KR20200025856A - Method for preparing gelled aromatic composition and preparing gelled aromatic composition - Google Patents

Abstract

The present invention relates to a method for producing a gel form fragrance composition. More specifically, provided is a gel form fragrance composition excellent in sustained release that can continuously emit fragrance using an extract of unripe green tangerine in Jeju region. In addition, the gel form fragrance composition has excellent durability and heat resistance, is barely damaged by impact, and is not liquefied even when stored at a high temperature for a long time.

Description

METHODS FOR PREPARING GELLED AROMATIC COMPOSITION AND PREPARING GELLED AROMATIC COMPOSITION

The present invention relates to a method for producing a fragrance composition on a gel and a fragrance composition on a gel, and excellent in sustained release that can continuously emit aroma, excellent heat resistance, which can maintain the gel phase even in high temperature environment A method for preparing a perfume composition on a gel and a perfume composition on a gel.

Recently, as the health is threatened by the lack of pleasant living environment and the deterioration of natural purification rate due to the rapidly changing environment, efforts are being made to make indoor air comfortable. A typical fragrance used to purify indoor air was used for the purpose of masking odors such as toilets with a strong scent, and this use still occupies a large part. However, it is now widely used for aromas in the interior or in the car, or even for psychological therapy.

A fragrance is a pleasant atmosphere of human beings by releasing natural or artificial scents in a certain space where a person can stay, for example, in a bathroom, living room, kitchen, room, warehouse, etc. It is a product used to help the life to eliminate the smell of the indoor odor and its purpose.

Conventionally, as a fragrance constituting such fragrance fragrance products, relatively volatile liquid components were often used to dissipate easily into the air. At this time, a liquid substance is stably contained and provided to the air. In order to faithfully perform the fragrance function by the component divergence, there is a need for a fragrance product having a special type of sealed container in which the liquid permeation can be restricted to the liquid substance while the liquid can be vaporized and diverted to the outside. .

The fragrance components each have a constant boiling point, and due to its easily volatilized nature, it is difficult to maintain the fragrance for a long time in nature, and thus, in order to maintain the fragrance for a long time, gelatin, agar, and carrageenan (coated with isobutylene maleic anhydride copolymer) An aqueous gel was prepared using a gelling agent such as Carragheenas).

However, since the gelling agents have to be processed through a warming process after being immersed in ionized water at a high temperature of 70 to 80 ℃ ℃, the manufacturing process of the aqueous gel has a disadvantage of complicated, and when the gel shrinks, the constituent material contained in the gel There was a problem that the separation process occurs.

Accordingly, there is a need to develop a fragrance composition having a good gel-release property that can prevent the separation of constituent materials even in a high-temperature environment, and that can release the fragrance for a long time.

(Patent Document 1) KR 10-0432674 B1

OBJECT OF THE INVENTION The object of the present invention relates to a process for the preparation of perfume compositions on gels and to perfume compositions on gels.

Another object of the present invention is to provide a fragrance composition on a gel and a fragrance composition on a gel which are excellent in sustained release property which can continuously give off fragrance.

Another object of the present invention is to provide a method for producing a perfume composition on a gel and a perfume composition on a gel which are excellent in durability and heat resistance, which do not cause damage even in impact, and which are not liquefied even when stored at a high temperature for a long time.

In order to achieve the above object, a method of preparing a fragrance composition on a gel according to an embodiment of the present invention comprises the steps of 1) preparing a first polymer mixture by mixing a polymer compound, a solvent, a pharmaceutical and a nucleating agent; 2) mixing the crosslinking agent and the solvent to prepare a crosslinking mixture; 3) preparing a second polymer mixture by mixing a tangerine extract (Citrus nippokoreana Tanaka) to the polymer mixture of step 1); And 4) mixing a crosslinked mixture with the second polymer mixture and stirring the mixture; 5) aging the stirred mixture of step 4), wherein the polymer is selected from the group consisting of polybutadiene, polyisoprene, polychloroprene and mixtures thereof.

Step 1) may be stirred for 30 minutes to 2 hours at a rate of 200 to 400 RPM at 10 to 20 ℃, to prepare a first polymer mixture in which the polymer, the flavor and the nucleating agent in the solvent is completely dissolved.

