KR102433106B1 - scented solid having high heat resistance - Google Patents

Abstract

The present invention relates to a perfume composition comprising microcrystalline wax. In particular, the perfume composition according to the present invention is stable even at a high temperature and has an excellent scent diffusing effect, so it has excellent scent diffusing property even in a closed space such as a car or a closet with a high temperature rise.

Description

High heat resistance solid air freshener {scented solid having high heat resistance}

The present invention relates to perfume compositions that are stable at high temperatures.

In response to the demand for various fragrances in residential spaces and limited indoor spaces, companies tried to achieve the above object through various application studies. Many studies such as liquid type, gel type, wax type, electric type, and membrane type suggest effective delivery methods, but there are disadvantages of each, so it is insufficient to have an emotionally completed scent diffusing system. The diffuser is a representative type of liquid fragrance, in which the contents are volatilized through the porous lid, but there is a limitation in that the fragrance characteristics change as the period elapses.

In addition, there is a limit in delivering the unique sensibility of the fragrance because the characteristics of the fragrance vary depending on the solvent used. In the case of electric type, plug-in or automatic injection type is the most representative. In the case of a plug-in, there is a space limitation such as a humid bathroom, and there is a disadvantage that the smell changes as time goes by due to heating of the contents including fragrance by electricity. In the case of the automatic injection type, when the fragrance is contained in a filled can and dispersed in the space in the form of an aerosol, there is a noise and a strong instantaneous smell, which limits the enhancement of sensibility. In the case of membrane air fresheners or wax-type air fresheners, it is necessary to improve problems such as leaks inside the vehicle and bursting and melting due to the increase in temperature inside the vehicle in summer.

The biggest constraint for stable odor expression in fragrances is the change of fragrance according to the change of external temperature, the change of odor and the change of the intrinsic odor by the base including the solvent designed to deliver the fragrance.

Therefore, there is a need for research on fragrances capable of stably dissipating fragrance without damaging the unique fragrance with fragrance and without deformation or melting even at high temperatures.

Republic of Korea Patent Publication No. 10-2016-0042586

The problem to be solved by the present invention is to provide a fragrance composition that does not deform or melt even at high temperatures, and can stably emit fragrance from a fragrance.

In order to solve the above problems, the present invention provides a fragrance composition comprising a microcrystalline wax, characterized in that the melting point of 90 to 125 ℃.

In the present invention, the melting point may be 90 to 125 ℃, preferably 93 to 120 ℃, more preferably 95 to 115 ℃.

The present inventors completed the present invention by confirming that the perfume composition according to the present invention does not leak or melt at high temperature, and it is stable at high temperature while containing a fragrance containing a large amount of fragrance component, and has an excellent effect of fragrance. The present invention was completed by confirming experimentally.

Hereinafter, the present invention will be described in detail. The terms or words used in the present specification and claims should not be construed as being limited to their ordinary or dictionary meanings, and the inventor may properly define the concept of the term in order to best describe his invention. Based on the principle that there is, it should be interpreted as meaning and concept consistent with the technical idea of the present invention.

The perfume composition according to the present invention contains microcrystalline wax, and exhibits excellent effects when the melting point of the composition is 90 to 125°C, and preferably, the composition according to the present invention contains natural wax, paraffin wax or both. may include The present inventors have experimentally confirmed that an excellent effect appears when microcrystalline wax is included as a perfume composition having a melting point of 90 to 125° C. through research, and when it further includes natural wax, paraffin wax, or both It was confirmed experimentally that a more remarkable effect was exhibited.

In the present invention, the "microcrystalline wax" has a predetermined crystallinity and strong hardness, and is a wax obtained by refining and separating the residual asphalt remaining after refining crude oil, C ₂₅ to C ₈₀ , preferably Preferably, it is a hydrocarbon mixture containing isoparaffins having a molecular weight of 300 to 1500, preferably 400 to 1200, more preferably 450 to 1000, having a molecular weight of C ₃₁ to C ₇₀ .

