JP2014210714A - Smoking agent composition - Google Patents

Abstract

PROBLEM TO BE SOLVED: To provide a smoking agent composition that emits a good fragrance even in a use after storage and transportation, that can suppress the problems such as dusting, coughing or spill from a container, and that has a proper time duration until the start of smoking.SOLUTION: A smoking agent composition is granular and contains a component (A): agent; a component (B): azodicarbonamide; and a component (C): fragrance, characterized in that the grain density is 1.05 to 1.20 g/cm. And also a smoking agent composition is characterized in that the BET specific surface area is 1.1 to 1.4 m/g.

Description

  The present invention relates to a smoke composition.

  For example, granular smoke containing antibacterial, bactericidal, insecticidal and other agents that have antibacterial, bactericidal, insecticidal and other effects in a humid bathroom or room where microorganisms such as bacteria and fungi are likely to propagate It is widely performed to control pests by smoking with an agent composition (for example, Patent Document 1). In the smoke composition, the exothermic base is burned or decomposed to generate gas and smoke particles, so that the chemical is smoked and ejected and diffused in the air in a short time.

In a smoke composition, various fragrance | flavors may be mix | blended for the purpose of improving the effective feeling after use and palatability by use (for example, patent documents 2, 3). However, since the fragrance | flavor mix | blended with the soot agent composition is easy to volatilize or decompose | disassemble with time, as the storage period before use becomes long, the fragrance felt after smoking becomes weak and it is difficult to obtain the effect of the intended fragrance. In addition, the smoke composition may collapse due to storage and transportation, resulting in problems such as powdering, waste, and spillage from containers. In particular, such a problem tends to occur when the smoke composition is stored at a high temperature. Therefore, the smoke agent composition is required to have good fragrance even after high temperature storage and use after transportation, and to be able to sufficiently suppress the occurrence of problems such as powdering, waste, and spilling from the container.
It is also very important that the smoke composition can efficiently smoke and scatter the drug.

JP-A-7-53302 JP-A-11-246306 JP 2011-12051 A

  The present invention has a good scent even after high-temperature storage and use after transportation, can suppress problems such as powdering, waste, spillage from containers, etc., and can smoke and scatter chemicals efficiently A composition is provided.

The smoke agent composition of the present invention is a granular smoke agent composition containing component (A): drug, component (B): azodicarbonamide, and component (C): fragrance, The particle density is 1.05-1.20 g / cm ³ .

The smoke agent composition of the present invention preferably has a BET specific surface area of 1.1 to 1.4 m ² / g.

  The smoke agent composition of the present invention has good fragrance even after high-temperature storage and use after transportation, can suppress problems such as powdering, waste, spillage from containers, etc., and efficiently smoke and scatter chemicals be able to.

It is sectional drawing which showed an example of the soot apparatus using the soot agent composition of this invention.

<Fumigant composition>
The smoke agent composition of the present invention (hereinafter simply referred to as “the smoke agent”) is a granular smoke agent containing the component (A), the component (B), and the component (C) described later. .

[Component (A)]
Ingredient (A) is a drug. The component (A) may be selected according to purposes such as antibacterial, sterilization, and insecticide.
It does not specifically limit as a chemical | medical agent, For example, an antibacterial agent, a disinfectant, a fungicide, an antifungal agent, a deodorant, an insecticide, a repellent, or those mixed agents etc. are mentioned. Specific examples include organic chemicals and silver inorganic antibacterial agents that are widely used for smoke agents.

  Examples of the organic drug include 3-methyl-4-isopropylphenol (IPMP), 3-iodo-2-propargylbutyl carbamate (IPBC), o-phenylphenol (OPP), methoxadiazone, and the like.

Examples of silver-based inorganic antibacterial agents include silver oxides, chlorides, nitrates, sulfates or particulate agents in which silver itself is supported on a carrier.
Examples of the carrier include phosphates (zirconium phosphate, calcium phosphate, etc.), metal oxides (silicon oxide, aluminum oxide, titanium oxide, zinc oxide, iron oxide, zirconium oxide, etc.), inorganic compounds (zeolite, clay). Minerals, silica gel, etc.). The carrier may be one type or two or more types.

As the drug, bactericides, antibacterial agents, fungicides, antifungal agents, and deodorants are preferable, and silver-based inorganic antibacterial agents, IPMP, IPBC, OPP, and methoxadiazone are more preferable.
Component (A) may be one type or two or more types.

