Oxidative hair dye composition

The two-layer structured hair dye composition, with oil on the upper surface to prevent oxidation, addresses issues of rapid dye oxidation and scalp irritation, achieving improved hair conditioning and dye retention while simplifying manufacturing.

WO2025110634A1PCT designated stage expired Publication Date: 2025-05-30UCL CO LTD

Patent Information

Application Number
PCT/KR2024/018060
Authority / Receiving Office
WO · WO
Patent Type
Applications
Current Assignee / Owner
Priority Date
2023-11-20
Filing Date
2024-11-15
Publication Date
2025-05-30

AI Technical Summary

Technical Problem

Existing hair dye compositions face challenges such as rapid oxidation of oxidizing dyes, scalp irritation, and hair damage due to the use of alkaline agents and hydrogen peroxide, and they often require complex nitrogen charging processes.

Method used

A two-layer structured first agent is used, where oil is positioned on the upper surface to prevent contact between oxygen and the oxidizing dye, thereby suppressing oxidation and reducing scalp irritation. This composition eliminates the need for nitrogen charging, simplifying the manufacturing process.

Benefits of technology

The use of a two-layer structured hair dye composition effectively inhibits oxidation, reduces scalp irritation, and provides better hair conditioning and dye retention, while also simplifying the manufacturing process and reducing costs.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention relates to an oxidative hair dye composition, and a hair dye comprising the oxidative hair dye composition, the oxidative hair dye composition comprising: a first agent comprising an oil and an oxidative dye; and a second agent comprising an oxidizing agent. The hair dye composition of the present invention contains the oil in the first agent so as to prevent contact between the oxidative dye and oxygen, and thus inhibits oxidation and provides excellent dye retention, conditioning and scalp protection effects.
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Description

Oxidizing hair dye composition

[0001] The present invention relates to an oxidative hair dye composition comprising a first agent comprising an oil and an oxidative dye; and a second agent comprising an oxidizing agent; and a hair dye comprising the oxidative hair dye composition.

[0002] Recently, as living standards have improved, interest in beauty has increased, and hair dyeing, which allows people to express their individuality, has become popular.

[0003] Among hair dyes for dyeing hair, oxidative hair dye compositions typically contain one or more oxidative dye intermediates and one or more couplers (first agent), and are mixed with an oxidizing agent (second agent) such as a hydrogen peroxide solution immediately before application to the hair to perform dyeing. The purpose of using such hair dyes is to dye hair as completely as possible and to maintain the dyeing effect for a long time.

[0004] Existing hair dye compositions are generally formed into a single formulation such as gel, cream, or liquid. In the case of cream formulations, there is the inconvenience of using them as they must be evenly applied to the hair using a separate tool such as a brush. In the case of liquid formulations, there is the inconvenience of using them as the liquid may flow down to the skin or contaminate the surrounding area during dyeing.

[0005] An oxidative hair dye composition is typically made by mixing a first agent including one or more oxidative dye precursors, one or more couplers, an alkaline agent, an antioxidant, and a reducing agent, and a second agent including hydrogen peroxide or the like immediately before the procedure and then applying the mixture to the hair to dye it. However, the first agent contains an oxidative dye and therefore oxidizes quickly, and the alkaline agent contained in the first agent and hydrogen peroxide in the second agent cause scalp irritation and hair damage. Active research is being conducted to solve these problems, and for example, methods to enhance the hair conditioning effect using silicone and cationic polymers have been studied. However, silicone can be harmful to the environment or biodiversity and can accumulate on the scalp, harming scalp health. Cationic polymers can also cause scalp itchiness and irritation. Therefore, there is an urgent need to develop a new hair dye that can prevent hair damage while maintaining the hair dyeing effect.

[0006] Korean Patent Publication No. 10-2020-0011674 discloses a hair dye additive composition containing coconut flower sugar, shrimp powder, and kelp powder, but does not separately disclose a composition for preventing self-oxidation of the first agent.

[0007] Against this backdrop, the inventors of the present invention have conducted extensive research efforts to develop a hair dye that can condition and prevent hair damage and protect the scalp, and as a result, have confirmed that when a first hair dye composition formed into a two-layer structure by including oil is prepared, oxidation is suppressed and scalp irritation is alleviated when dyeing with the hair dye composition, thereby completing the present invention.

[0008] The present invention aims to solve the above-mentioned problems and other problems related thereto.

[0009] One exemplary object of the present invention is to provide an oxidative hair dye composition comprising: a first agent comprising oil and an oxidative dye; and a second agent comprising an oxidizing agent.

[0010] Another exemplary object of the present invention is to provide a hair dye comprising the above-described oxidative hair dye composition.

[0011] The technical problem to be achieved according to the technical idea of ​​the invention disclosed in this specification is not limited to the problem to solve the above-mentioned problem, and other problems not mentioned will be clearly understood by those skilled in the art from the description below.

[0012] This is explained in detail as follows. Meanwhile, each description and embodiment disclosed in this application can also be applied to each other description and embodiment. In other words, all combinations of the various elements disclosed in this application fall within the scope of this application. Furthermore, the scope of this application is not limited by the specific descriptions described below.