Step 2) is to stir for 10 to 20 minutes at a rate of 50 to 150 RPM at 10 to 20 ℃, to completely dissolve the cross-linking agent in the solvent.

Step 3), 3-1) mixing the tangerine extract (Citrus nippokoreana Tanaka) to the polymer mixture of the step 1), the first stirring for 10 to 20 minutes at a rate of 10 to 50 RPM at 10 to 20 ℃ step; 3-2) after the first stirring step, the first stabilization step to stabilize the reaction for 30 to 60 minutes at 10 to 20 ℃; 3-3) after the first stabilization step, a second stirring for 30 to 60 minutes at a rate of 50 to 100 RPM at 30 to 40 ℃; 3-4) a second stabilizing step of stabilizing the reaction at 40 ° C. for 30 to 60 minutes after the second stirring step; And 3-5) after the second stabilization step, a third stirring for 10 to 30 minutes at a rate of 50 to 150 RPM at 50 to 60 ℃.

The crosslinking agent is selected from the group consisting of alkylpropyldiamine, polyoxyalkylenediamine, polyoxyalkylenetriamine and mixtures thereof.

The tangerine extract is a fermented tangerine extract.

The perfume composition on the gel according to another embodiment of the present invention is prepared by using the method for preparing the perfume composition on the gel.

Hereinafter, the present invention will be described in more detail.

Method for producing a fragrance composition on a gel according to an embodiment of the present invention comprises the steps of 1) preparing a first polymer mixture by mixing a polymer compound, a solvent, a pharmaceutical and a nucleating agent; 2) mixing the crosslinking agent and the solvent to prepare a crosslinking mixture; 3) preparing a second polymer mixture by mixing a tangerine extract (Citrus nippokoreana Tanaka) to the polymer mixture of step 1); 4) mixing a crosslinked mixture with the second polymer mixture and stirring the mixture; 5) aging the stirred mixture of step 4).

More specifically, the first polymer mixture is prepared by mixing a polymer compound, a solvent, a perfume, and a nucleating agent. In this case, the polymer compound may be selected from the group consisting of polybutadiene, polyisoprene, polychloroprene and mixtures thereof.

The nucleating agent is any one or more selected from the group consisting of gelatin, carrageenan, agar, xanthan gum, gellan gum fumed silica, wet silica, and mixtures thereof, but is not limited to the above examples, and a crosslinking agent selectable by those skilled in the art Can be used without limitation.

The fragrance is an organic substance with a strong scent added to add a fragrance, which means excellent volatility at room temperature, and the fragrance used in the fragrance composition can be used without limitation.

In order to homogeneously dissolve the high molecular compound, the fragrance and the nucleating agent, the first polymer mixture is first prepared. At this time, to prepare a uniform first polymer mixture, step 1) is stirred for 30 minutes to 2 hours at a rate of 200 to 400 RPM at 10 to 20 ℃. More specifically, step 1) is stirred for 1 hour at a rate of 300RPM at 20 ℃. Under the stirring conditions, it is possible to produce a uniform first polymer mixture. In the case where the uniform first polymer mixture is not prepared, that is, when the stirring process is performed under different stirring conditions, it is impossible to prepare the uniform first polymer mixture, and a nonuniform polymer mixture is prepared to prepare a fragrance composition on the gel. In the case of manufacturing, there exists a problem of inferior durability. That is, the problem that the fragrance on a gel is broken even with a small impact arises, and the problem which cannot use it as a vehicle fragrance etc. arises.

The first polymer mixture may be prepared, and then a crosslinking agent and a solvent may be mixed to prepare a crosslinking mixture. The crosslinking agent is selected from the group consisting of alkylpropyldiamine, polyoxyalkylenediamine, polyoxyalkylenetriamine and mixtures thereof, but is not limited to the above examples, and any crosslinking agent selectable by those skilled in the art can be used without limitation. It is possible.

Step 2) may be stirred for 10 to 20 minutes at a rate of 50 to 150 RPM at 10 to 20 ℃, to completely dissolve the cross-linking agent in the solvent. More specifically, the mixture is stirred at 20 ° C. at a speed of 150 RPM for 15 minutes. The crosslinking agent may be completely dissolved in the organic solvent under the stirring conditions.