  1-30 mass% is preferable and, as for content of the component (A) in the smoke agent (100 mass%) of this invention, 1-20 mass% is more preferable. If content of a component (A) is more than a lower limit, the effect by a component (A) will be fully easy to be acquired. In addition, since the ratio of the component (A) to the component (B) does not become too small, particularly in the case where the component (A) is an organic drug, an excessive amount of heat is added to the component (A) at the time of smoke, so that the component (A ) Is easily suppressed, and the scattering rate of the component (A) becomes better. If content of a component (A) is below an upper limit, it will become easy to formulate a smoke agent to a granular form. Moreover, when content of a component (A) exceeds 30%, the effect by a component (A) will not change so much.

[Component (B)]
Component (B) is azodicarbonamide. Component (B) is an exothermic base and plays a role of ejecting and scattering effective components such as component (A) and component (C). The component (B) is heated and foamed and melted with the component (A) and the component (C), and the component (A) and the component (C) are sufficiently smoked by the action of the pyrolysis gas of the component (B). Is done.

  50-90 mass% is preferable and, as for content of the component (B) in the smoke agent (100 mass%) of this invention, 70-80 mass% is more preferable. If content of a component (B) is more than a lower limit, it will be easy to disperse | distribute an active ingredient efficiently. If content of a component (B) is below an upper limit, the scattering of the powder by the residue after smoking will decrease, and it will be hard to pollute the room etc. which smoke.

[Component (C)]
Ingredient (C) is a fragrance. Component (C) plays a role of improving palatability, effectiveness, etc. by imparting a scent by soot and masking the smoke agent odor during soot.
The fragrance is not particularly limited, and examples thereof include fragrances described in the following documents.
“Perfume and Flavor Chemicals”, Vol. Iand II, Steffen Arctander, Allured Pub. Co. (1994),
"Synthetic fragrance chemistry and product knowledge", Motoichi Into, Chemical Industry Daily (1996),
"Perfume and Flavor Materials of Natural Origin", Steffen Arctander, Allured Pub. Co. (1994),
"Encyclopedia of Scent", Japan Fragrance Association, Asakura Shoten (1989),
"Perfumery Material Performance V.3.3", Boelens Aroma Chemical Information Service (1996),
“Flower oils and Floral Compounds In Perfumery”, Danute Lajaujis Anonis, Allured Pub. Co. (1993), etc.

Perfumes include γ-undecalactone, γ-decalactone, iso-e-super, acetyl cedrene, ambroxan, damascon, hexylcinnamic from the masking effect of odor when smoked and the residual scent after treatment. Aldehydes and coumarins are preferred.
Component (C) may be one type or two or more types.

  0.1-2 mass% is preferable, as for content of the component (C) in the smoke agent (100 mass%) of this invention, 0.3-1 mass% is more preferable, 0.4-0.8 Mass% is particularly preferred. If content of a component (C) is more than a lower limit, the scent of a smoke agent will become favorable even after a preservation | save, and the fragrance after smoke will also become favorable. If content of a component (C) is below an upper limit, it will be easy to provide moderate fragrance by soot. Moreover, the scent of the smoke agent after a preservation | save becomes more stable, and the scattering rate of a component (A) tends to become high.

Moreover, the smoke agent of this invention may contain arbitrary components other than a component (A)-(C) in addition to a component (A)-(C).
Examples of optional components include binders, surfactants, excipients, exothermic aids, stabilizers, efficacy enhancers, and antioxidants.
The optional component may be one type or two or more types.

When a binder is contained in the smoke agent of the present invention, granule formability is improved.
Examples of the binder include celluloses (carboxymethylcellulose, hydroxymethylcellulose, hydroxypropylmethylcellulose, etc.), starch polymer compounds (starch, starch, etc.), natural polymer compounds (arabic gum, etc.), and synthetic polymers. Examples thereof include molecular compounds (polyvinyl alcohol, polyvinyl pyrrolidone, etc.).

  When the smoke agent of this invention contains a binder, as for content of the binder in the smoke agent (100 mass%) of this invention, 3-8 mass% is preferable. If the content of the binder is equal to or higher than the lower limit, the time from installation to the start of smoke can be made longer, and it is easy to prevent the user from smoking at the start of smoke. If the content of the binder is not more than the upper limit value, good smoke performance (jet power) is likely to be obtained.

