JP3453292B2 - Smoking agent composition - Google Patents

Description

Detailed Description of the Invention

[0001]

TECHNICAL FIELD OF THE INVENTION

2. Description of the Related Art Hitherto, various fumigants or fumigants containing azodicarbonamide, which are useful as gas generating agents, have been devised. Azodicarbonamide is an organic foaming agent having self-extinguishing property, as is well known.
Even if a part of the preparation is heated by a heat source such as a match flame or an igniter to start the thermal decomposition reaction, it has the property of stopping the thermal decomposition reaction if the supply of heat from the outside is interrupted.

Therefore, the self-combustion continuous smoking agent containing azodicarbonamide generates a relatively large amount of heat due to decomposition of dinitrosopentamethylenetetramine, nitrocellulose, etc., and mainly burns a substance having self-combustion continuity. Used as an agent and mixed with azodicarbonamide as a gas generating agent (Japanese Patent Publication No. 1-28022).
issue). However, since these substances require a considerable amount of the above-mentioned main combustion agent that is dangerous for fire, etc., the manufacturing cost increases due to safety measures in manufacturing, and the above-mentioned main combustion agent is There was a problem such as the odor of smoke gas generated during combustion.

Therefore, the content of the main combustion agent in the smoking agent has been reduced, but problems such as a decrease in diffusibility of the agent and disappearance of the effect of self-combustion itself have occurred.

Further, a smoke composition has been proposed in which self-decomposition continuity is added to azodicarbonamide by adding a pesticide, azodicarbonamide and zinc oxide (Japanese Patent Laid-Open No. 5-294803). ), When commercializing this composition as a smoke agent, further improvement was required in terms of indoor pollution after use. In addition, it was found that the smoke rate greatly depends on the particle size and apparent specific gravity of the smoke agent, and more stable performance was required.

[0005]

SUMMARY OF THE INVENTION In view of the above-mentioned circumstances, the present invention provides a smoking agent containing a combustion agent and azodicarbonamide by reducing the content of the combustion agent, thereby reducing the manufacturing cost and the manufacturing time. It is intended to provide a self-burning continuous smoking agent with improved safety, reduced odor of smoke gas generated during use, excellent drug diffusion, and improved indoor pollution.

[0006]

DISCLOSURE OF THE INVENTION The inventors of the present invention have conducted earnest studies on a self-combustion continuous smoking agent containing a combustion agent and azodicarbonamide. As a result, azodicarbonamide has zinc stearate and stearic acid. By adding an organic or inorganic salt such as magnesium, zinc carbonate or zinc oxide as a decomposition accelerator of azodicarbonamide, the content of the combustor such as nitrocellulose in the smoking agent composition can be reduced to 20% by weight or less. However, it was found that the composition has self-burning continuity, is excellent in diffusibility of a drug, and is improved in terms of indoor pollution after use.

Further, the smoke agent composition of the present invention is 3350.
The particle size is adjusted so that the weight percentage that passes through the sieve of 1 μm and remains on the sieve of 1700 μm is 60% or more, preferably 80% or more, and the apparent specific gravity is 0.6 to 0.8 g / ml. It was found that by doing so, the smoke agent composition has an excellent volatilization rate of the drug into the air and reachability to the gap, and the smoke rate is adjusted to an appropriate smoke speed at which there is no risk of the user smoking. .

That is, the present invention relates to the total weight of the composition,
A smoke agent composition comprising 1 to 20% by weight or less of a combustion agent, 30 to 70% by weight of azodicarbonamide, and a decomposition accelerator of azodicarbonamide. More specifically, the azodicarbonamide decomposition accelerator is one or more decomposition accelerators selected from the group consisting of zinc stearate, magnesium stearate, zinc carbonate and zinc oxide. Agent composition. Furthermore, the particle size is 1700 μm
The smoking agent composition has a weight ratio of 3350 μm of 60% or more and an apparent specific gravity of 0.6 to 0.8 g / ml.

The combustion agent in the present invention may be any as long as it can be generally used as a smoke agent combustion agent. Specifically, nitrocellulose, dinitrosopentamethylenetetramine, oxybisbenzenesulfonyl hydrazide, Examples include nitroguanidine, a composition comprising an oxidizing agent such as potassium chlorate and ammonium nitrate, and a combustible substance such as sugar and wood flour.