More specifically, the solvent of steps 1) and 2) is at least one selected from the group consisting of water, mono alcohols having 1 to 5 carbon atoms and diols having 2 to 5 carbon atoms, and preferably ethanol.

Using the solvent, step 1) is to prepare a polymer compound into a liquid polymer compound, the uniform flavor and nucleating agent is mixed in the liquid polymer compound, step 2) is an organic solvent to prepare a crosslinking compound Allow the crosslinking agent to be uniformly mixed in.

Step 3) is a step of preparing a second polymer mixture by mixing the tangerine extract (Citrus nippokoreana Tanaka) to a uniformly mixed polymer compound.

The tangerine extract is similar to tangerine (Citrus unshiu Markovich), but shows a large difference in the sustained release, durability and heat resistance of the fragrance composition on the gel prepared compared to the case of using the tangerine extract or dermis extract.

In general, the tangerine extract or dermis extract used in the fragrance composition is used as a fragrance for the majority, and is used to provide a tangerine fragrance as a tangerine extract or dermis extract, which is a sustained release, durability and Not effective in heat resistance

On the other hand, when using a mixture of citrus extract (Citrus nippokoreana Tanaka), synergistic effect is shown by the mixing action with the nucleating agent, compared to the case without containing the tangerine extract, sustained release, Excellent effect in durability and heat resistance.

At this time, the step of preparing the second polymer mixture, 3-1) mixed with the tangerine extract (Citrus nippokoreana Tanaka) to the polymer mixture of the step 1), 10 to 20 at a rate of 10 to 50 RPM at 10 to 20 ℃ First stirring for minutes; 3-2) after the first stirring step, the first stabilization step to stabilize the reaction for 30 to 60 minutes at 10 to 20 ℃; 3-3) after the first stabilization step, a second stirring for 30 to 60 minutes at a rate of 50 to 100 RPM at 30 to 40 ℃; 3-4) a second stabilizing step of stabilizing the reaction at 40 ° C. for 30 to 60 minutes after the second stirring step; And 3-5) after the second stabilization step, a third stirring for 10 to 30 minutes at a rate of 50 to 150 RPM at 50 to 60 ℃.

More specifically, 3-1) mixing the tangerine extract (Citrus nippokoreana Tanaka) to the polymer mixture of the step 1), the first stirring for 15 minutes at a speed of 50 RPM at 15 ℃; 3-2) a first stabilizing step of stabilizing the reaction at 15 ° C. for 60 minutes after the first stirring step; 3-3) after the first stabilization step, a second stirring at 40 ° C. at a rate of 100 RPM for 40 minutes; 3-4) a second stabilization step of stabilizing the reaction at 40 ° C. for 60 minutes after the second stirring step; And 3-5) after the second stabilization step, a third stirring for 30 minutes at a rate of 100 RPM at 60 ℃.

Even if the mixture of the tangerine extract is mixed with the first polymer mixture, the stirring process is carried out, and then the process is carried out to prepare the fragrance composition on the gel, the prepared fragrance composition on the gel has excellent sustained release, Although durability and heat resistance are exhibited, as described above, when the stirring process and the stabilization process are carried out step by step, the effect of mixing between the nucleating agent and the tangerine extract can be enhanced in the second polymer mixture, so that the sustained release, durability and heat resistance The preparation of perfume compositions on good gels is possible.

More specifically, the extract is a tangerine ethanol extract, the ethanol extract may be eluted with ethanol pulverized crushed dried tangerine, the extraction temperature is extracted from 10 ℃ to 100 ℃, preferably room temperature Can be.

The extraction solvent may be used 2 to 50 times by weight of the sample, preferably 2 to 20 times. For extraction, the sample may be left for 1 to 72 hours for leaching in the extraction solvent, in particular 1 to 24 hours.

The filtered extract may be a result obtained by concentrating under reduced pressure with a vacuum rotary concentrator, but is not limited thereto, and includes an extract, a diluent or concentrate of the extract, a dried product obtained by drying the extract, or a modifier or purified product thereof.

