JP6322176B2 - Disinfection method - Google Patents

Description

  The present invention relates to a sterilization method.

Conventionally, methods for using various drugs are known as methods for sterilizing molds, bacteria, and the like, and the modes of use are also various.
For example, Patent Document 1 discloses a method for sterilizing a space in which glycol ether is volatilized in the space as a method for sterilizing microorganisms such as molds, yeasts, viruses, and bacteria present in air in a closed space such as a room. doing.
Further, Patent Document 2 discloses a sterilization method using a sterilizing agent such as benzalkonium chloride as a sterilization method against microorganisms such as mold that floats in the air or adheres to furniture. And a method of spraying in an accumulator spray container is described.

JP 2007-09738 A JP 2010-083806 A

  As described above, sterilization methods using various drugs have been known so far. However, in the sterilization method described in Patent Document 1, natural volatilization or forced volatilization is cited as an aspect of volatilizing glycol ether in the space. In the case of forced volatilization, for example, in a heat volatilization method using a heater or the like, a transpiration aid or the like is required to volatilize glycol ether more efficiently, and as a simple and efficient sterilization method Was insufficient. Moreover, in the sterilization method of patent document 2, although the aspect which accommodates and sprays a chemical | medical solution in a pressure accumulation type spray container is mentioned, it mixes with a solvent etc. and sprays as a chemical | medical solution. The dispersibility of the disinfectant was insufficient. Accordingly, an object of the present invention is to provide a sterilization method that allows simple and efficient diffusion and provides a better sterilization effect.

The inventors of the present invention have newly found that fungi and bacteria can be sterilized well by heating azodicarbonamide with a predetermined heat source and evaporating it, and have completed the present invention.
That is, the present invention is as follows.
A sterilization method for sterilization using azodicarbonamide,
Heating the azodicarbonamide with a heat source to evaporate,
The sterilization method, wherein the heat source is a heat source having a maximum temperature reached by heating of 380 ° C or higher.

  According to the present invention, azodicarbonamide is evaporated by heating the azodicarbonamide with a heat source having a maximum heating temperature of 380 ° C. or higher. It is possible to satisfactorily sterilize mold, germs, etc. that have propagated on placed articles. Also, since azodicarbonamide itself foams, there is no need to use other transpiration aids, etc., and it is simple and efficient. Also, azodicarbonamide itself transpirations and diffuses to exert a sterilization effect, Sterilization can be performed reliably and extensively.

It is sectional drawing of the water container 9 containing the self-heating apparatus 1 and the hydrothermal reaction liquid W for demonstrating one Embodiment of the hydrolysis exothermic system used for the microbe elimination method of this invention. In Test Example 1, it is a schematic view of a bathroom in which azodicarbonamide is evaporated by the self-heating device 1. 6 is a graph showing a change in heat generation temperature of a heat source used in Test Example 2.

Hereinafter, the sterilization method of the present invention will be described in more detail.
The sterilization method of the present invention is a sterilization method for sterilization using azodicarbonamide, and includes a step of evaporating the azodicarbonamide by heating with a heat source, and the heat source has a maximum heating temperature of 380 ° C. or higher. It is the heat source which becomes.

In the present invention, “sterilization” refers to a decrease in the number of microorganisms such as molds and bacteria that can be grown from an object (for example, indoor ceiling or wall).
In the present invention, the bacteria to be sterilized include bacteria and fungi. Specific examples of bacteria include bacteria of the genus Pseudomonas such as Pseudomonas aeruginosa, Escherichia such as Escherichia coli, bacteria of the genus Bacillus subtilis, Bacillus subtilis, and Bacillus subtilis. And Gram-positive bacteria such as Staphylococcus genus such as Metylobacterium mesophilicum, Staphylococcus aureus, and lactic acid bacteria. Specific examples of fungi include the genus Cladosporium (Cladosporum), such as Cladosporium cladosporioides, and the genus Penicillium (Acergillus sp.), Such as Penicillium citrus, etc. Rhodotorula (Rhodotorula, Rhodotorula, Rhodotorula, Rhodotorula, Rhodotorula, Auridium, Rhodotorula mucilaginosa, etc. Examples thereof include black yeasts such as genus reobasidum and genus Exophiala, genus Forma, genus Candida, genus Saccharomyces, and the like.
In the present invention, the space to be sterilized is not particularly limited, but a sealed space is preferable, for example, in a general house indoors such as a bedroom, living room, kitchen, toilet, bathroom, closet, closet, public bath, etc. It is particularly preferable to use in a space where microorganisms such as molds and bacteria are likely to grow.