When the smoke agent of the present invention contains a surfactant, the granule formability is improved and the smoke performance becomes more stable.
Examples of the surfactant include an anionic surfactant, a cationic surfactant, and a nonionic surfactant.

Examples of the anionic surfactant include alkyl benzene sulfonate, polyoxyethylene (POE) -alkyl ether sulfate, α-olefin sulfonate, higher alcohol sulfate, and the like.
Examples of the cationic surfactant include alkyl trimethyl ammonium salt, alkyl dimethyl benzyl ammonium salt, alkyl amine salt and the like.
Examples of the nonionic surfactant include sorbitan fatty acid esters, glycerin fatty acid esters, polyglycerin fatty acids, sucrose fatty acid esters, propylene glycol fatty acid esters, glycerin alkyl ethers, POE-sorbitan fatty acid esters, POE- Examples include glycerin fatty acid esters, POE-propylene glycol fatty acid esters, POE-alkyl ethers, POE / polyoxypropylene (POP) -alkyl ethers, alkanolamides, and the like.

As the surfactant, a fatty acid ester of a polyhydric alcohol or an ethylene oxide adduct thereof is preferable, and sorbitan fatty acid esters, POE-sorbitan fatty acid esters, and glycerin fatty acid esters that are liquid at room temperature are more preferable.
Examples of sorbitan fatty acid esters include monooleate and monolaurate.
Examples of glycerin fatty acid esters include glyceryl monocaprylate.

  When the surfactant is contained in the smoke agent of the present invention, the content of the surfactant in the smoke agent (100 mass) of the present invention is preferably 2 to 10% by mass, and 3 to 8% by mass. More preferred. If the content of the surfactant is not less than the lower limit, it is easy to lengthen the time from installation to the start of smoke, and it is easy to prevent the user from smoking at the start of smoke. If the content of the surfactant is not more than the upper limit value, good smoke performance (jet power) is obtained, and the time until the start of smoke does not become too long.

Examples of the excipient include inorganic mineral substances (clay, kaolin, talc, diatomaceous earth, etc.) and the like.
When the smoke agent of the present invention contains an excipient, the content of the excipient in the smoke agent (100 mass) of the present invention is preferably 2 to 45% by mass, and 10 to 30% by mass. More preferred. When the content of the excipient is at least the lower limit value, the granule formability is improved and the smoke performance is more stable. If the content of the excipient is not more than the upper limit value, sufficient smoke performance (jet power) can be easily obtained.

Examples of exothermic aids include zinc oxide and melamine.
Examples of the stabilizer include dibutylhydroxytoluene, butylhydroxyanisole, propyl gallate, epoxy compounds (epoxidized soybean oil, epoxidized linseed oil, etc.) and the like.
Examples of the potentiating agent include piperonyl butoxide, S-421 and the like.
Examples of the antioxidant include dibutylhydroxytoluene (BHT) and tocopherol.

The particle density of the smoke agent of the present invention is 1.05-1.20 g / cm ³ . When the particle density is 1.05 g / cm ³ or more, it is difficult for the smoke agent to collapse even during high-temperature storage or transportation, and it is possible to suppress problems such as dusting, waste, and spillage during use. In addition, since the fragrance is less likely to be scattered during high temperature storage or transportation, a good scent can be realized even after smoke storage after high temperature storage or transportation. In addition, when the particle density is 1.20 g / cm ³ or less, the fragrance is efficiently scattered during smoke so that a good fragrance is realized, the smoke agent is not easily overheated, and the fragrance is hardly changed. .
The particle density of the smoke agent of the present invention is preferably 1.10 to 1.20 g / cm ³ .
The particle density of the smoke agent is measured by the method described in the examples. The particle density of the smoke agent can be controlled by adjusting the mixing conditions, granulation conditions, cutting conditions and the like of each component as will be described later.

1.1-1.4 m < ² > / g is preferable and, as for the BET specific surface area of the smoke agent of this invention, 1.2-1.3 m < ² > / g is more preferable. If the BET specific surface area is equal to or more than the lower limit value, the fragrance is likely to be scattered at the time of smoke, and the scent after smoke is better. If the BET specific surface area is less than or equal to the upper limit value, the fragrance is less likely to be scattered during high-temperature storage or transportation, and good scenting can be easily achieved even after high-temperature storage or after transportation.
The BET specific surface area of the smoke agent is measured by the method described in the examples. The BET specific surface area of the smoke smoke agent can be controlled by the component (B), the components used such as the surfactant and the binder, the amount of added water, and the pressurized state during granulation.