More preferably, the tangerine extract may be a fermented tangerine extract. In the case of using the tangerine extract, the unique flavor of the tangerine is contained, when mixed with the flavor, the aroma of the inherent flavor is a problem that is diluted with the tangerine aroma.

Thus, in the case of using the fermented tangerine extract, compared to the case of using the tangerine extract, while the inherent flavor of the tangerine is removed, the effect of mixing with the nucleating agent was confirmed to be excellent.

The microorganisms used for the fermentation are Lactobacillus salivarius, Lactobacillus acidophilus, Lactobacillus brevis, Lactobacillus rhamnosus, Lactobacillus rhamnosus and Lactobacillus plantarum. Lactobacillus plantarum, Lactobacillus helveticus, Lactobacillus fermentum, Lactobacillus paracasei, Lactobacillus paracasei, Lactobacillus casei, Lactobacillus del brui del bruii Lactobacillus kefir, Lactobacillus kefir, Lactobacillus keuter, Lactobacillus buchneri, Lactobacillus gasseri, Lactobacillus johonsonii, Lactobacillus kefir, etc. Lactococcus lactis, lactoco Lactococcus plantarum, Lactococcus raffinolactis, Enterococcus faecalis, Enterococcus faecium, Streptococcus thermophilus, Streptococcus thermophilus Lactic acid cocci and Bifidobacterium animals, Bifidobacterium bifidum, Bifidobacterium, such as Leukonostoc lactis, Leukonostoc mesenteroides, etc. Bifidobacterium breve, Bifidobacterium infantis, Bifidobacterium longum, Bifidobacterium pseudolongum, Bifidobacterium turmofilum , Bifidobacterium adolescentis, and the like, and may also include Bifidobacterium adolescentis. Lactobacillus casei, Lactobacillus rhamnosus, Bifidobacterium bifidum bifidus, Bifidobacterium breve bifidus, and Lactobacillus casei, and Lactobacillus casei Bacillus adophyllus (Lactobacillus acidophilus) may be one or more selected from the group consisting of.

More specifically, the first polymer mixture includes 50 to 100 parts by weight of the polymer compound, 50 to 80 parts by weight of perfume and 1 to 5 parts by weight of nucleating agent based on 100 parts by weight of the solvent. The crosslinking mixture contains 10 to 20 parts by weight of the crosslinking agent based on 100 parts by weight of the solvent. The second polymer mixture includes 5 to 10 parts by weight of the tangerine extract based on 100 parts by weight of the first polymer mixture. By the mixing action between the components within the above weight range, it is possible to prepare a fragrance composition on a gel having excellent sustained release, durability and heat resistance.

According to the manufacturing method of the fragrance | flavor composition on the gel of this invention, it is providing the fragrance | flavor composition on the gel excellent in the sustained release which can continuously give off fragrance.

In addition, it is excellent in durability and heat resistance, it is possible to provide a gel-like perfume composition that does not cause damage even in impact, and does not liquefy even if stored for a long time at high temperature.

Hereinafter, embodiments of the present invention will be described in detail so that those skilled in the art can easily implement the present invention. As those skilled in the art would realize, the described embodiments may be modified in various different ways, all without departing from the spirit or scope of the present invention.

[ Production Example : Preparation of Fragrance Composition on Gel]

1. Preparation of Tangerine Extract and Fermented Tangerine Extract

The dried tangerine was pulverized, ethanol as an extraction solvent was added to the pulverized tangerine at a ratio of 1:10 (w: v), and then completely immersed, and extracted three times for 3 hours while refluxing at 80 ° C. The extract was Whatman No. It filtered with 2 filter paper. The filtrate was concentrated under reduced pressure at 60 ℃ to prepare a powder sample was used in the experiment.

Bacillus strain culture was added to the extract and fermented to obtain a fermentation extract. After the fermentation extraction step, filtration may be performed to remove unreacted solids. Filtration is preferably performed at least once using a 0.1-3 μm filter. If the pore size of the filter is less than 0.1 μm, the filter is very precise and ultra-high (ultrafiltration method), so there is a problem of poor economical efficiency. If the pore size exceeds 3 μm, there is no bactericidal power and fungi or bacteria are included in the final extract and contaminated during distribution. There is a problem that is likely to be.