Azodicarbonamide is a synthetic chemical substance of yellow-orange crystals at room temperature and has a molecular weight of 116.1.
Azodicarbonamide is a kind of organic foaming agent used in the rubber and plastics industry. When it is thermally decomposed by heating, a foaming action is generated and transpiration occurs to produce a gas, a solid residue, and a sublimate. The decomposition temperature of azodicarbonamide is about 200 ° C., the decomposition temperature and the decomposition rate can be adjusted, the amount of gas generated is large, and the diffusibility is excellent. As azodicarbonamide, a commercially available product or one synthesized by a known method can be used. Examples of commercially available products include “Uniform AZ (trade name)” manufactured by Otsuka Chemical Co., Ltd. and “Cell Microphone (trade name)” manufactured by Sankyo Kasei Co., Ltd.

  The sterilization method of the present invention is a method for satisfactorily sterilizing molds, germs, and the like by heating azodicarbonamide with a predetermined heat source and evaporating it. In the present invention, the azodicarbonamide is evaporated and heated and decomposed by heating the azodicarbonamide with a predetermined heat source, and the decomposed product acts on the cell walls of the cells such as molds and various bacteria to kill the cells. It is guessed.

  The heat source that can be used for heating azodicarbonamide is not particularly limited as long as it is a heat source having a maximum temperature reached by heating of 380 ° C. or higher. In the present invention, the maximum temperature reached by heating refers to the maximum temperature reached by the heat source itself. Examples of the heat source include a heater and a heat generating agent. In the case of direct ignition, an igniting agent may be used as a heat source. Among them, from the viewpoint of easy handling, efficient evaporation of heated azodicarbonamide, and volatility, heating is performed using a hydrothermal system that generates heat using a hydrothermal substance and a hydrothermal reaction liquid as a heat generating agent. It is preferable to do. With a hydrothermal system, many azodicarbonamides can be efficiently evaporated to an adaptation location (eg, indoors, bathrooms, etc.).

The hydrothermal exothermic system mentioned as an example of the heating means of azodicarbonamide is a system that causes hydrothermal exothermic reaction between the hydrothermal exothermic substance and the hydrothermal reaction liquid. The hydrothermal exothermic substance is a substance that self-heats by reaction with the hydrothermal exothermic reaction solution, and examples thereof include calcium oxide (quick lime), calcium carbonate, magnesium chloride, and aluminum chloride. By using one or a combination of two or more of these, it is possible to adjust the maximum temperature reached by the heat source. Furthermore, the temperature duration of 300 ° C. or higher can be adjusted.
Examples of the hydrothermal reaction liquid include water or a liquid obtained by adding various additives to water. Examples of such additives are those that do not hinder the evaporation of azodicarbonamide and those that do not lower the reactivity of water with respect to the exothermic substance, and specifically include organic solvents and liquid stabilizers.

  Moreover, as a heating means of azodicarbonamide other than the above hydrothermal system, for example, a heating wire such as a nichrome wire, a flat plate shape or a ring shape, an electric heating system using a heater using a semiconductor, etc .; iron powder and Mixing an oxidizer such as ammonium chlorate, mixing a metal and a metal oxide or oxidizer having a lower ionization tendency than the metal, a mixture of iron and potassium sulfate, iron sulfate, metal chloride, iron sulfide, etc. Contacting with water or oxygen, contacting a mixture of a metal having a higher ionization tendency than iron and a halide of a metal having a lower ionization tendency than iron with water, contacting a mixture of the metal and bisulfate with water, aluminum and A system that generates heat by an oxidation reaction such as adding water to a mixture of alkali metal nitrates; a metal that contacts a mixture of sodium sulfate and iron carbide with oxygen Using a system like that generates heat by utilizing an oxidation reaction of the compound, a method of heating and the like.

  In the sterilization method of the present invention, the maximum temperature reached by the heat source used for heating the azodicarbonamide is 380 ° C. or higher, preferably 400 ° C. or higher. If it is a heat source with the maximum temperature reached by heating of 380 ° C. or higher, azodicarbonamide can be evaporated so as to obtain a good sterilizing effect.

