JP3011318B2 - Method for producing flaky insect repellent composition - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for producing an insect repellent composition comprising paradichlorobenzene as a main component. More particularly, the present invention relates to a production method capable of obtaining a solid of an insect repellent composition in a flake form.

[0002]

2. Description of the Related Art Conventionally, solid paradicrolbenzene preparations have been used as the most powerful insect repellents for clothing and the like. Recently, however, improved compositions of this paradichlorobenzene preparation have been developed. . An example is an insect repellent composition disclosed in JP-A-6-199605.

[0003] The insect repellent composition disclosed herein is characterized in that a natural plant essential oil or an extracted component thereof is contained in paradichlorobenzene in a molten state. According to such an improved insect repellent composition, is contained held with natural plant essential oils, etc., uniform and stable in parametric dichlorobenzene solid, also at the time of use, with the sublimation of Parajikurorubenzen natural Vegetable essential oils etc. are also volatilized at the same time to produce a mixed gas thereof. According to this mixed gas, the enhanced insect repellent action is continuously exhibited as compared with that of the single agent of solid paradichlorobenzene, and the irritating odor peculiar to the sublimation gas of paradichlorobenzene is attenuated. The effect is exhibited.

According to the conventional method for producing such an improved insect repellent composition, according to the above-mentioned patent publication, a mixed liquid of paradichlorobenzene and an essential oil of a natural plant is used as a container in the first method. In the second method, the mixed molten liquid is cooled in a fixed mold to obtain a fixed solid, and in the third method, In this method, the molten mixture obtained in the above method was directly poured into ice water to be cooled and solidified, and then dehydrated and dried.

[0005]

In the above-mentioned conventional insect repellent composition, since the cooled solid is obtained as a lump in the first method, it is necessary to prepare the lump as an insect repellent. This was done by crushing the material to make it finer, or by further pulverizing it and compressing it. However, this method has the disadvantages that the production process is complicated, requires a long time, and that the contained natural plant essential oil and the like excessively flow out during crushing or pulverization.

In the second method, it is necessary to maintain a high temperature state of the mixed melt for a long time,
In addition, in order to efficiently obtain a large amount of preparations, a large number of molds are required, so that the equipment configuration becomes large.In addition, since the process of pouring the mixed melt into the mold is included, production efficiency is reduced. There is a disadvantage that it is relatively low.

The third method has the advantage that the cooled solid can be obtained in the form of crystalline powder. However, since the cooling process is carried out in water, dehydration and drying steps are required, and the production of the same is difficult. It has the drawback that it requires time, and the dry solid obtained has the drawback that the water content is relatively high. This dehydration is relatively difficult.

Accordingly, in the present invention, an insect repellent composition comprising paradichlorobenzene as a main component and containing essential plant essential oils and the like is provided.
A method for manufacturing, cooling solid was obtained in an easy flake form formulated, moreover aimed at providing a way Ru can according to further than simplified process under anhydrous conditions.

[0009]

In order to achieve the above-mentioned object, the present invention relates to a method for producing a flaky insect repellent composition, comprising the steps of: mixing paradichlorobenzene with a natural vegetable essential oil or an extract component thereof; From 60 ° C to 100 ° C
A step of obtaining a mixture in a temperature state and, while stirring the mixed melt , a temperature of not less than ice temperature and not more than 25 ° C.
And a cooling step by quenching under rapid temperature conditions .

[0010] In this production method, the above-mentioned mixed melt is prepared by preliminarily mixing paradichlorobenzene crystals and natural vegetable essential oils, and heating the mixture to a temperature higher than the melting temperature of paradichlorobenzene while stirring. By
Alternatively, it can be obtained by preliminarily heating only the crystal of paradichlorobenzene to a temperature higher than its melting temperature and pouring and mixing a natural vegetable essential oil or the like into the melt.

The mixed melt is kept at a temperature of 60 ° C. to 100 ° C., preferably at a temperature of 60 ° C. to 80 ° C., in particular, in order to reduce the adverse effects of volatilization and disappearance of natural vegetable essential oils.
In order to stabilize the molten state, the temperature is preferably about 65 ° C. If this temperature is lower than 60 ° C., paradichlorobenzene is not sufficiently melted, and a uniform mixed state of each component cannot be obtained. On the other hand, if this temperature exceeds 100 ° C., the volatilization amount of the natural vegetable essential oil and the like becomes inconceivable, and the required amount cannot be mixed.