2. Example 1

50 parts by weight of polybutadiene, 100 parts by weight of ethanol, 50 parts by weight of lemongrass oil and 5 parts by weight of dry silica were mixed, and stirred at a rate of 300 RPM at 20 ° C. for 1 hour to prepare a first polymer mixture. Thereafter, 5 parts by weight of the tangerine extract was added to 100 parts by weight of the first polymer mixture, the first stirring was performed at 15 ° C. at a speed of 50 RPM for 15 minutes, and after the first stirring, the reaction was stabilized at 15 ° C. for 60 minutes. After stabilization, a second stirring was performed for 40 minutes at 35 ° C. at a rate of 100 RPM, and after the second stirring, the reaction was stabilized at 40 ° C. for 60 minutes. After the stabilization, the second polymer mixture was prepared by third stirring at 60 ° C. at a rate of 100 RPM for 30 minutes.

10 parts by weight of polyoxyalkylenediamine as a crosslinking agent was mixed with 100 parts by weight of ethanol and stirred at 20 ° C. at a speed of 150 RPM for 15 minutes to prepare a crosslinking mixture.

The second polymer mixture and the crosslinked mixture were mixed and stirred at 20 ° C. at a speed of 150 RPM for 15 minutes, and the mixed solution was aged for 1 hour to prepare a fragrance composition on a gel.

3. Example 2

Except that 10 parts by weight of the tangerine extract was prepared in the same manner as in Example 1.

4. Example 3

Except for putting 5 parts by weight of fermented tangerine extract instead of the tangerine extract, it was prepared in the same manner as in Example 1.

5. Example 4

Except for putting 10 parts by weight of fermented tangerine extract instead of the tangerine extract, it was prepared in the same manner as in Example 1.

6. Comparative Example 1

It was prepared in the same manner as in Example 1 except that the tangerine extract was not added.

6. Comparative Example 2

Except that 1 part by weight of the tangerine extract, it was prepared in the same manner as in Example 1.

7. Comparative Example 3

Except that 15 parts by weight of the tangerine extract was prepared in the same manner as in Example 1.

8. Comparative Example 4

Except for putting 1 part by weight of fermented bilberry extract instead of the bilberry extract, it was prepared in the same manner as in Example 1.

8. Comparative Example 5

Except for putting 15 parts by weight of fermented tangerine extract instead of the tangerine extract, it was prepared in the same manner as in Example 1.

 [ Experimental Example  1: durability test]

Maximum stress, strength, hardness and yield value were measured for the perfume compositions on the gels of Examples 1, 3 and Comparative Example 1 to test the durability of the perfume compositions on the gel.

As a specific experimental method, the physical properties were measured with a rheo meter (used model: compact-100II, the sun company), and the physical properties were measured by compressing an adapter of 1.77 cm ² area at a speed of 120 mm / min perpendicular to the gel surface.

Example 1 Example 3 Comparative Example 1 Center Outskirts Center Outskirts Center Outskirts burglar 1455 g / cm ² 1432g / cm ² 1620g / cm ² 1614g / cm ² 1411g / cm ² 1301 g / cm ² Hardness 6155g / cm ² 6205g / cm ² 7110g / cm ² 7100g / cm ² 6215g / cm ² 6005g / cm ²

As shown in Table 1, in the case of Example 1 and Example 3, it can be seen that the excellent strength and hardness are exhibited, and in addition, it can be seen that the strength and hardness almost similar in the central and outer parts.

On the other hand, the fragrance composition on the gel of Comparative Example 1 did not occur a uniform crosslinking reaction between the central portion and the outer portion, it was confirmed that a large difference in strength and hardness.

[ Experimental Example  2: heat resistance test]

The fragrance composition on the gels of Examples 1 to 4 and the fragrance composition on the gels of Comparative Examples 1 and 5 were stored at 60 ° C. for 4 weeks to observe whether the gel phase was retained.

Example 1 Example 2 Example 3 Example 4 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Comparative Example 5 Heat resistance Insoluble Insoluble Insoluble Insoluble record record record record record

Table 2 is an experimental result for keeping the gel phase by storing for 4 weeks at 60 ℃, in the case of Examples 1 to 4, the gel phase was maintained even if stored for 4 weeks at 60 ℃, Comparative Examples 1 to 5 Melting occurred within one week, or melted within two weeks.