The microcrystalline wax that can be used in the present invention is a commercially available microcrystalline wax, for example, but not limited thereto, trade names Multi wax W-445 (Sonneborn), Hi wax (Hi). wax) 400P, 410P (Mitsui), KahlWax, etc. can be used.

Microcrystalline wax contains a large amount of Branched Alkyl Hydrocarbon, so it generally melts at a higher temperature than paraffin wax. have In addition, the ability to absorb oil is greater than that of paraffin wax, which is advantageous for impregnating perfume, and the purification method is also different.

In the present invention, the microcrystalline wax may be included in an amount of 10 to 90% by weight, preferably 20 to 85% by weight, and more preferably 30 to 80% by weight, based on the total weight of the composition.

In the present invention, the "natural wax" includes both animal natural wax and vegetable natural wax, and the animal natural wax is not limited thereto, but wax obtained from beeswax (beeswax), wool wax, whale, etc. and shellac obtained from insects. The vegetable natural wax includes, but is not limited to, soy wax, carnauba wax, and candelilla wax.

The natural wax includes both commercially available natural wax as well as natural wax directly collected from nature.

As used herein, the term "beeswax" is also referred to as beeswax or beeswax, but is not limited thereto. For example, naturally, bees collect sugar from flowers by enzymatic action. It is a yellow substance that is made in the body through the passage of time and secreted by the lower abdominal gland of a worker bee. The beeswax used in the composition according to the present invention may be processed and used after removing impurities by filtering the beeswax through a filter.

In the present invention, the beeswax may contain 40 to 90% by weight of wax ester, 1 to 30% by weight of free fatty acids, 0.1 to 5% by weight of free alcohol, or a mixture of two or more thereof, based on the total weight of the beeswax, preferably 62 to 75% by weight of wax esters, 5 to 16% by weight of free fatty acids, 1 to 2% by weight of free alcohols or a mixture of two or more thereof, more preferably a mixture of both. In addition, it may contain 10 to 20 wt% of a C ₂₀ to C ₄₀ hydrocarbon or 2 to 5 wt% of a glyceride (C ₁₄ , C ₁₆ or C ₁₈ ).

In the present invention, the "paraffin wax" is a crude wax containing a lubricating oil component with a high boiling point in crude oil, which is purified by excluding oil components such as lubricating oil, and is a linear hydrocarbon in molecular structure. It is an alkane (alkane) hydrocarbon, usually represented by the chemical formula of CnH2n+2 (n≥19), and is a mixture of hydrocarbon molecules consisting of 20 to 40 carbon molecules.

The paraffin wax may have a melting point of 40 to 90°C. In addition, in the present invention, the paraffin wax can be classified into high melting point paraffin wax and low melting point paraffin wax, and the high melting point paraffin wax refers to paraffin wax having a melting point of 60 to 90° C., preferably 65 to 85° C. . In addition, the low melting point paraffin wax means a paraffin wax having a melting point of 40 to 60 ℃, preferably 45 to 55 ℃.

Preferably, the composition according to the present invention may further include natural wax, paraffin wax, or both in addition to the microcrystalline wax, and the natural wax, paraffin wax, or both of them is 1 to 20% by weight, preferably based on the total weight of the composition. For example, 5 to 15% by weight may be included.

The present inventors experimentally confirmed that the composition exhibits a more excellent effect by further including natural wax, paraffin wax, or all of them in addition to the microcrystalline wax. That is, the present invention preferably includes not only microcrystalline wax, but also natural wax, paraffin wax, or all of them to provide a fragrance composition that has excellent fragrance and is stable even at high temperatures.

In addition, the perfume composition according to the present invention may include a fragrance. In the present invention, the fragrance is not limited thereto, but fragrances that can be used in fragrance products such as general air fresheners and deodorants, as well as human body cleansing products such as shampoo and body wash, laundry products such as detergents and softeners, and cosmetics such as perfumes can be used. .