[0012] The heating method for obtaining the mixed melt can be, for example, a means for continuously applying the calorific value of the hot water heated to a certain appropriate temperature to the above-mentioned respective component materials via the receivers contained therein. .

In the above-mentioned cooling step, the quenching treatment can be carried out by means for continuously applying the cooling temperature of a certain temperature to the above-mentioned mixed molten liquid via a receiver contained therein. In this case, the temperature of the cold water is 25 ° C.
If the ratio exceeds 3, the solidification efficiency of the mixed melt becomes poor, and a flake-like solid having a uniform size cannot be obtained. As for the lower limit, it is sufficient if the temperature is higher than the ice temperature, but it is not economical to lower the water temperature more than necessary.

This cooling step is performed while stirring the mixture. It is desirable that the stirring be performed so as to always cover the whole of the mixture. This agitation can be performed, for example, in such a manner that the receiver containing the mixture is inclined. In this case, the stirring efficiency is increased.

In the above-mentioned method of the present invention, thyme white oil and lemongrass, which are used as natural plant essential oils, when used in a state of being contained in solid paradichlorobenzene, have an effect of enhancing insect repellency. Various things such as oil, cassia oil, Pimento oil, Hinoki oil, Hiba oil are included. In addition, the extracted components of the natural plant essential oils include components such as citral, cinnamic aldecht, thymol, and eugenol, which have the same effect of enhancing insect repellency as described above.

In this case, the blending ratio of the natural plant essential oil or its extracted component to the whole raw material is 0.1% by weight or less.
It is in the range of 5% by weight. In this case, depending on the kind of the natural plant essential oil, etc., if the compounding amount is less than 0.1% by weight, an effective enhancing effect of insect repellent effect cannot be obtained, and if the compounding amount exceeds 5% by weight, The amount of the essential oil leached onto the solid surface of the preparation becomes excessive.

Further, in the production method of the present invention, in addition to the above-described natural plant essential oil or its extracted component, a mixture further containing a fragrance can be used as a raw material. Examples of the flavor include natural flavors of aromatic components such as bouquet, jasmine, floral, and citrus, as well as various compounded flavors.

In this case, the amount of the fragrance is preferably 0.01% by weight to 0.5% by weight based on the whole raw material of the insect repellent composition, which is preferable for stably exhibiting the effect of the fragrance. Is an amount ranging from 0.1% to 0.3% by weight. When the amount is less than 0.01% by weight,
If an effective fragrance effect is not obtained, and if it exceeds 0.5% by weight, fragrance performance becomes excessive and uneconomical, and the insect repellent effect is reduced.

The flake of the solidified product obtained by the production method of the present invention described above, one side has the shape of a rectangular shape like the shape of 1 mm to 3 mm, and breathable within the enclosure remains in flake form In addition to being usable in a state, the flakes can be used as they are, or they can be further powdered to form tablets, or can be formulated as existing dosage forms such as granules.

[0020]

In the present invention, the following effects are produced.
In the step of obtaining the mixed melt, the natural vegetable essential oil or an extract component thereof is uniformly mixed with stirring in a paradichlorobenzene melt.

Next, the temperature between 60 ° C. and 100 ° C.
The cooling process for the mixed melt in the
The temperature of the ice to 25 ° C
The cooling and solidification in the form of flakes can be obtained by performing the quenching under the rapid cooling condition .

During the cooling process, the mixed solution is under agitation, and thus, in the obtained flake-like solidified product, the natural vegetable essential oil or its extracted component is uniformly dispersed in the crystalline solid of paradichlorobenzene. It is contained and retained in a state. This holding state is the same even when the fragrance is contained as a component.

Therefore, at the time of use, the above-mentioned flake-like solidified product is allowed to undergo sublimation of paradichlorobenzene at room temperature,
The natural plant essential oil or its extracted components are also volatilized at the same time, and a mixed gas of these two components is diffused around. As a result, effects such as enhancing the insect repellent effect and attenuating the pungent odor from paradichlorobenzene are produced.