In addition, assuming that it is used as a vehicle gel phase perfume composition for the summer season, the storage experiment was conducted for 4 weeks at 80 ℃, it was confirmed that the gel phase for 4 weeks only in the case of Examples 3 and 4.

[ Experimental Example  3: sustained release experiment]

In order to test the fragrance of the fragrance composition on the gel of Examples 1, 3 and Comparative Example 1, the experiment was conducted for 4 weeks by measuring the microbalance of the weight change amount of the gel daily in a 30 ° C. incubator.

In Comparative Example 1, a weight change of 0.35 to 0.25 g was observed for one week, and a sustained fragrance effect was confirmed, but after 2 weeks, the weight was changed to about 0.1 to 0.05 g, and after 3 weeks, the weight was changed. The change was confirmed to be insignificant.

This means that after 2 weeks, it does not show a sustained fragrance effect, which means that it does not exhibit sustained release.

On the other hand, in the case of Example 1 and Example 3, the weight change was 0.35 to 0.20g for one week, the weight change was about 0.15 to 0.10g after two weeks, and the weight of 0.10 to 0.05g after three weeks. It was confirmed that the change was continuously indicated.

By checking the weight change of 0.04g (Example 3) until the last day of the four weeks the experiment, it was confirmed that the fragrance effect is maintained for four weeks.

Although the preferred embodiments of the present invention have been described in detail above, the scope of the present invention is not limited thereto, and various modifications and improvements of those skilled in the art using the basic concepts of the present invention defined in the following claims are also provided. It belongs to the scope of right.

Claims (7)

1) preparing a first polymer mixture by mixing a polymer compound, a solvent, a reagent, and a nucleating agent;
2) mixing the crosslinking agent and the solvent to prepare a crosslinking mixture;
3) preparing a second polymer mixture by mixing a tangerine extract (Citrus nippokoreana Tanaka) to the polymer mixture of step 1);
4) mixing a crosslinked mixture with the second polymer mixture and stirring the mixture; And
5) aging the stirred mixture of step 4),
The polymer compound is selected from the group consisting of polybutadiene, polyisoprene, polychloroprene and mixtures thereof
Process for preparing perfume composition on gels.
The method of claim 1,
Step 1) is stirred for 30 minutes to 2 hours at a rate of 200 to 400 RPM at 10 to 20 ℃, to prepare a first polymer mixture in which the polymer, the perfume and the nucleating agent in the solvent is completely dissolved
Process for preparing perfume composition on gels. The method of claim 1,
Step 2) is to stir for 10 to 20 minutes at a rate of 50 to 150 RPM at 10 to 20 ℃, to completely dissolve the crosslinking agent in the solvent
Process for preparing perfume composition on gels.
The method of claim 1,
Step 3),
3-1) mixing the tangerine extract (Citrus nippokoreana Tanaka) to the polymer mixture of step 1) and first stirring for 10 to 20 minutes at a rate of 10 to 50 RPM at 10 to 20 ℃;
3-2) after the first stirring step, the first stabilization step to stabilize the reaction for 30 to 60 minutes at 10 to 20 ℃;
3-3) after the first stabilization step, a second stirring at 30 to 40 ° C. at a rate of 50 to 100 RPM for 30 to 60 minutes;
3-4) a second stabilization step of stabilizing the reaction at 40 ° C. for 30 to 60 minutes after the second stirring step; And
3-5) after the second stabilization step, comprising a third stirring for 10 to 30 minutes at a rate of 50 to 150 RPM at 50 to 60 ℃
Process for preparing perfume composition on gels.
The method of claim 1,
The crosslinking agent is selected from the group consisting of alkylpropyldiamine, polyoxyalkylenediamine, polyoxyalkylenetriamine and mixtures thereof
Process for preparing perfume composition on gels.
The method of claim 1,
The bilberry extract is fermented bilberry extract
Process for preparing perfume composition on gels.
Prepared by a process for the preparation of the perfume composition on a gel according to claim 1.
Perfume composition on gel.