In the present invention, the perfume is included in the wax structure to form a stable composition. The stable composition of the present invention provides the emotional quality of a good fragrance, which provides a fresh feeling by continuously supplying the encapsulated fragrance while maintaining a stable form in an enclosed space. In the present invention, the fragrance may preferably provide a lasting fragrance.

In the present invention, the fragrance may be included in an amount of 1 to 50% by weight, preferably 5 to 40% by weight, more preferably 10 to 30% by weight, based on the total weight of the composition.

In the present invention, a fragrance may be added to eliminate off-flavor and to keep the odor on the surface for a longer period of time. The composition according to the present invention can use all conventional fragrances, and as the fragrance component, both hydrophobicity or hydrophilicity fragrances can be used.

In addition, the perfume may represent hydrophobicity as logP, which is a log value of the octanol/water partition coefficient, and it may be said that the greater the value, the greater the hydrophobicity. In this case, the greater the hydrophobicity, the better the reverberation property. In general, fragrances for fragrances have a disadvantage in that the designed fragrance is not constantly maintained, although a fragrance with a low hydrophobicity is preferred to a fragrance with a high hydrophobicity in order to improve the fragrance.

LogP, which is a log value of the octanol/water partition coefficient, can be calculated as shown in Equation 1 below.

[Equation 1]

The criterion of hydrophobicity of the perfume used in the present invention is logP 3 . That is, the present inventors have confirmed that desirable reverberation properties are exhibited when the perfume has a logP value of about 3 or more, preferably about 3.1 or more, and most preferably about 3.2 or more.

In addition, in order to make the fragrance last longer, the fragrance must have at least partial hydrophobicity and a relatively high boiling point. That is, the perfume may have a log value of the octanol/water partition coefficient of 3 to 8, and a boiling point of 200 to 500° C., preferably a log value of the octanol/water partition coefficient of 3.2 to 8, and a boiling point It may be 220 to 500 ℃.

Since the properties of the perfume components have various isomers and have a large influence on substances existing in the vicinity, it is not easy to clearly distinguish them with a numerical value such as logP, which is a physical property. Accordingly, the numerical values described above are approximate values for indicating the properties of the fragrance and should be interpreted flexibly in the interpretation of the numerical range.

In addition, the hydrophobic fragrance may be included in 5 to 80% by weight relative to the total weight of the fragrance, preferably in 10 to 60% by weight, more preferably in 15 to 50% by weight.

Table 1 below shows the molecular weight, boiling point, and logP values for some of the various fragrances that can be used in the present invention, and the results of evaluating the degree of reverberation after 3 hours at 90° C. when included in the fragrance composition according to the present invention is a table

spice name CAS No. Molecular Weight boiling point
(℃) logP degree of reverberation Aurantiol 89-43-0 305 450 4.2 O Amyl cinnamate 3487-99-8 218 312 3.8 O Bacdanol 28219-61-6 208 287 4.3 O Cashmeran 33704-61-9 206 285 4.5 O Cervolide 6707-60-4 256 409 3.7 O Cinnamyl cinnamate 122-69-0 264 370 5.5 O Citral 5392-40-5 152 103 3.4 X Dihydro myrcenol 18479-58-8 156 196 3.0 X Ethylene brassylate 105-95-3 270 332 4.6 O Galaxolide 1222-05-5 258 326 5.3 O Helvetolide 141773-73-1 284 346 4.7 O Hexadecalonide 109-29-5 254 358 6.7 O Hexyl Salicylate 6259-76-3 222 290 5.1 O Iso-E Super 54464-57-2 234 312. 3.6 O Iso-propyl myristate 110-27-0 271 320 7.2 O Limonene 5989-27-5 136 176 4.6 X Lyral 31906-04-4 210 319 2.1 X Methyl dihydrojasmonate 24851-98-7 226 308 2.7 O Phenyl ethyl phenyl acatete 102-20-5 240 325 3.8 O Romandolide 236391-76-7 270 308 4.6 O Tonalid 1506-02-1 258 393 5.1 O Trisamber 338735-71-0 250 263 6.2+ O