When a fragrance is contained as a component, a volatile gas of the fragrance is included in the mixed gas at the time of use, and this has a sufficient deodorizing action against pungent odor from paradichlorobenzene and It also has a deodorizing effect on the aroma of the natural plant essential oil or its extracted component, and as a whole, produces an aroma effect peculiar to the perfume.

[0025]

【Example】

(Example 1) 100 kg of p-dichlorobenzene crystal powder was fed into a kettle (150 liter capacity) having a double-walled side wall that formed a gap through which water could pass, and 0.5 kg of lemongrass oil was poured into this. Then, this was stirred and mixed by a stirrer provided in the above-mentioned kettle. During the stirring, warm water of about 65 ° C. was continuously passed through the gap of the kettle to obtain a mixed melt of the above components.

Next, with the above-described stirring state, the water was passed continuously while maintaining the temperature of the kettle at about 20 ° C. by lowering the water passing temperature. As a result, a flake-like cooled solidified product was obtained after about 30 minutes.

8 g of the cooled solidified product (formulation A) was mixed with a non-woven material (60 μm thick) and a polypropylene film material (40 μm thick).
Thick) and stored in a wrapper made of laminate material,
Also, the cooled solidified product is tableted in the form of flakes,
g / tablet (formulation B), and the cooled solidified product was pulverized to a particle size of 10 mesh to obtain a 4 g / tablet tablet (formulation C). Two were stored in the same wrapper as above. This cooled solidified product was formed into a sphere (formulation D), and 8 g of the product was stored in a wrapper similar to that described above to produce a product.

Using the products of each of the above-mentioned preparations as samples, the following tests were conducted at room temperature (about 25 ° C.) and at an average humidity of 60%. First, the initial weight of a 30 × 30 mm wool muslin was measured, and five whales (20 days old, 10 samples) were released as test insects on the surface of the wool muslin, and wrapped in a wire net. Samples were used.

Also, a storage case (50 l capacity) made of cardboard paper was prepared, and the above-mentioned samples were dispersed and arranged in three equal positions in the storage case. The storage case was closed with a lid and left as it was for one week. . Next, the lid of the storage case was opened, and one of the test materials described above was placed inside the specimen and closed with the lid. One week after the arrangement, the test material was taken out, the state of damage to the wool muslin was observed, and data was taken one week later. Next, the storage case was left for one week with the lid closed, then the lid was opened, a new one of the test materials was placed, and the lid was closed. One week after the arrangement, the test material was taken out, the state of damage to the wool muslin was observed, and the data was obtained three weeks later. Data after 5 weeks were obtained in the same manner as above.

Further, two tablets of 4 g / tablet consisting only of paradichlorobenzene were stored in the same zipper as the above, and used as a control sample. The same test as above was performed by using 10 packs of this control sample as control (1) and using 3 packs of this control sample as control (2).
Weekly, three-week, and five-week-old food damage status data were obtained.

Based on the data on the state of damage for each product sample and each control sample obtained in this way and the data on the state of damage caused by the control when no insecticide is used, the following formula is used. Table 1 below shows the calculated rate of food damage inhibition (%).

(Equation 1)

[Table 1]

From the results shown in Table 1, it can be seen that the preparation of the present invention has the same insect repellent effect at about one third of the standard dose of paradichlorobenzene (80 g / 50 l), in other words, enhanced insect repellency. It turns out that the effect is obtained continuously.

In addition, in the case of the preparation of the present invention, the aroma generated during the period of use is mainly due to the aroma peculiar to the contained lemongrass oil, and this aroma causes pungent odor from paradichlorobenzene. It was also confirmed that it had been attenuated. In addition, leaching of natural plant essential oils and the like was hardly observed on the surface of the preparation.

Example 2 100 kg of p-dichlorobenzene crystal powder was supplied into the above-mentioned kettle, and the mixture was stirred at about 65 ° C. while being stirred by a stirrer provided in the kettle.
Was continuously passed through to obtain a melt of paradichlorobenzene. Then, a time white oil 50 was added to the melt.
0 g and 100 g of the fragrance of the bouquet aroma component were sequentially added and mixed by stirring.