Nitrocellulose is particularly preferable as the combustion agent of the present invention.

The azodicarbonamide decomposition accelerator in the present invention is a smoker or fumigant containing a combustion agent and azodicarbonamide, which improves the decomposition rate without lowering the decomposition temperature of azodicarbonamide. Any condition may be satisfied, and specific examples thereof include zinc stearate, magnesium stearate, zinc carbonate, and zinc oxide.

The decomposition accelerators may be used alone or in admixture of two or more.

Since these decomposition accelerators have different degrees of promotion of thermal decomposition, they can be appropriately selected in accordance with their promoting ability, and they are 0.0 to the compounding amount of azodicarbonamide.
It is effective to add 1 to 50% by weight, preferably 0.1 to 20% by weight.

The content of azodicarbonamide in the composition of the present invention is 30 to 70 based on the total weight of the smoke agent composition.
Weight percent is preferred. If the content is less than 30% by weight, the volatilization rate of the drug is low, and if it is significant, the self-decomposition continuity may be impaired. On the other hand, if it exceeds 70% by weight, the amount of decomposed gas generated per unit time becomes too large due to the addition of the decomposition accelerator, and there is a problem in safety during manufacturing and storage.

[0015]

BEST MODE FOR CARRYING OUT THE INVENTION The smoke agent composition of the present invention can be produced, for example, as follows.

Examples of the agents that can be used in the smoke agent composition of the present invention include various agents such as insecticides and bactericides, and mixtures thereof depending on the purpose.

Examples of the above insecticides include permethrin, allethrin, resmethrin, cyphenothrin,
Pyrethroids such as Praresulin and Phenothrin,
Organophosphorus agents such as fenitrothion, dichlorvos (DDVP), diazinon, prothiophos and vitex, and carbamate agents such as propoxur and methoxadiazone can be used.

As the above-mentioned bactericides, bactericides for agricultural chemicals such as isophthalonitrile, procymidone, bailetone and morestan, siabendazole, 3-iodo-2-propynyl butyl carbamate (IPBC), IF-1000 and the like for environmental hygiene A germicide or the like can be used.

The content of the drug in the present invention is preferably 2% by weight or more and 20% by weight or less based on the total weight of the smoke agent composition. Further, the drug is not limited to one kind, and it is possible to contain two or more kinds.

Further, an inorganic mineral substance such as clay, kaolin, talc, diatomaceous earth or the like can be added to the smoke composition of the present invention as a filler.

As a method for molding the smoke agent composition of the present invention, for example, it can be molded as follows.

The components of the composition are weighed out and thoroughly mixed with a kneader or the like, and an appropriate amount of water is added and kneaded. The kneaded product is granulated using a die having a constant area of openings and a pre-extrusion or a lateral extrusion granulator. Further, the granulated product is cut into a certain size with a cutter or the like and dried. At this time, in order to make the granulated product have a constant particle size, the granulated product is passed through a sieve before or after drying to be sized.

[0023] At this time, for example, the granulated product has a particle size of 1
The smoking agent granules having a particle size of 700 μm to 3350 μm have a weight ratio of 60% or more, preferably 80% or more and an apparent specific gravity of 0.6 to 0.8 g / ml. It is possible to obtain a smoking agent composition having an excellent volatilization rate into the air and reachability to a gap, and a smoke rate adjusted to an appropriate smoking speed at which a user is not likely to smoke.

In order to obtain a molded product having such a particle size and an apparent specific gravity, it is possible to appropriately adjust the above-mentioned kneading, granulation and cutting conditions by a cutter or the like.

That is, the apparent specific gravity of the granulated product can be adjusted by appropriately combining the particle size of the granulated product, the rheology of the above kneaded product, and the pressed state during granulation. Further, the rheology of the above kneaded product can be appropriately adjusted by the compounding component, the amount of added water, the kneading time, the kneader performance and the like. The pressurized state during granulation is affected by the porosity of the die and the thickness of the die, in addition to the performance of the granulator.

Further, the granulated product is sized, for example, the granulated product is passed through a 3350 μm sieve to obtain 1700 μm.
It is also possible to adjust the ratio of the weight remaining on the sieve of 60 to be 60% or more.