  In the present invention, at the time of heating, the heat source preferably maintains a temperature of 300 ° C. or higher for at least 120 seconds, more preferably 150 seconds or longer, and further preferably 180 seconds or longer. The heat source preferably maintains a temperature of 320 ° C. or higher for at least 100 seconds, more preferably 130 seconds or longer, and still more preferably 150 seconds or longer. The heat source preferably maintains a temperature of 340 ° C. or higher for at least 70 seconds, more preferably 100 seconds or longer, and still more preferably 120 seconds or longer. Thereby, the disinfection effect can be improved.

The amount of azodicarbonamide used in the sterilization method of the present invention may be set as appropriate depending on the volume of the space to be sterilized, but the azodicarbonamide generally used per 1 m ³ is 0.4-2. 0 g, preferably 0.5 to 1.5 g per m ³ . By setting the amount of azodicarbonamide to be in the above range, a good sterilization effect by azodicarbonamide can be obtained.
That is, a good sterilization effect is obtained by heating 0.4 to 2.0 g of azodicarbonamide per 1 m ^{3 of} space with a heat source having a maximum heating temperature of 380 ° C. or more to evaporate azodicarbonamide. Can do.

A preferred embodiment in the sterilization method of the present invention is an embodiment in which azodicarbonamide is used as an effective component for sterilization.
In the sterilization method of the present invention, any component can be evaporated together with azodicarbonamide as long as the effects of the present invention are exhibited. Examples of components to be evaporated together with azodicarbonamide include fragrances, solvents, deodorants, transpiration aids, stabilizers, insecticides, insect repellents and the like. In particular, the fragrance is preferably vaporized together with azodicarbonamide in order to mask the unique odor during the evaporation of azodicarbonamide and enhance the feeling of use. However, when liquid components such as solvents, including fragrances, are evaporated together with azodicarbonamide, the efficiency of evaporation decreases, so these liquid components may not be evaporated or may be the minimum necessary amount even if evaporated. preferable.

Examples of the fragrances include natural fragrances extracted from various plants and animals, synthetic fragrances synthesized chemically, and blended fragrances made by mixing a large number of these fragrance components.
Fragrances can be found in various literatures, for example, “Perfume and Flavor Materials of Natural Origin”, Steffen Arctander, Allured Pub. Co. (1960), “Encyclopedia of Scents”, edited by Japan Fragrance Association, Asakura Shoten (1989), “Flowers oils and Floral Compounds In Perfumery”, Danute Pajaudis Anonis, Allred Pub. Co. (1993), “Perfume and Flavor Chemicals (aroma chemicals)”, Vols. I and II, Stephen Arctander, Allured Pub. Co. (1994), “Fundamentals of perfumes and incense”, edited by Motoki Nakajima, Sangyo Tosho (1995), “Synthetic perfumes Chemistry and product knowledge”, Motoichi Into, Kagaku Kogyo Nipposha (1996), “Encyclopedia of Scents” The fragrances described in “Encyclopedia”, Mitsatsu Yatakai, Maruzen (2005) and the like can be used. Each of which is incorporated herein by reference. Specific examples of the fragrance are specifically shown below, but are not limited thereto.