Next, with the above-described stirring state, the water was continuously passed while the temperature of the water in the kettle was lowered to about 25 ° C. As a result, a flake-like cooled solidified product was obtained after about 30 minutes. The cooled solidified product was pulverized to a particle size of 10 mesh, and two tablets (formulation E) of 4 g / tablet were stored in the same sachet as above to produce a product.

Further, the flavoring compound to be blended was made into 500 g of the fragrance component of jasmine, and two tablets (formulation F) of 4 g / tablet were prepared in the same manufacturing method as described above and put in a wrapper as described above to commercialize. did.

Next, using each of the products of Formulation E and Formulation F as a sample, a test for insect repellency was carried out in the same manner as in Example 1, and the results are shown in Table 2 below.

[Table 2]

From the results, it was found that the effect of enhancing the insect repellent effect was comparable to that of the above-mentioned formulation A, and that of formulation E
And Formulation F. In addition, leaching of natural vegetable essential oil and the like was hardly observed on the surface of any of the preparations.

Next, in a storage case (within a capacity of 50 l) made of cardboard paper, the upper and lower parts of the suit made of wool are folded and stored in a usual manner.
A total of three packets were placed one at a time in the middle and lower positions, and the storage case was left closed. One week after the standing, the suit was taken out and the state of flavor was confirmed as follows. The product of Formulation F was confirmed in the same manner as described above.

5 men and women in their 20s to 40s (10 in total)
A) wearing the suit, and the type of fragrance sensed by the smell was determined according to the following criteria. That is, when it is assumed that no fragrance other than the fragrance is sensed, ◎ is when the fragrance of essential oil is sensed other than the fragrance of fragrance, and × is when the irritating odor of paradichlorobenzene is sensed. . The results are shown in Table 3 below.

[Table 3]

From these results, the insect repellent composition according to this example makes it possible to simultaneously remove the pungent odor caused by p-dichlorobenzene and the aroma caused by natural plant essential oils, and the type of aroma depends on the insect repellent effect. Since it does not affect the flavor, it is possible to appropriately select one containing a fragrance of an aromatic component according to preference.

[0042]

Since the present invention is configured as described above, the following effects are exhibited. According to the production method of the present invention, a flake-like solidified product can be directly obtained without going through a crushing step for a bulk solid, a dehydration step, and a drying step as in the conventional method. Therefore, a flake-like cooled solid can be obtained in a relatively short time by a simpler facility.

Since the obtained flake-like cooled solid is composed of a mixture of natural vegetable essential oil and the like in a molten state of paradichlorobenzene, it is uniformly and stably contained in the cooled solid. Therefore, the insect repellent effect enhanced during the use process and the effect of attenuating the pungent odor of paradichlorobenzene are stably exhibited.

In particular, when paradichlorobenzene contains a natural plant essential oil or the like or an extract thereof and a fragrance, the pungent odor of paradichlorobenzene and the aroma based on the natural plant essential oil or the extract thereof are reduced. In the state where the deodorizing effect is exhibited, a fragrance peculiar to the fragrance is obtained. Therefore, an insect repellent composition having an aroma according to the taste of a person can be obtained.

Further flaky solid obtained is because it is a side small of rectangular shape of 1 mm to 3 mm, in addition that may be used as it is as a formulation, the solidified product itself as it is tabletted and the granules Processing is also very easy.

──────────────────────────────────────────────────続 き Continued on the front page (58) Field surveyed (Int. Cl. ⁷ , DB name) A01N 65/00-65/02 A01M 1/20 A01N 29/04-29/08

Claims (3)

(57) [Claims] 1. A mixed melt of paradichlorobenzene and a natural vegetable essential oil or an extract thereof is prepared at a temperature of 60 ° C. or more and 100 ° C. or less.
A step of obtaining the mixture at the temperature below, and stirring the mixed melt while passing the ice temperature of 25 ° C. or lower through a receiving container.
A method for producing a flaky insect repellent composition, comprising a cooling step of quenching under temperature conditions . 2. A cooling step, continuous cold water cold constant temperature
To made by a process that extend to the molten mixture through a receiver
The method for producing a flaky insect repellent composition according to claim 1 , wherein: 3. A mixed-melt is produced para-dichlorobenzene benzene, natural plant essential oils or flaky insect repellent composition according to claim 1 or 2, characterized in that it consists of the extraction Ingredient and perfume Method.