JPS5946483B2 - Manufacturing method of solid aroma composition - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to a method for producing a solid fragrance composition for deodorizing or numbering purposes.

In particular, the present invention relates to a method for producing an aromatic composition having a suction expectorant effect or a therapeutic effect on respiratory diseases in animals when limonene is the main ingredient.

The present inventor first developed an aromatic component mainly composed of volatile terpene hydrocarbons (hereinafter simply referred to as terpenes) into polyethylene and/or hydrogenated castor oil (hereinafter referred to as hydrogenated castor oil).
It has been found that it is possible to solidify the product and mold it into a molded product with sufficient strength to eliminate the syneresis phenomenon.

However, the above-mentioned molded products do not have sufficient strength, and during use, as the aromatic components volatilize, the molded products often crack or the translucent molded products turn white, which is an unfavorable phenomenon in terms of appearance.

Also, the rate of volatilization increases depending on the temperature and air circulation conditions (
The variable and difficult to control rate of volatilization can lead to unnecessary loss of large amounts of aromatic components and shortened service life.

The present inventor has researched ways to improve such aromatic molded products, and by adding raw rubber or higher aliphatic alcohol (hereinafter referred to as higher alcohol), the strength of the molded product can be increased and cracks or whitening can be prevented during use, and temperature differences The present invention succeeded in significantly reducing the fluctuation in the volatilization rate caused by polyethylene and/or hydrogenated castor oil, and also succeeded in imparting gloss to the skin of the molded product. , a method for producing a solid aroma composition characterized by adding raw rubber and/or higher alcohol.

The terpene, which is the main aromatic component of the composition of the present invention, may be any terpene as long as it is volatile, and volatile terpenes generally have an aroma.

Such substances include those whose main component is α-pinene, d-
I) Those whose main component is monene, and various other terpenes, but among these, limonene is particularly
As shown on page 1017 of the 7th edition of the Index, it has an expectorant effect and a therapeutic effect on respiratory diseases in animals, and the composition according to the present invention can be expected to have these effects as well.

The choice of such terpene is a matter of discretion based on production conditions, intended use, and aroma preference.

Further, terpenes are often produced and handled as a mixture, but in the present invention, a mixture may be used.

Furthermore, terpenes often contain oxygen compounds such as alcohols, aldehydes, ketones, and carboxylic acids naturally or by autoxidation, but they may also contain these.

Furthermore, the fragrance can be strengthened by adding an appropriate amount of a blended fragrance or fragrance crude oil to the terpene, preferably 10% by weight or less (hereinafter % indicates weight%).

In addition, terpenes include allethrin, DDVP (dimethyl 2,2
dichlorovinyl phosphate), DDT, γ-BHC
An appropriate amount of a volatile insecticide such as, preferably 30% or less, may be added.

Further, in order to prevent oxidation of terpenes during the manufacturing process and storage period, it is preferable to add an antioxidant as necessary.

Such antioxidants may be any commonly used antioxidants, such as alkylphenols.

Although various cases have been described above, terpenes are present in at least 60% or more of the aromatic components and constitute the main component of the aromatic components.

Any type of polyethylene can be used as the solidifying agent, but low-density or medium-density polyethylene has a low melting temperature.
The rigidity of the solidified product is preferable because it does not cause syneresis in dogs.

Moreover, any commercially available hydrogenated castor oil may be used.

The raw rubber referred to in the present invention is synthetic rubber or natural rubber itself, which is known as a compounding raw material for manufacturing various rubber products, such as ethylene propylene rubber (EPT), chloroprene rubber (CR), styrene-butadiene rubber ( SBR)
, isoprene rubber (IR), butadiene rubber (BR),
Examples include inbutylene isoprene rubber (IIR), styrene rubber (SR), chloroprene nitrile rubber, acid polypropylene, various other synthetic rubbers, and natural or modified natural rubbers such as veil crepe, smoked sheet, and chlorinated rubber.

Further, any higher alcohol may be used as long as it is solid at room temperature, and examples thereof include cetyl alcohol, lauryl alcohol, and stearyl alcohol.

It is sufficient that the above-mentioned solidifying agent be added in an amount of 9 to 20 parts per 100 parts by weight of the aromatic component (hereinafter, parts are by weight).

That is, if it is less than 9 parts, the rigidity of the solidified product is insufficient for the purpose or syneresis occurs, which is not preferable.

On the other hand, addition of 20 parts or more is unnecessary.

Further, the amount of raw rubber and/or higher alcohol added to polyethylene and/or hydrogenated castor oil in the above-mentioned solidifying agent is 50% or less to sufficiently achieve the purpose.