  The shape of the smoke agent of the present invention is not particularly limited, and a columnar shape is preferable. When the smoke agent of the present invention is cylindrical, it is easy to suppress problems such as powdering, waste, spillage, etc. even during high-temperature storage or use after transportation, and the diameter is 1. It is preferably 5 to 2.5 mm and a length of 5 to 10 mm.

Because smoke agents produce an effect by generating a large amount of smoke, it is important to control the time from installation to the start of smoke so that the user does not suffer from smoke at the start of smoke It is.
The time from the installation to the start of smoke in the soot agent of the present invention, that is, the time from the installation to the start of smoke generation is preferably 20 seconds or more, and more preferably 25 seconds or more.

[Production method]
The method for producing the smoke agent of the present invention in the form of granules can adopt a known production method according to the target shape, for example, extrusion granulation method, compression granulation method, stirring granulation method, rolling rolling Examples thereof include a granulation method and a fluidized bed granulation method.

Specific examples of the extrusion granulation method include the following methods.
Components (A) to (C) and optional components to be used as necessary are mixed by a kneader or the like, further mixed with an appropriate amount of water, and the resulting mixture is formed into a die having a certain area of pores. Granulate with the pre-extrusion or transverse extrusion granulator used. Thereafter, the granulated product is cut into a certain size using a cutter or the like, and then dried in a dryer to obtain a smoke agent.

The particle density of the smoke agent can be controlled by adjusting the mixing conditions, granulation conditions, cutting conditions and the like of each component. That is, the particle density of the smoke agent can be controlled by appropriately combining the rheology of the mixture and the pressure state during granulation.
The rheology of the mixture can be appropriately adjusted depending on the blending component, the amount of added water, kneading time, kneader performance, and the like.

The pressure state at the time of granulation can be adjusted as appropriate depending on the die opening diameter, the die opening rate, and the die thickness, in addition to the granulator performance.
The die opening diameter is preferably 1.5 to 2.5 mm.
The die opening rate is preferably 25 to 40% from the viewpoint that a smoke agent having the above particle density can be easily obtained.

[how to use]
A publicly known method can be adopted for the smoke method using the smoke agent of the present invention. For example, the method of accommodating the smoke agent of this invention in containers, such as a metal container and a ceramic container, and smoking by heating a smoke agent directly or indirectly is mentioned.
The method of heating the smoke agent is preferably a method of heating indirectly. By indirectly heating the soot agent, it is easier to reduce indoor pollution due to the burning residue of the soot agent than directly heating it.

As a method of indirectly heating the smoke agent, any method can be used as long as it can supply heat energy to the smoke agent to a temperature at which the component (B) can be thermally decomposed without burning the smoke agent. A publicly known heating method that is usually used in the soot method can be employed.
Specifically, for example, a method (i) in which a substance that generates heat upon contact with water is brought into contact with water and the smoke agent is heated using the reaction heat, iron powder and an oxidizing agent (such as ammonium chlorate) (Ii), etc., using a heat generated by an oxidation reaction by mixing with a metal oxide or an oxidation reaction by mixing a metal and a metal oxide or oxidant having a lower ionization tendency than the metal (ii), etc. Is mentioned. Of these, method (i) is preferred from the viewpoint of practicality.

  Examples of substances that generate heat upon contact with water include calcium oxide, magnesium chloride, aluminum chloride, calcium chloride, and iron chloride. Among these, calcium oxide is preferable as a substance that generates heat upon contact with water from the viewpoint of practicality.

The use amount of the smoke agent of the present invention may be appropriately set according to the volume of the space where the smoke treatment is performed, and is preferably 0.1 to 2.4 g, more preferably 0.4 to 2.0 g per 1 m ^3. .

Hereinafter, the smoke method using the smoke device 10 illustrated in FIG. 1 will be described as an example of the smoke method using the smoke agent of the present invention.
As shown in FIG. 1, the smoke device 10 is schematically configured by a housing 12, a heating unit 20 provided in the housing 12, and a smoke agent unit 32 provided in the housing 12. Has been. The housing 12 includes a substantially cylindrical main body 14, a bottom portion 16, and a lid portion 18 provided on the upper portion of the main body 14. A smoke agent container 30 is provided in the housing 12, and the smoke agent container 30 is filled with the smoke agent to form a smoke agent part 32.