That is, the fragrance that can be used in the present invention is not limited thereto, but oranthiol, amyl cinnamate, bacdanol, cashmeran, serbolide, cinnamyl cinnamate, ethylene brasylate, galaxolide, helvetol Ride, hexadecanolide, hexyl salicylate, iso-E super, iso-propyl myristate, methyl dihydrojasmonate, phenyl ethyl phenyl acetate, romandolide, tonalide, trisamber or mixtures of two or more thereof can be used

In addition, preferably, the composition according to the present invention may further include a polymer, and the polymer may improve usability by increasing the reverberation of an additional fragrance.

Therefore, it is preferable that the polymer is a nonionic polymer and has oil absorption. That is, the polymer may be a nonionic oil-absorbing polymer, but is not limited thereto, and may include, for example, polyethylene glycol, a copolymer of polyoxyethylene and polyoxypropylene, etc., and commercially available products include PEG 400 , Poloxamer or Pluronics may be included.

The polymer may be included in an amount of 0.01 to 20% by weight, preferably 0.05 to 15% by weight, and more preferably 0.1 to 10% by weight, based on the total weight of the composition.

In addition, preferably, the composition according to the present invention may further include a surfactant, and the surfactant helps to mix the wax and the fragrance, and cracks that may occur due to non-uniform distribution of the fragrance in the wax as the fragrance is emitted during use, etc. It can have excellent usability by preventing odor and increasing the reverberation of the fragrance.

The surfactant may be included in 0.5 to 15% by weight relative to the total weight of the composition, preferably 1 to 10% by weight, more preferably 2 to 7% by weight.

In addition, the present invention provides a fragrance comprising the composition.

The fragrance is not limited to any form, but may preferably be in a solid form.

The perfume composition according to the present invention is stable even at a high temperature and has an excellent scent diffusing effect, and thus has excellent scent diffusing property even in a closed space such as a car or a closet with a high temperature rise.

Hereinafter, examples and examples will be described in detail to describe the present invention in detail. However, the embodiments and embodiments according to the present invention may be modified in various other forms, and the scope of the present invention should not be construed as being limited to the embodiments and examples described below. The examples and examples of the present invention are provided in order to more completely explain the present invention to those of ordinary skill in the art.

Preparation of Examples and Comparative Examples

The present inventors prepared a perfume composition having a composition as shown in Table 3 below, using the perfume as shown in Table 2 below.

Since the perfume composition according to the present invention consists of paraffin wax, microcrystalline wax, fragrance and other components, the fragrance is stably dispersed in the high melting point wax during the production process of the present perfume composition and is present in the composition during the molding and cooling process. it is important In order to maintain the fragrance in the high melting point wax, it must first be combined and melted according to the characteristics of the wax. After the fragrance is added, the fragrance is evenly dispersed in the wax. A functionally functioning composition could be maintained.

No. spice name CAS No. Content (wt%) One Aurantiol 89-43-0 10.0 2 Bacdanol 28219-61-6 10.0 3 Citral 5392-40-5 10.0 4 Ethylene brassylate 105-95-3 5.0 5 Galaxolide 1222-05-5 5.0 6 Hexyl Salicylate 6259-76-3 5.0 7 Iso-E Super 54464-57-2 5.0 8 Lyral 31906-04-4 30.0 9 Methyl dihydrojasmonate 24851-98-7 10.0 10 Phenyl ethyl phenyl acatete 102-20-5 5.0 11 Trisamber 338735-71-0 5.0 Sum 100.0