The igniter used in the smoke agent composition of the present invention may be any igniter that heats a part of the smoke agent composition to generate heat enough to start smoking. It may be one.

The smoking agent composition of the present invention contains a binder such as carboxymethylcellulose, hydroxypropylmethylcellulose, polyvinyl alcohol, starch, etc., a potency enhancer such as piperonyl butoxide, S-421, B, etc.
Antioxidants such as HT and tocopherol, and additives such as fragrances can be appropriately mixed.

[0029]

EXAMPLES The present invention will be described in detail below with reference to examples, but the present invention is not limited to these examples.

Example 1. Manufacturing method of smoking agent granules 60% by weight of azodicarbonamide (hereinafter referred to as AZ),
4% by weight of nitrocellulose (hereinafter referred to as NC), 1% by weight of zinc oxide, 5% by weight of hydroxypropylmethylcellulose (hereinafter referred to as HPMC), 25% by weight of talc and 5% by weight of phenothrin as an active ingredient were respectively weighed and kneaded by a kneader. After thoroughly mixing and stirring, water was added and kneaded, and granulated using a pre-extrusion granulator having a die having an opening with a diameter of 2 mm. Further, the granulated product was cut into a certain size with a cutter and dried to obtain a smoking agent granule of Example 1.

Example 2. Manufacturing method of smoke agent granules AZ 50% by weight, NC 4% by weight, zinc oxide 3% by weight, H
PMC 5% by weight, talc 33% by weight and methoxadiasone 5% by weight as an active ingredient were respectively weighed out, thoroughly mixed and stirred by a kneader, and then kneaded by adding water to pre-extrude a die having an opening with a diameter of 2 mm. Granulated using a granulator. Further, this granulated product was cut into a certain size with a cutter and dried to obtain a smoking agent granule of Example 2.

Comparative Example 1. Manufacturing method of smoking agent granules 60% by weight of AZ, 4% by weight of NC, 5% by weight of HPMC, 26% by weight of talc and 5% by weight of phenothrin as an active ingredient are respectively weighed out, and the same as in Example 1 below.
The smoking agent granules of Comparative Example 1 were obtained.

Comparative Example 2. Manufacturing method of smoking agent granules AZ 50% by weight, NC 4% by weight, HPMC 5% by weight, talc 36% by weight and methoxadiasone 5% by weight as an active ingredient were weighed, respectively, and smoked in Comparative Example 2 in the same manner as in Example 2 below. Smoke powder granules were obtained.

Test Example 1. Smoke State of Smoke Agent Granules 25 g of the smoke agent composition of Examples 1 and 2 and Comparative Examples 1 and 2.
Was charged into a metal container, and smoking was started using an igniter whose heat generating agent was composed of silicon iron and a metal oxide. The smoke test is 6
In the tatami room, whether or not smoke was continuously and quickly observed was visually observed, and the case where smoke was continuously and quickly was regarded as good, and the case where smoke was slow was regarded as bad.

The volatilization rate of the active ingredient was calculated as follows. The sample is smoked in a room with an internal volume of 6380 L, the room air is stirred by a fan, and then about 20 L of room air is passed through a glass tube filled with silica gel for chromatography using a vacuum pump to adsorb the active ingredient on the silica gel. . Next, the active ingredient is eluted and collected with acetone and quantified by gas chromatography, and the amount (A) of the active ingredient in the collected indoor air is determined. On the other hand, the total amount (B) of active ingredients in the sample is determined by gas chromatography. From these values, the volatilization rate is calculated by the following equation 1.

[0036]

[Equation 1]

The results are shown in Table 1.

[0038]

[Table 1]

Example 3. Manufacturing method of smoke agent granules AZ 55% by weight, NC 4% by weight, zinc oxide 1% by weight, H
PMC (5% by weight), talc (30% by weight) and phenothrin (5% by weight) as an active ingredient were weighed and thoroughly mixed and stirred by a kneader, and then water was added and kneaded to obtain a diameter of 2
Granulation was performed using a pre-extrusion granulator with a die having mm openings. Further, the granulated product was cut into a certain size with a cutter and dried to obtain a smoking agent granule of Example 3.

Comparative Example 3. Manufacturing method of smoke agent granules AZ 65% by weight, zinc oxide 6% by weight, HPMC 5% by weight, talc 19% by weight and phenothrin 5% by weight as an active ingredient were weighed out, respectively. The smoker granules were obtained.

