive German cockroach were determined by using the total amount injection type aerosol agent of the samples 15 to 16.
The results are shown in Table 9.

As shown in Table 9, even under the condition that the content ratio (volume ratio) of the undiluted solution and the propellant is 10:90, the plastic installed on the ceiling surface by blending the powdery substance in the raw material of the total amount spray type aerosol. It was found that the KD effect and lethal effect in the cup were improved.

1 Total spray type aerosol 2 Plastic cup 10 Laboratory

Claims (2)

An aerosol composition consisting of a stock solution containing a powdery substance and an active ingredient and a propellant is filled in a pressure-resistant container.
A total amount injection type aerosol agent, ^{wherein the injection amount per 1 m 3} of the aerosol composition is in the range of 0.001 to 1 g / sec. From a total amount injection type aerosol composition in which an aerosol composition consisting of a stock solution containing a powdery substance and an active ingredient and a propellant is filled in a pressure-resistant container, the aerosol composition is applied in the range of 0.001 ^{to 1 g / sec per 1 m 3.} A method for spraying a total amount injection type aerosol agent, which comprises spraying.

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