The above-mentioned aromatic components and solidifying agents may be heated at a temperature suitable for each component, for example, 80 to 120°C, for a period of 1j9, melted or homogenized, and then cooled to room temperature = 1j9. It may be molded into a shape or cut into a certain shape after solidification.

When adding raw rubber, it is preferable to dissolve it in terpene in advance and use it as a highly concentrated terpene solution.

As shown in the formulation example below, the present invention contains aromatic terpenes at a high concentration of at least 60% or more, and depending on the purpose of use, it can be contained as high as 80 to 90% without causing syneresis. The addition of raw rubber and/or higher alcohol increases the strength of the solidified molded product and prevents cracking during use.It also reduces the rate of volatilization and prevents volatilization due to temperature differences. This shows the effect of reducing fluctuations in speed and extending the period of use of the solidified molded product.

In addition, by adding raw rubber, the molded product becomes glossy,
It has the effect of preventing whitening.

This will be explained in detail below using Examples and Comparative Examples.

Example 1 Polyethylene ■ in Examples has a molecular weight of 40,000 to 50,000 and a density of 0.92 to 0.95.
has a molecular weight of 1500. It has a density of 0.91 to 0.93.

Moreover, lauryl alcohol was used as the higher alcohol.

In addition, when blending raw rubber, dissolve it in the terpene in advance.
A 0% concentration terpene solution was added to the fragrance along with other formulations.

Heating was carried out at 80° C. for 3.5 minutes. After melting, the mixture was cooled to form a molded product.

The strength of the molded product was determined by measuring the penetration level, the occurrence of cracks during use, and whether or not the molded product broke when subjected to a constant impact while in a solidification container.

The strongest one was graded as good, and the following were graded as acceptable.

Even if it is judged as acceptable, there is no problem in practical use, but cracks were observed during use.

The skin of the molded product was examined for the presence or absence of gloss by observing the skin when it was removed from the solidification container.

The whitening of the molded product was investigated to determine whether it whitened or remained translucent as the aromatic components evaporated.

The presence or absence of syneresis was determined by observing whether there was any free liquid when removing the molded product.

The rate of volatilization was expressed as the percentage weight loss after 1 and 20 days when the molded product was exposed to use in a room at 20°C.

Examples 1 to 7 *1 Examples 1 to 3 and 6 are 95% d-limonene, 4°5,
No. 7 used 85% d IJ monene, and 0.2% of 2,6 ditertiary butyl-p-cresol was added as an antioxidant in both cases.

*2 As raw rubber, Example 3 is EPT (Mikata Petrochemical Co., Ltd. 4
045), 4 is IIR (Japan Synthetic Rubber HT-10-
66) and 5 used natural rubber, 5BR (Nippon Zeon 1502) was used in 6, and BR (Nippon Zeon 1220) was used in 7.

In addition, the same experiment was repeated by adding 5% lemon flavor crude oil to the aromatic components of each example, but the results were the same and the volatilization rates were approximately similar, so the description is omitted.

Comparative Examples 1 to 4 Molded products made from the compositions of Examples 1 to 4 excluding raw rubber and lauryl alcohol did not exhibit any syneresis phenomenon, but had fair strength.

Furthermore, the molded product lacked luster, and cracking and whitening were observed during use.

Examples 8 to 13 All molded products had excellent strength and gloss, and no whitening or syneresis was observed.

*3. *4 In Example 8, the above EPT was used as raw rubber.

1 part each of SBR, 2 parts in total. In 2, 1 part each of BR and IIR were used. In 10, chlorinated rubber (CR-5 made by Denka) was used, and in 11, the above SBR was used. In No. 12, IR (Nippon Zeon 2200) was used, and in No. 13, CP (
This is the case where electrochemical system M40) was used.

The aromatic component of Example 8 was 95% d-limonene, the aromatic components of Examples 9 and 10 were 95% d-limonene with 5% lemon flavor crude oil added, and the aromatic component of Example 11 was 85% d-limonene. 5% lemon flavored crude oil is added to d-limonene.

The aroma components of the same 12 are 95% d-limonene 72%, lemon fragrance crude oil 5%, and DDVP 23%.
The fragrance component of No. 3 is α-pinene with the addition of 5% lemon flavored crude oil and 0.2% of the aforementioned antioxidant.

Example 14 The volatilization rates of the molded products of Examples 1 to 4 and Comparative Examples 1 to 4 were measured at different temperatures, and the results are shown in the following table.

Claims (1)

[Claims] 1. A method for producing a solid aromatic composition, which comprises adding crude rubber and/or higher aliphatic alcohol when solidifying an aromatic component mainly composed of volatile terpene hydrocarbons with polyethylene and/or hydrogenated castor oil.