Comparative Example 4. Smoke agent granule manufacturing method NC 30% by weight, HPMC 5% by weight, talc 60% by weight
And 5% by weight of phenothrin as an active ingredient was weighed out, and the smoke agent granules of Comparative Example 4 were obtained in the same manner as in Example 3 below.

Comparative Example 5. Manufacturing method of smoking agent granules 60% by weight of AZ, 5% by weight of zinc oxide, 5% by weight of HPMC, 25% by weight of talc and 5% by weight of phenothrin as an active ingredient were respectively weighed, and the same procedure as in Example 3 was carried out. The smoker granules were obtained.

Test Example 2. Indoor Staining of Smoke Agent Granules 25 g of the smoke agent composition of Example 3 and Comparative Examples 3, 4 and 5 was filled in a metal container and smoked using an igniter in which the heat generating agent consisted of silicon iron and a metal oxide. Smoke started. In the smoke test, the interior of the 6 tatami mat was sealed and smoked, the room was ventilated 2 hours later, and the flooring and floor conditions were visually observed. The case where it was not possible was regarded as minor. The results are shown in Table 2.

[0044]

[Table 2]

Test Example 3. Effect of AZ decomposition accelerator Thermal analysis (DTA) was performed on a mixture of 90% by weight of AZ and 10% by weight of the decomposition accelerator shown in Table 3 in a mortar,
The decomposition temperature was measured. Furthermore, as an evaluation of the state of accelerated decomposition, 10 g of the sample was placed on an aluminum foil to start smoking.
It was visually observed whether or not smoking was continued and swift, and the case where it was continued and swift was rated as good, and the case where smoking was slow was rated as bad. As a result, the decomposition temperature of AZ was the same as that of the non-addition group, when any of the decomposition accelerators was added. Table 3 shows the smoke status of each test area.
Shown in.

[0046]

[Table 3]

Test Example 4. Particle size and appearance of smoker granules
Specific gravity and smoking time AZ 60% by weight, NC 3% by weight, zinc oxide 3% by weight, carboxymethyl cellulose 5% by weight, clay 22% by weight
Then, 7% by weight of permethrin as an active ingredient was weighed out, sufficiently mixed and stirred by a kneader, kneaded by adding water, and granulated by using a pre-extrusion granulator of a die having a hole having a diameter of 2 mm. Further, this granulated product was cut into a certain size with a cutter and dried to obtain smoking agent granules of Examples 8 to 12 shown in Table 4. In addition, the particle size distribution was classified by using a sieve of 3350 and 1700 μm, and shown by weight% with respect to the total amount. The apparent specific gravity is 10
The weight of granules that can be filled in a 0 mL container was measured and determined.

25 g of the smoke agent composition shown in Examples 8 to 12
Was charged into a metal container, and smoking was started using an igniter whose heat generating agent was composed of silicon iron and a metal oxide. The time from the start of smoking to the end was measured. The results are shown in Table 4.

[0049]

[Table 4]

[0050]

EFFECTS OF THE INVENTION By using the smoking agent composition of the present invention, the diffusibility of the drug is excellent and the odor of the generated gas is reduced as compared with the conventional one, and the manufacturing cost and the manufacturing time are reduced. It is possible to provide a self-burning continuous smoking agent which is excellent in safety and has improved indoor pollution properties.

Continuation of front page (58) Fields investigated (Int.Cl. ⁷ , DB name) A01N 25/20 101

Claims (4)

(57) [Claims] 1. A smoke containing 1 to 20% by weight or less of a combustor, 30 to 70% by weight of azodicarbonamide, and a decomposition accelerator of azodicarbonamide, based on the total weight of the composition. Agent composition. 2. The smoke composition according to claim 1, wherein the combustor is nitrocellulose. 3. A decomposition accelerator for azodicarbonamide,
The smoke agent composition according to claim 1, which is one or more decomposition accelerators selected from the group consisting of zinc stearate, magnesium stearate, zinc carbonate, and zinc oxide. 4. The smoke agent granule having a particle size of 1700 μm to 3350 μm has a weight ratio of 60% or more and an apparent specific gravity of 0.6 to 0.8 g / ml. The smoke composition described.