Examples of natural perfumes include natural essential oils such as orange oil, lemon oil, lavender oil, lavandin oil, bergamot oil, patchouli oil, cedarwood oil, peppermint oil, thyme oil, clove oil, cinnamon oil, eucalyptus oil, tea tree oil Is mentioned.
Synthetic fragrances include, for example, α-pinene, β-pinene, limonene, p-cymene, terpinolene, α-terpinene, γ-terpinene, α-ferrandolene, myrcene, camphene, osimene and other hydrocarbon terpenes; heptanal, octanal Aldehydes such as decanal, benzaldehyde, salicylaldehyde, phenylacetaldehyde, citronellal, hydroxycitronellal, citral, α-hexylcinnamic aldehyde, lyial, cyclamenaldehyde, rilal, heliotropin, helional, vanillin, ethylvanillin; Formate, methyl acetate, methyl propionate, ethyl isobutyrate, propyl butyrate, isobutyl acetate, isobutyl butyrate, isobutyl isova Rate, ethyl-2-methylvalerate, isoamyl acetate, amylpropionate, allyl hexanoate, ethyl acetoacetate, ethyl heptylate, methyl benzoate, ethyl benzoate, ethyl octylate, benzyl acetate, nonyl acetate, ortho- ter-butylcyclohexyl acetate, linalyl benzoate, ethyl cinnamate, methyl salicylate, hexyl salicylate, hexyl butyrate, menthyl acetate, terpinyl acetate, phenylethyl isobutyrate, methyl jasmonate, methyl dihydrojasmonate, ethylene brushate , Γ-undecalactone, γ-nonyllactone, cyclopentadecanolide, coumarin and other ester lactones; anisole, p-cresylmethi Ethers such as ether, dimethylhydroquinone, methyleugenol, β-naphthol methyl ether, β-naphthol ethyl ether, anethole, diphenyl oxide, rose oxide, galaxolide, ambrox; isopropyl alcohol, cis-3-hexenol, heptanol, 2- Alcohols such as octanol, dimethol, dihydromyrsenol, linalool, benzyl alcohol, citronellol, geraniol, nerol, terpineol, l-menthol, cedrol, thymol, anis alcohol, phenylethyl alcohol, hexanol, etc .; diacetyl, menthone, isimenton, acetophenone , Α- or β-damascon, α- or β-damasenone, α-, β- or γ-ionone, α-, β- or γ-me Luyonone, methyl-β-naphthyl ketone, benzophenone, tentalome, acetyl cedrene, α- or β-isomethylionone, α-, β- or γ-iron, maltol, cis-jasmon, dihydrojasmon, l-carvone, dihydrocarvone, Ketones such as methyl amyl ketone, camphor, 1,8-cineol, allyl amyl glycolate, isopulegol, ligustral, allyl caproate and the like. These fragrances can be used singly or in combination of two or more kinds as a blended fragrance. Furthermore, a fragrance | flavor can also be used as a mixture (fragrance | flavor composition) containing a fragrance | flavor component, a solvent, a fragrance | flavor stabilizer, etc.

  Examples of the solvent include water, ethanol, propanol, benzyl alcohol and other alcohols, ethylene glycol, diethylene glycol, dipropylene glycol, glycerin, 1,3-butanediol and other polyhydric alcohols, ethylene glycol monomethyl ether, ethylene glycol mono Ethyl ether, ethylene glycol monopropyl ether, ethylene glycol monobutyl ether, diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, diethylene glycol monopropyl ether, diethylene glycol monobutyl ether, diethylene glycol monoisobutyl ether, triethylene glycol monobutyl ether, propylene glycol monomethyl ether, propylene glycol Dimethyl ether, dipropylene glycol monomethyl ether, tripropylene glycol monomethyl ether, tripropylene glycol monobutyl ether, propylene glycol monopropyl ether, dipropylene glycol monopropyl ether, propylene glycol monobutyl ether, propylene glycol-tert-butyl ether, dipropylene glycol mono Glycol ethers such as butyl ether, dipropylene glycol dimethyl ether, phenyl carbitol, phenyl cellosolve and benzyl carbitol, paraffins such as liquid paraffin and n-paraffin, esters such as diethyl phthalate, benzyl benzoate, triethyl citrate and isopropyl myristate , Other 3-methyl- - methoxybutanol, N- methylpyrrolidone, propylene carbonate, and the like. These solvents can be used alone or in any combination of two or more. Moreover, it can mix with the said fragrance | flavor component and can also be used as a fragrance | flavor composition.

When the fragrance is transpired into the space together with azodicarbonamide, the fragrance is preferably used so that the transpiration concentration of the fragrance in the space is 1 to 300 mg / m ^3, and becomes 5 to 150 mg / m ^3. It is more preferable to use as described above. When the transpiration | concentration density | concentration of the fragrance | flavor in space is the said range, a disinfection effect can be improved synergistically with azodicarbonamide. Moreover, the unpleasant smell which arises when azodicarbonamide is evaporated can be suppressed, and a use feeling can be improved more.

  Examples of the deodorant include lauryl methacrylate, geranyl chlorinate, catechin, polyphenol, charcoal and the like.

  Examples of the transpiration aid include zinc stearate, aluminum stearate, barium stearate, calcium stearate, zinc oxide, zinc carbonate, calcium carbonate, titanium dioxide, carbon black, antimony trioxide, decabromodiphenylene oxide, anhydrous Examples include merit acid, maleic anhydride, benzotriazole, 4,4′-oxybis (benzenesulfonyl hydrazide), urea and the like.