[0013] As one aspect for achieving the above object, the present invention provides an oxidation hair dye composition comprising: a first agent including oil and an oxidizing dye; and a second agent including an oxidizing agent.

[0014] In the present invention, the first agent may be formed of a plurality of layers including an upper layer including the oil, and a lower layer formed below the upper layer and including the oxidizing dye.

[0015] In one embodiment of the present invention, the first agent may be formed of two layers including an upper layer containing the oil and a lower layer of water containing the oxidizing dye.

[0016] Conventional hair dyes contain oxidizing dyes that are prone to oxidation in the air, and thus, antioxidants and / or reducing agents are essential to prevent this. Furthermore, conventional hair dyes require nitrogen charging when filling containers with the dye, which complicates the process and is cost-effective. In contrast, the present invention positions oil on the upper surface of the first agent, thereby preventing contact between oxygen and the oxidizing dye, thereby inhibiting oxidation. Furthermore, a separate nitrogen charging process is unnecessary, simplifying the manufacturing process and providing superior economic efficiency.

[0017] In the present invention, the oil may be at least one selected from the group consisting of ester oil, hydrocarbon oil, silicone oil, and vegetable oil.

[0018] In the present invention, the ester oil is cetyl ethylhexanoate, dicaprylyl carbonate, isopropyl myristate, isopropyl palmitate, caprylic / capric triglyceride, triethylhexanoin, coco-caprylate / caprate, isoamyl laurate, C 12-15 It may be alkyl benzoate, tripentanoin, neopentanoate, neopentyl glycol diheptanoate, PEG-7 glyceryl cocoate, PEG-7 caprylic / capric glyceride, ethylhexyl palmitate, cetyl palmitate, dicaprylyl carbonate or cetyl ethylhexanoate.

[0019] In the present invention, the hydrocarbon oil is mineral oil, squalane, hydrogenated polydecene, undecane, tridecane, polybutene, hydrogenated polybutene or C 13-15 It could be an alkane.

[0020] In the present invention, the silicone oil may be dimethicone, cyclopentasiloxane, cyclohexasiloxane, diphenylsiloxyphenyl trimethicone, phenyl trimethicone, or caprylyl methicone.

[0021] In the present invention, the vegetable oil may be sweet almond oil, corn oil, soybean oil, rapeseed oil, cottonseed oil, coconut oil, apricot kernel oil, castor seed oil, meadowfoam seed oil, grape seed oil, macadamia seed oil, olive oil, sunflower seed oil, jojoba seed oil, argan kernel oil, avocado oil, green tea seed oil, evening primrose oil, camellia seed oil, baobab seed oil, yuzu seed oil, flaxseed oil, or Brazil nut seed oil.

[0022] In the present invention, the oil may be included in an amount of 5 parts by weight or more, specifically 8 parts by weight or more, and more specifically 10 parts by weight or more, based on 100 parts by weight of the first agent.

[0023] In one embodiment of the present invention, the oil may be included in an amount of 5 to 30 parts by weight based on 100 parts by weight of the first agent, specifically 5 to 25 parts by weight, and more specifically 5 to 20 parts by weight.

[0024] If the oil is less than 5 parts by weight based on 100 parts by weight of the first agent, it is impossible to completely block contact with air and thus prevent oxidation. If it is more than 30 parts by weight, the oil ratio is too high and the layer separation speed of the first agent may be very slow.

[0025] Specifically, in an embodiment of the present invention, it was confirmed that when the first agent containing 30% or 40% of oil was left for 24 hours, layer separation did not occur well, whereas when the first agent contained less than 30% of oil, layer separation occurred well.

[0026] In the present invention, the first agent may include a surfactant.

[0027] In the present invention, the HLB value (Hydrophile-Lipophile Balance) of the surfactant may be 10 to 30, specifically 10 to 25, and more specifically 10 to 21.

[0028] Specifically, in an embodiment of the present invention, when the HLB value of the surfactant included in the first agent was 10 or higher, the layer separation of the first agent was performed well at an appropriate speed, but when the HLB value was 3.7, 4.9, or 8, it was confirmed that the layer separation was slow, the water-soluble dye was decomposed, and the layer ratio was non-homogeneous.

[0029] In the present invention, the surfactant may be included in an amount of 0.1 to 1.5 parts by weight relative to 100 parts by weight of the first agent, and specifically, may be included in an amount of 0.3 to 1.5 parts by weight.

[0030] Specifically, in the examples of the present invention, when the first agent contained 0.3%, 0.8%, 0.5%, and 1% of the surfactant, respectively, the layer separation was well achieved, but when the surfactant was not included, the interface was uneven and the surface was not smooth, and when the surfactant was included at 2%, the layer separation was not achieved.

[0031] In the present invention, the surfactant may be at least one selected from an anionic surfactant, a nonionic surfactant, a cationic surfactant, and an amphoteric surfactant.