Since the perfume composition according to the present invention consists of paraffin wax, microcrystalline wax, fragrance and other ingredients, it is important to ensure that the fragrance is stably dispersed in the high melting point wax during the production process of the composition and is present in the composition during the molding and cooling process. It is important. In order to maintain the fragrance in the high melting point wax, it must first be combined and melted according to the characteristics of the wax. After the fragrance is added, the fragrance is evenly dispersed in the wax. A functionally functioning composition could be maintained.

no. division Ingredients (wt%) Comparative Example 1 Comparative Example 2 Comparative Example 3 Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 One natural wax Soywax 20.0 - 10.0 - - - - - - 5.0 2 Beeswax 50.0 - - - - - - - - - 3 paraffin wax low melting point paraffin wax - 35.0 10.0 - - - - - 10.0 - 4 high melting point paraffin wax - 35.0 50.0 - - - - - 5.0 5 microcrystalline wax Multi wax W-445 - - - 70.0 - - 40.0 10.0 15.0 15.0 6 Hi wax 410P - - - - 70.0 - 20.0 20.0 25.0 25.0 7 Hi wax 400P - - - - - 70.0 10.0 40.0 20.0 20.0 8 copolymer EMA 1605 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 9 Surfactants Sorbitan monostearate 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 5.0 10 Spices Composite Fragrance of Table 2 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 20.0 Sum 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 100.0 Melting point (℃) 50 60 60 80 95 105 100 110 105 100

The wax used in the present invention was used in Comparative Examples and Examples by arranging commercially used raw materials, which can be replaced with raw materials having similar properties at the same level. As the wax used in Comparative Example, soy wax and bees wax were used as natural waxes most often used in general candles. In addition, paraffin wax was used as a petroleum-based wax widely used in the manufacture of candles, and the melting point of general paraffin wax exists between 47°C and 60°C. In the present invention, paraffin wax is divided into low melting point and high melting point according to melting point. In the present invention, low melting point paraffin wax has a melting point of around 50° C., and high melting point paraffin wax has a melting point of about 70° C. was used.

In the present invention, the microcrystalline wax increases the melting point of the wax, strengthens the properties of the formulation, and affects the degree of impregnation of the fragrance. In the case of multi-wax, W-445 wax having a melting point of 82° C. was used among the waxes of Sonneborn. In addition, the invention was completed by mixing Mitsui's 410P having a melting point of 125°C and 400P having a melting point of 115°C.

In the present invention, a polymer and a surfactant were additionally used to complete the formulations of Comparative Examples and Examples.

Experimental Example 1: High-temperature evaluation

For high-temperature evaluation of the perfume composition according to the present invention, the present inventors judged whether it melted or bent by leaving it in a high-temperature oven at 90 ° C for 3 hours. After cooling, the intensity of the fragrance was evaluated on a scale of 1 to 5 to evaluate the relative reverberation. The evaluation criteria were the same as in Table 4 below based on the standard product at room temperature.

score Evaluation contents 1 point no odor 2 points Smell is very weak compared to standard products 3 points Smell is weaker than standard products 4 points Slightly weaker odor than standard products 5 points Same smell as standard product

Comparative Examples 1 to 3 are combinations of waxes generally used in scented candles. As a result of the evaluation at high temperature for Comparative Examples 1 to 3, all of the dripping occurred, and it was confirmed that the dripping degree was improved as the application amount of the petroleum-based high melting point paraffin wax was increased. This was judged to be due to the large amount of wax with a low melting point such as soy wax, and Comparative Example 2 to which the high melting point paraffin wax was applied maintained a more stable state than Comparative Example 1, but it was bent or melted than Comparative Example 3 using more high melting point paraffin wax. Falling was more severe.