  Examples of the stabilizer include dibutylhydroxytoluene, butylhydroxyanisole, tocopherol and the like.

Examples of insecticides include natural pyrethrin, pyrethrin, allethrin, phthalthrin, resmethrin, framethrin, permethrin, phenothrin, ciphenothrin, praretrin, transfluthrin, methfluthrin, profluthrin, imiprothrin, empentrin, ethofenprox, and sylfluofen. Insecticides; Carbamate insecticides such as propoxur and carbaryl; Organophosphorus insecticides such as fenitrothion and DDVP; Oxadiazole insecticides such as methoxadiazone; Phenylpyrazole insecticides such as fipronil; Neonicochi such as imidacloprid and dinotefuran Noid insecticides; sulfonamide insecticides such as amidoflumet; pyrrole compounds such as chlorfenapyr; metoprene, hydroprene Insect juvenile hormone-like compounds; anti-juvenile hormone-like compounds such as plecosene; molting hormone-like compounds such as ecdysone; essential oils such as phytoncide, light-loading oil, orange oil, cinnamon oil, and clove oil; 1 type (s) or 2 or more types, such as ammonium salt and a benzyl salicylate, are mentioned.
Among them, pyrethroid insecticides, carbamate insecticides, oxadiazole insecticides and sulfonamide insecticides are preferable in terms of good volatility, and in particular, ciphenothrin, permethrin, methoxadiazone, propoxle, amidoflumet, etofen. Prox is preferred.

  As a pest repellent, 1 type (s) or 2 or more types, such as a diet, di-n-butyl succinate, hydroxyanisole, rotenone, ethyl-butylacetylamino propionate, are mentioned, for example.

  As one aspect of the sterilization method of the present invention, for example, a method using a heat transpiration agent containing azodicarbonamide and heating it with a predetermined heat source to decompose and evaporate azodicarbonamide to sterilize, etc. Is mentioned.

  In this invention, as long as the effect of this invention is show | played in a heat transpiration | evaporation agent, arbitrary components can be contained and it can evaporate with azodicarbonamide. Examples of the component to be evaporated together with azodicarbonamide include the above-mentioned fragrances, solvents, deodorants, transpiration aids, stabilizers, insecticides, insect repellents and the like.

  In addition, when making a heat transpiration agent contain a fragrance | flavor, content of a fragrance | flavor can be adjusted suitably so that it may become a predetermined | prescribed balance. A fragrance | flavor is normally contained in 0.01-20 mass% in a heat | fever transpiration agent, Preferably, 0.1-10 mass% is contained. When a fragrance is contained, if the content is less than 0.01% by mass, sufficient scenting may not be obtained, and if it exceeds 20% by mass, the scent may become too strong. Moreover, in the case of a liquid, it is preferable to contain so that the evaporation efficiency of azodicarbonamide may not be lowered.

  Examples of the dosage form of the heat transpiration agent include granules, powders, fine granules, and liquids. Especially, it is preferable to set it as solid forms, such as a granule, a powder agent, and a fine granule. In order to granulate and dry the heat transpiration agent, the dosage form of the heat transpiration agent can be made into a granule, a powder, a fine granule, etc. by containing a binder, an excipient and the like. When granulating the heat transpiration agent, for example, in the case of a granule, the particle size is preferably about 1 to 5 mm.

Examples of binders used when granulating the heat transpiration agent include celluloses such as carboxymethylcellulose, hydroxymethylcellulose, and hydroxypropylmethylcellulose; starches such as starch and starch; natural polymer compounds such as gum arabic; polyvinyl alcohol 1 type, or 2 or more types, such as synthetic polymer compounds, such as polyvinylpyrrolidone.
What is necessary is just to contain these binders so that it may become 0.5-5 mass% with respect to a heat transpiration agent.

  Examples of the excipient include pearlite, talc, diatomaceous earth, clay, bentonite, and clay mineral which are inorganic porous bodies.

The heat transpiration agent may further contain a disintegration aid, if necessary, for example, organic acid esters such as paraoxybenzoic acid ester, stearic acid ester, ethyl lactate, chlorophenyl salicylate; malic acid, fumaric acid When a disintegration aid such as an organic acid such as tartaric acid, adipic acid, or succinic acid is used, disintegration of the preparation by heating is promoted, and the transpiration and volatilization of the drug can be made smooth.
Further, if necessary, various surfactants, efficacy enhancers, dyes and the like can be contained.