The lid portion 18 has a through hole, and examples thereof include a mesh, a punching metal, and a lattice frame. Examples of the material of the lid portion 18 include metals and ceramics.
The material of the main body 14 is the same as that of the lid 18.

  The smoke agent container 30 functions as a container that fills the smoke agent part 32 and also functions as a heat transfer part that transmits the thermal energy generated in the heating part 20 to the smoke agent part 32. Examples of the smoke agent container 30 include a metal container.

  The heating unit 20 is not particularly limited, and can be appropriately determined in consideration of the amount of heat necessary for the smoke agent unit 32 to smoke. The heating unit 20 is preferably formed by filling a substance that generates heat upon contact with water, and is particularly preferably formed by filling calcium oxide. The heating unit 20 may be formed by partitioning and filling iron powder and an oxidant with a partition material, and partitioning a metal and a metal oxide or oxidant having a smaller ionization tendency than the metal with a partition material. It may be formed by filling.

  What is necessary is just to determine the bottom part 16 according to the mechanism of the heating part 20 suitably. For example, when the heating unit 20 is made of a substance (calcium oxide or the like) that generates heat upon contact with water, a nonwoven fabric or a metal mesh can be used for the bottom 16. By making the bottom part 16 into a nonwoven fabric or a metal mesh, water can penetrate into the heating part 20 from the bottom part 16 to generate reaction heat, thereby heating the smoke agent.

  In the smoke method using the smoke device 10, the smoke device 10 is first installed in the target space. Next, the heating unit 20 generates heat according to the mechanism of the heating unit 20. For example, when the heating part 20 filled with calcium oxide is provided, the bottom part 16 is immersed in water. When the heating unit 20 generates heat, the smoke agent part 32 is heated via the smoke agent container 30. As for the smoke agent of the heated smoke agent part 32, gas arises by decomposition | disassembly of a component (B), a component (A) and a component (C) smoke with this gas, and pass the through-hole of the cover part 18. Scatter. Thereby, a component (A) and a component (C) are spread | diffused in object space, and a microorganisms suppression effect, a deodorizing effect, etc. are acquired.

  The smoke agent of the present invention described above has a particle density controlled within a specific range, so that it is difficult to collapse even during high-temperature storage or transportation, and the perfume is prevented from being scattered before use. When smoked, the active ingredient is efficiently scattered by the rapid decomposition of the component (B). Therefore, even if the smoke agent of the present invention is stored at a high temperature or after transportation, the effect of the drug can be sufficiently obtained, and a good scent can be realized. In addition, since the smoke agent of the present invention is not easily broken during storage and transportation, occurrence of problems such as powdering, waste, and spillage from containers is suppressed during use.

EXAMPLES Hereinafter, although an Example demonstrates this invention in detail, this invention is not limited by the following description.
[Raw materials]
[Component (A)]
A-1: Silver-supported zeolite-based inorganic antibacterial agent (trade name “Zeomic AJ10N”, manufactured by Sinanen Zeomic Co., Ltd.).
A-2: Metoxadiazone (trade name “Elemic”, manufactured by Sumitomo Chemical Co., Ltd.).
A-3: IPMP.

[Component (B)]
B-1: Azodicarbonamide (trade name “Daiblow AC.2040 (C)”, manufactured by Dainichi Seika Kogyo Co., Ltd.).

[Component (C)]
C-1: A fragrance having the composition shown in Table 1.

[Optional ingredients]
D-1: Hydroxypropyl methylcellulose (trade name “Metroze 60SH-50”, manufactured by Shin-Etsu Chemical Co., Ltd.).
D-2: Sorbitan fatty acid esters (monooleate) (trade name “Emazol O-10V”, manufactured by Kao Corporation).
D-3: Clay (trade name “MK-300”, manufactured by Showa KDE Co., Ltd.).