In Examples 1 to 3 to which the microcrystalline wax having a high melting point in the present invention was applied, it was confirmed that the higher the melting point, the better the stability at high temperature. However, in the case of Example 1 to which the multi-wax having a low melting point was applied, it was confirmed that deformation occurred over time at 90°C. In addition, in Examples 2 and 3 to which a wax having a melting point of 110° C. or higher was applied, as the temperature increased, cracks and cracks on the surface appeared after aging at a high temperature, and thus the appearance was not good. This was determined to be because, in the case of a wax having a high melting point, the penetration rate of the liquid fragrance was lowered.

Examples 4 and 5 showed better results in surface cracking and stability over time when various types of microcrystalline wax were mixed and used. It was confirmed that the appearance quality was improved at the content of

In Examples 6 and 7, when petroleum-based waxes other than natural waxes, which are known to have compatibility with respect to fragrance, were mixed, they were superior in maintaining the appearance of appearance such as cracking, cracking, and warping, compared to the case where only microcrystalline wax was used. It was also confirmed that the characteristics of In addition, when soy wax having excellent compatibility with fragrances was applied, the smoothness of the surface was found to be the best. In terms of fragrance characteristics, it was found that when a wax having excellent compatibility for fragrance was mixed, the phenomenon of fragrance leakage was reduced even in the long-term room temperature fragrance evaluation.

When the reverberation strength was evaluated after elapsed time for 3 hours at a high temperature of 90°C, it was found that the reverberation property was also good when the shape was well maintained like the appearance quality. The results are shown in Table 5 below.

Comparative Example 1 Comparative Example 2 Comparative Example 3 Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 Average 0.8 1.1 1.5 2.7 2.9 2.9 3.5 4.0 4.0 4.1

Experimental Example 2: Evaluation of scent diffusing properties in space

In order to evaluate the scent diffusing properties of the Examples and Comparative Examples according to the present invention, the present inventors measured the intensity of the scent present in the space after 1 day and 7 days after leaving it at room temperature so that natural scent diffused in a 4.5 m ³ space. It was evaluated by a 5-point evaluation method.

A total of 10 evaluators were trained in advance for clear recognition. The evaluation was conducted one by one in a stand-alone evaluation booth equipped with forced ventilation facilities. In order to increase the accuracy of the evaluation, the evaluation of more than three at a time was limited.

Table 6 below is a standard for evaluating scent diffusing properties in a space.

score Evaluation contents 1 point Smells not very good 2 points smell not good 3 points Smell is normal 4 points smell good 5 points smells very good

The results are shown in Table 7 below. Similar results were obtained for the intensity of fragrance after aging at high temperature, and the degree of decrease in fragrance after 7 days was also found to be good.

Comparative Example 1 Comparative Example 2 Comparative Example 3 Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 7 1 day later 4.3 4.2 4.3 4.3 4.2 4.2 4.4 4.5 4.5 4.5 after 7 days 2.2 2.1 2.2 2.8 3.0 3.0 3.4 3.5 3.7 3.9

That is, the present inventors confirmed that the difference in scent diffusion according to the passage of time at room temperature was small as the appearance quality was maintained stable at 90°C and high temperature for 3 hours and there was no cracking or breakage.

Claims (7)

microcrystalline wax and paraffin wax;
The melting point of the microcrystalline wax is 110 ℃ to 150 ℃,
The melting point of the paraffin wax is 60 to 90 ℃,
Fragrance composition, characterized in that the melting point is 90 to 125 ℃. The method of claim 1,
The composition is perfume composition, characterized in that it further comprises a natural wax. The method of claim 1,
The composition is a fragrance composition, characterized in that it comprises 1 to 50% by weight of the total weight of the composition. 4. The method of claim 3,
The perfume has a log value of the partition coefficient of octanol/water of 3 to 8, and a perfume composition having a boiling point of 200 to 500° C. in an amount of 5 to 80% by weight based on the total weight of the perfume. The method of claim 1,
The microcrystalline wax is contained in an amount of 10 to 90% by weight based on the total weight of the composition. delete A fragrance comprising the composition according to any one of claims 1 to 5.