  In addition, in implementing this invention, the example of a prescription of a heat transpiration agent is as Table 1 below.

  Hereinafter, as one aspect of the sterilization method of the present invention, a heating transpiration agent containing azodicarbonamide is heated using a hydrothermal heat generation system, and the sterilization method by evaporating azodicarbonamide will be described. The sterilization method of the present invention is not limited to this.

  As described above, the hydrothermal exothermic system is a system that generates heat using the hydrothermal exothermic substance and the hydrothermal exothermic reaction liquid. A method for heating the heating transpiration agent using the self-heating device 1 and the hydrolysis-exothermic reaction liquid W as shown in FIG. By heating the heat evaporating agent with the self-heating device 1, azodicarbonamide or the like in the heat evaporating agent can be evaporated in the form of smoke. The heating transpiration agent usually contains an organic foaming agent for evaporating the active ingredient, but in the sterilization method of the present invention, the active ingredient azodicarbonamide itself also has a function as an organic foaming agent, By heating the heat evaporating agent, the azodicarbonamide evaporates and other components can be evaporated together.

  As described above, when the above-mentioned heat evaporating agent is heated using the self-heating device 1 to evaporate azodicarbonamide, it is preferable because other components can evaporate together with azodicarbonamide. In the heat transpiration agent, azodicarbonamide is an effective component for sterilization and has a function as a foaming agent. Therefore, it is not necessary to use another foaming agent, which is efficient and preferable.

  A method for evaporating azodicarbonamide by heating the heating transpiration agent 7 containing azodicarbonamide using the self-heating device 1 will be described below. By putting the self-heating device 1 into the container 9 containing the water exothermic reaction liquid W, the water exothermic reaction liquid W flows into the outer container 2 through the water passage hole, permeates the nonwoven fabric sheet 3 and enters the water exothermic substance 8. Contact with. The heat evaporating agent 7 is heated by the reaction heat generated by the contact between the hydrothermal exothermic reaction liquid W and the hydrothermal exothermic substance 8, and the azodicarbonamide evaporates. The hot-melt resin film 6 is melted by heat radiation from the heat-evaporating agent 7 and contact with the heat-evaporating agent evaporated in the self-heating device 1, and the azodicarbonamide is heated and melted. Evaporated and discharged to the outside (indoors, etc.) efficiently through the ventilation holes. As a result, the azodicarbonamide released to the outside diffuses to the application site.

  In such a self-heating device 1, it is preferable to use 1 to 20 times by mass of the hydrothermal exothermic substance with respect to the heating transpiration agent in order to set the maximum temperature reached by heating to 380 ° C. or higher. As a mass, it is preferable to use 1 to 500 g of hydrothermal exothermic substance as a guide for 1 to 50 g of the heat transpiration agent. Furthermore, what is necessary is just to add the liquid for hydrothermal exothermic reaction so that it may become 0.2-2 mass times with respect to the hydrothermal exothermic substance.

  The self-heating device 1 is used as a heat source, and when heating is started after removing the heating transpiration agent 7 from the self-heating device 1, the bottom of the partition member 4 in FIG. 1 (the partition member 4 and the heating transpiration agent). It is only necessary that heating can be performed so that the temperature at which an arbitrary position (for example, a position indicated by X in FIG. 1) is measured is 380 ° C. or higher, preferably 400 ° C. or higher.

  Moreover, it is preferable that the temperature of arbitrary locations in the bottom part of the said partition member 4 (surface where the partition member 4 and the heating transpiration agent 7 contact) will be 300 degreeC or more for at least 120 seconds, and will be 300 degreeC or more for at least 150 seconds. It is more preferable that the temperature is 300 ° C. or higher for at least 180 seconds. The temperature is preferably maintained at a temperature of 320 ° C. or higher for at least 100 seconds, more preferably 130 seconds or longer, and further preferably 150 seconds or longer. The temperature is preferably maintained at a temperature of 340 ° C. or higher for at least 70 seconds, more preferably 100 seconds or longer, and still more preferably 120 seconds or longer. By making the heating conditions as described above, a better sterilization effect can be obtained in the sterilization method of the present invention.

  EXAMPLES Hereinafter, although an Example and a comparative example demonstrate this invention further, this invention is not restrict | limited to the following example at all.