[Particle density]
2 g of the smoke agent was immersed in 20 mL of water placed in a graduated cylinder, the volume of the excluded water was measured, and the particle density of the smoke agent was calculated by the following equation (1).
Particle density (g / cm ³ ) = smoke mass (g) / volume of water excluded (cm ³ ) (1)

[BET specific surface area]
The BET specific surface area of the smoke agent was measured by a BET one-point method based on the amount of nitrogen adsorption using a rapid surface area measuring device SA-1000 (manufactured by Shibata Kagaku Kogyo Co., Ltd.).

[Evaluation of storage stability]
[(1) Evaluation of fragrance]
Prepare a container of the container “Barusan starting with water (for 6-8 tatami mats)” (trade name, manufactured by Lion Co., Ltd.), put 5 g of the smoke agent in each case into the smoke agent container in the container, and cover the lid. And it preserve | saved for one month at 50 degreeC, and the 50 degreeC preservation | save goods were obtained. Similarly, a 20 ° C. storage product stored for 1 month at 20 ° C. was also prepared. Then, the lid of each container was opened, and the fragrance of the 50 ° C. stored product was evaluated based on the fragrance of the 20 ° C. stored product.
(Double-circle): The fragrance of a 50 degreeC preservation | save goods is not different from a 20 degreeC preservation | save goods.
○: The fragrance of the 50 ° C. stored product is slightly weaker than that of the 20 ° C. stored product, but there is no problem.
(Triangle | delta): The fragrance of a 50 degreeC preservation | save goods is quite weak compared with a 20 degreeC preservation | save goods.
X: The fragrance of a 50 degreeC preservation goods is hardly felt compared with a 20 degreeC preservation goods.

[(2) Evaluation of powder standing when opening)
The 50 ° C. stored product obtained in the same manner as in the evaluation of (1) fragrance was opened immediately after shaking 10 times up and down, and the degree of powder formation (musiness) was evaluated according to the following criteria.
(Double-circle): It does not feel a waste and cannot confirm powdering at all.
○: I don't feel any mess and I don't know how to stand up unless I look closely.
(Triangle | delta): Although a feeling does not feel, powdering can be confirmed visually.
X: The dusting can be clearly confirmed visually and feels ugly.

[(3) Evaluation of fragrance after smoke]
Prepare a container of “Barusan starting with water (for 6-8 tatami mats)” (trade name, manufactured by Lion Co., Ltd.), and store 5 g of the smoke agent of each example in the smoke agent container in the container, 37 g of calcium oxide was accommodated in the heating agent accommodating part in the container, and after producing a smoke device similar to the smoke device 10 of FIG. 1, it was covered and stored at 50 ° C. for 1 month.
Next, a plastic container for water supply containing 23 mL of water is installed in the center of a test room measuring 3.42 m long, 3.82 m wide and 2.40 m high, and the smoke device is placed in the plastic container. And started smoke. Smoke was conducted with the test chamber sealed. Two hours after the start of smoke, the scent after smoke was evaluated according to the following criteria.
A: The scent of the added fragrance is clearly felt.
○: The fragrance of the added fragrance is felt without any problem.
(Triangle | delta): The fragrance of the added fragrance | flavor is felt slightly.
X: The fragrance of the added fragrance | flavor is hardly felt.

[(4) Evaluation of active ingredient scattering rate]
(In the case of component (A-1))
100 mg of the smoke agent of each example was put in an aluminum cup, and the aluminum cup was placed on a hot plate set at 350 ° C. and smoked by heating. Collect all the residue remaining in the aluminum cup after smoking, elute the component (A) from the residue with 5% by weight dilute nitric acid, quantify by ICP emission analysis, and leave the component (A ). Moreover, the quantity of the component (A) in 100 mg of smoke agents which did not smoke was also quantified similarly, and the active ingredient scattering rate was computed by the following Formula (2).
Effective ingredient scattering rate (%) = [(amount of component (A) in 100 mg of smoke agent) − (amount of component (A) in residue after smoke)] ÷ (component in 100 mg of smoke agent ( A) Amount) × 100 (2)
Evaluation of the active ingredient scattering rate was performed according to the following criteria.
A: The active ingredient scattering rate is 70% or more.
A: The active ingredient scattering rate is 50% or more and less than 70%.
X: The active ingredient scattering rate is less than 50%.

(In the case of component (A-2) and component (A-3))
100 mg of the smoke smoke agent of each example was put in an aluminum cup, the aluminum cup was placed on a hot plate set at 350 ° C., and the smoke was heated and smoked in a room with an internal volume of 6380 L. After stirring the room air with a fan, about 20 L of room air was passed through a glass tube filled with silica gel for chromatography using a vacuum pump, and the smoked component (A) was adsorbed onto the silica gel. Next, the component (A) adsorbed on the silica gel was eluted and collected with acetone, and quantified by gas chromatography. Further, the component (A) was eluted and collected from 100 mg of the smoke agent not smoked with acetone, quantified by gas chromatography, and the effective component scattering rate was calculated by the following equation (3).
Effective component scattering rate (%) = (Amount of component (A) in collected indoor air) ÷ (Amount of component (A) in 100 mg of smoke agent) × 100 (3)
Evaluation of the effective component scattering rate was performed in the same manner as in the case of the component (A-1).

[(5) Evaluation of time to start smoke]
Prepare a container of “Barusan starting with water (for 6-8 tatami mats)” (trade name, manufactured by Lion Co., Ltd.), and store 5 g of the smoke agent of each example in the smoke agent container in the container, Calcium oxide 37g was accommodated in the heating agent accommodating part in a container, and the smoke device similar to the smoke device 10 of FIG. 1 was produced.
Next, a plastic container for water supply containing 23 mL of water was installed, the smoke device was placed in the plastic container, and smoke was started. The time from when the smoke device was put into the plastic container until the smoke began to come out vigorously from the smoke device was visually measured as “time to start smoke (seconds)”. Considering the possibility of smoke from the installation of the smoke device until leaving the site, the “time to start smoke (seconds)” was evaluated according to the following criteria.
(Double-circle): Time until smoke start is 25 seconds or more.
○: Time until the start of smoke is 20 seconds or more and less than 25 seconds.
X: Time until the start of smoking is less than 20 seconds.

[Manufacture of smoke agents]
[Examples 1 to 13, Comparative Examples 1 and 2]
After stirring and mixing with a kneader (S5-2G type, manufactured by Moriyama Co., Ltd.) so that each component has the composition shown in Table 2 at room temperature (20 ° C.), 10 parts by mass with respect to 100 parts by mass as a whole Was added and mixed to obtain a mixture. The resulting mixture was granulated using a die pre-extrusion granulator (EXK-1, manufactured by Fuji Powder Co., Ltd.) having an opening having a diameter of 2 mm, to obtain a granulated product. The obtained granulated material was cut into a length of 5 to 10 mm by a flash mill (FL300, manufactured by Fuji Paudal Co., Ltd.), and then dried by a dryer (RT-120HL, manufactured by Alp Co., Ltd.) set at 70 ° C. The drying time was adjusted so that the moisture content described in (1) was obtained, and a granular smoke was obtained. Various evaluation tests were performed on the obtained smoke agent.
In the pre-extrusion granulator, the particle density of the smoke agent is adjusted by adjusting the extrusion speed (number of rotations) in the range of 10-20 rpm and adjusting the die opening rate in the range of 25-45%. did.

As shown in Table 2, in the smoke agents of Examples 1 to 13 containing the components (A) to (C) and having a particle density of 1.05 to 1.20 g / cm ³ , (1) fragrance Evaluation of (2) Evaluation of powder formation at opening (Muse), (3) Evaluation of scent after smoke, (4) Evaluation of active ingredient scattering rate, and (5) Evaluation of smoke start time Both were good.
On the other hand, in the smoke agent of Comparative Example 1 having a particle density of less than 1.05 g / cm ³ , the smoke agent is apt to collapse, so there is powdering and mess when opening after shaking, and fragrance is insufficient. And the time to start smoking was short.
In addition, in the smoke agent of Comparative Example 2 having a particle density of more than 1.20 g / cm ³ , the smoke agent is difficult to collapse more than necessary, so that the active ingredient scattering rate by smoke is low, and the scent after smoke is emitted. Was insufficient.

DESCRIPTION OF SYMBOLS 10 Smoke apparatus 12 Case 14 Main body 16 Bottom part 18 Lid part 20 Heating part 30 Smoke agent container 32 Smoke agent part

Claims (2)

A granular smoke agent composition containing component (A): drug, component (B): azodicarbonamide, and component (C): fragrance,
A smoke agent composition having a particle density of 1.05-1.20 g / cm ³ . The smoke agent composition of Claim 1 whose BET specific surface area is 1.1-1.4m < ² > / g.

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