In this test, a heat transpiration agent containing azodicarbonamide was prepared, and the sterilization effect obtained by transpiration of azodicarbonamide by heating the heat transpiration agent using a predetermined hydrothermal system was examined. .
<Test Example 1>
In this test, the self-heating apparatus 1 which is one embodiment of the hydrothermal exothermic system was used to examine the sterilization effect obtained by heating the transpiration agent containing azodicarbonamide and evaporating the azodicarbonamide. .

[Production of heat transpiration agent]
In the blending components shown in Table 2, each component was mixed, granulated, and dried to produce a granular heat transpiration agent 7. The particle size per one heat transpiration agent is about 3 mm, and the length is about 5 mm.

As the blending components in Table 2, the following were used.
Active ingredient: Azodicarbonamide (trade name: Uniform AZ (Otsuka Chemical Co., Ltd.))
Binder: pregelatinized starch

[Production of self-heating device]
<Sample 1>
The self-heating device 1 includes a bottomed cylindrical outer container 2 having a diameter of 53 mm, a height of 63 mm, and a depth of 40 mm, and contains 65 g of calcium oxide as the hydrothermal substance 8. The outer container 2 has a plurality of water holes at the bottom, and the water holes were closed with a non-woven sheet 3 having water permeability. Further, the inside of the outer container 2 was partitioned into two spaces by the partition member 4. The partition member 4 has a cylindrical shape and the bottom portion has a substantially hollow hemispherical shape, and its side wall is arranged concentrically with the peripheral wall of the outer container 2.
The hydrothermal exothermic substance 8 is filled in the space formed by the peripheral wall of the outer container 2, the partition member 4, and the nonwoven fabric sheet 3, and 5 g (azodicarbonamide 4) of the produced heat transpiration agent 7 is contained inside the partition member 4. .9 g) was accommodated. Further, the upper open surface of the outer container 2 is covered with a lid member 5 in which seven openings of 0.8 cm ² are formed in a region corresponding to the upper open surface of the partition member 4, and the opening of the lid member 5 is The self-heating device 1 was manufactured by closing with a hot-melt resin film 6 having a vent hole. The produced self-heating device 1 was used as a sample 1.

<Sample 2>
A self-heating device 1 was prepared in the same manner as the sample 1 except that the amount of calcium oxide as a hydrothermal substance was 37 g. The produced self-heating device 1 was used as a sample 2.
<Sample 3>
The self-heating device 1 was produced in the same manner as the specimen 1 except that the hydrothermal substance was a mixture of 55 g of calcium oxide and 10 g of calcium carbonate. The produced self-heating device 1 was used as a specimen 3.
<Sample 4>
The self-heating device 1 was produced in the same manner as the sample 1 except that a mixture of 29.3 g of the hydrothermal exothermic substance calcium oxide and 5.7 g calcium carbonate was used. The produced self-heating device 1 was used as a specimen 4.

A PDA medium inoculated with black mold was prepared according to the following procedure.
1. A PDA slant medium was prepared in a test tube using 10 mL of PDA (potato dextrose agar medium).
2. Above 1. Inoculated with spores of Cladosporium cladosporoides on the PDA slant culture medium prepared in the above, and the black mold was cultured at 25 ° C. for 4 days.
3. 2. 9 mL of physiological saline and 1 mL of PDB (potato dextrose medium) were added to the slant culture medium in which the black mold was cultured, and a spore solution was prepared by scraping black mold from the medium surface using a platinum loop.
4). 3. above. The spore solution was subjected to gauze filtration, and the filtrate was diluted 10,000 times with physiological saline to obtain an inoculum solution.
5. To the PDA plate medium prepared by using 12 mL of PDA in a sterilized petri dish of φ85 mm (trade name: Full Steri Deep Petri dish sterilized φ90 × 20 manufactured by Actect Co., Ltd.) 100 μL of the bacterial solution prepared in step 1 was inoculated to prepare a test medium.

The self-heating device of any one of specimens 1 to 4 in the bathroom 11 in a sealed space of 4.4 m ³ (1.6 m (vertical) × 1.25 m (horizontal) × 2.2 m (height)) shown in FIG. 1 was installed, and the medium prepared above was installed for each of the ceiling part 13, the wall part 14, and the floor part 15 of the bathroom 11 (location indicated by a black circle (●) in FIG. 2). As a control (untreated), the medium was left outside the bathroom. Table 3 shows the temperature and humidity of the bathroom.
The installation place of the self-heating device 1 was the central part of the floor of the bathroom, and it was heated and evaporated by being immersed in a container 9 containing 22 mL of water (hydrolysis reaction liquid W).
After heating and transpiration, the room was unventilated for 90 minutes, and then the ventilation fan was operated to ventilate the bathroom for 30 minutes.
Thereafter, the medium was collected, and left to stand at 25 ° C. for 4 days to culture black mold.

[Evaluation]
The number of bacteria (colony number) of black mold on the PDA slant medium was counted, and the average value of the number of bacteria (colony number) for each ceiling, wall, and floor of the bathroom was calculated. Moreover, the sterilization rate represented by the following formula was calculated.
Bacterial eradication rate (%) = {1− number of bacteria in each part (number of colonies) / number of bacteria in control (untreated) (number of colonies)} × 100
The above test was performed twice in total, and the calculated number of bacteria (colony number) and the sterilization rate are shown in Table 3 (the number of bacteria and the sterilization rate in Table 3 are the values calculated in the test performed twice in total. Average value).

<Test Example 2>
In this test, the exothermic temperature of the self-heating device (heat sources 1 to 4) obtained by removing the heat evaporating agent from the self-heating device 1 (specimens 1 to 4) produced in Test Example 1 was measured.

[Measurement of heat generation temperature of self-heating device]
Heat generation was started for the self-heating device 1 (heat sources 1 to 4) obtained by removing the heat evaporating agent 7 from the self-heating device 1 (specimens 1 to 4) produced in Test Example 1, and the transition of the heat generation temperature was measured. Specifically, in the hydration exothermic system of FIG. 1, after removing the heat transpiration agent 7, a temperature probe (K-type thermocouple (manufactured by Shin-Tetsu Kogyo Co., Ltd .: sheath thermocouple) φ0.3 mm (MAX 600 ° C.))). Since the temperature probe is linear, the temperature probe was passed through the glass tube, the tip was bent, and the probe was pressed down at the end of the glass tube, so that the temperature probe was closely attached and fixed to the can bottom. Heat generation was started in this state, and the heat generation temperature was measured and recorded over time using MT100 manufactured by Graphtec Corporation. The result is shown in FIG. Table 4 shows the maximum temperature reached by heating, the time for which the temperature of 300 ° C. or higher is continued, the time for which the temperature of 320 ° C. or higher is continued, and the time of continuing the temperature of 340 ° C. or higher. Note that heat sources 1 to 4 in Table 4 and FIG. 3 are obtained by measuring changes in heat generation temperature of the self-heating devices obtained by removing the heat evaporating agent from the water heating system of Samples 1 to 4, respectively. In addition, this test was performed three times for each specimen. The maximum temperature reached in heating in Table 4, the time of continuing the temperature of 300 ° C or higher, the time of continuing the temperature of 320 ° C or higher, and the temperature of 340 ° C or higher The time during which the temperature is continued is an average value of values calculated in a test performed three times for each specimen.

As shown in Tables 3 and 4, in the case of Samples 1 to 3 using the heat sources 1 to 3 having the heat source where the maximum temperature reached by heating is 380 ° C. or higher, compared to the case of Sample 4 using the heat source 4 The disinfection effect was remarkably good. In addition, heat sources 1 to 3 had an exothermic temperature of 300 ° C. or higher for at least 120 seconds.
Moreover, in the sample 3, as a result of using calcium carbonate in addition to calcium oxide as a hydrothermal substance, the maximum temperature reached by heating was slightly lowered, but the time for which the temperature of 300 ° C. or higher was continued was long, and was 300 ° C. or higher. It was found that the duration of temperature also affects the disinfection effect.

DESCRIPTION OF SYMBOLS 1 Self-heating device 2 Outer container 3 Nonwoven fabric sheet 4 Partition member 5 Lid member 6 Hot melt resin film 7 Heating transpiration agent 8 Hydrothermal substance 9 Container W Hydrothermal reaction liquid

Claims (1)

A sterilization method for sterilization using azodicarbonamide as an active ingredient ,
Heating the azodicarbonamide with a heat source to evaporate,
The heat source Ri hydrolytic heating system der which the reached heating maximum temperature is 380 ° C. or higher,
Sterilization wherein that you use azodicarbonamide 0.4~2.0g per space 1 m ³ of the sterilization target.