[0032] In the present invention, the anionic surfactant is sodium laureth sulfate, sodium lauryl sulfate, ammonium laureth sulfate, ammonium lauryl sulfate, mipa-laureth sulfate, potassium cocoyl glycinate, disodium laureth sulfosuccinate, sodium cocoyl isethionate, sodium C 14-16It may be at least one selected from among olefin sulfonate, sodium cocoyl glycinate, sodium lauroyl glutamate, sodium cocoyl alaninate, sodium methyl cocoyl taurate, and sodium lauroyl methylaminopropionate.

[0033] In the present invention, the nonionic surfactant may be at least one selected from among sorbitan sesquioleate, coceth-7, PPG-1-PEG-9-lauryl glycol ether, PEG-40-hydrogenated castor oil, PEG-60 hydrogenated castor oil, polysorbate 20, polysorbate 60, polysorbate 80, octyldodeceth-5, octyldodeceth-25, decyl glucoside, oleth-2, oleth-5, and oleth-10.

[0034] In the present invention, the cationic surfactant may be at least one selected from cetrimonium chloride, light trimonium chloride, behentrimonium chloride, daicocodimonium chloride, cetrimonium methosulfate, behentrimonium methosulfate, and steattrimonium chloride.

[0035] In the present invention, the amphoteric surfactant may be at least one selected from coco-betaine, disodium cocoamphodiacetate, cocamidopropyl betaine, lauryl betaine, cocamidopropyl hydroxysultaine, and cocamide mipa.

[0036] In the present invention, the oxidizing dye is p-nitro-o-phenylenediamine, 2-amino-4-nitrophenol, 2-amino-5-nitrophenol, 2-amino-3-hydroxypyridine, 5-amino-o-cresol, m-aminophenol, o-aminophenol, p-aminophenol, 2,4-diaminophenoxyethanol hydrochloride, toluene-2,5-diamine hydrochloride, m-phenylenediamine hydrochloride, p-phenylenediamine hydrochloride, hydroxypropylbis(N-hydroxyethyl-p-phenylenediamine hydrochloride), toluene-2,5-diamine, p-phenylenediamine, N-phenyl-p-phenylenediamine, picramic acid, p-nitro-o-phenylenediamine sulfuric acid, p-methylaminophenol sulfuric acid, 5-amino-o-cresol sulfuric acid, m-aminophenol sulfuric acid, o-aminophenol sulfuric acid, sulfuric acid It may be at least one selected from among p-aminophenol, toluene-2,5-diamine sulfate, m-phenylenediamine sulfate, p-phenylenediamine sulfate, N,N-bis(2-hydroxyethyl)-p-phenylenediamine sulfate, 2,6-diaminopyridine, 2,4-diaminophenol hydrochloride, 1,5-dihydroxynaphthalene, sodium picramic acid, 2-amino-5-nitrophenol sulfate, o-chloro-p-phenylenediamine sulfate, 1-hydroxyethyl-4,5-diaminopyrazole sulfate, hydroxybenzomorpholine, 6-hydroxyindole, α-naphthol, resorcinol, 2-methylresorcinol, gallic acid, catechol, and pyrogallol.

[0037] In the present invention, the oxidative dye may be present in an amount of 0.001 to 5 parts by weight relative to 100 parts by weight of the first agent.

[0038] In the present invention, the first agent may further include a coupler.

[0039] The above coupler may be at least one selected from 2-methyl-5-hydroxyethylaminophenol, p-amino-o-cresol, m-aminophenol, 2,4-diaminophenoxyethanol hydrochloride, m-phenylenediamine hydrochloride, m-phenylenediamine, N-methyl-p-phenylenediamine, p-amino-o-cresol sulfate, 4-ethoxym-phenylenediamine sulfate, m-phenylenediamine sulfate, α-naphthol, resorcinol, and 2-methylresorcinol.

[0040] In the present invention, the coupler may be present in an amount of 0.001 to 5 parts by weight relative to 100 parts by weight of the first agent.

[0041] In the present invention, the first agent may further include an alkaline agent.

[0042] The above alkaline agent may be at least one selected from ammonia water, monoethanolamine, triethanolamine, arginine, aminomethylpropanol, sodium hydroxide, potassium hydroxide, ammonium bicarbonate, sodium bicarbonate, and sodium carbonate.

[0043] In the present invention, the alkaline agent may be present in an amount of 0.01 to 20 parts by weight relative to 100 parts by weight of the first agent.

[0044] In the present invention, the first agent may further include a metal ion sequestering agent, an antioxidant, and / or a conditioning agent.

[0045] In the present invention, the metal ion sequestering agent may be at least one selected from among EDTA, EDTA-2NA, EDTA-3NA, EDTA-4NA, tetrasodium etidronate, etidronic acid, pentasodium pentitate, sodium stannate, and tetrasodium pyrophosphate.

[0046] In the present invention, the metal ion sequestering agent may be 0.01 to 1 part by weight relative to 100 parts by weight of the first agent.

[0047] In the present invention, the antioxidant may be at least one selected from ascorbic acid, erythorbic acid, sodium sulfite, cysteine, cysteine ​​hydrochloride, thioglycolate, and thioglycolic acid.

[0048] In the present invention, the antioxidant may be present in an amount of 0.01 to 2 parts by weight relative to 100 parts by weight of the first agent.

[0049] In the present invention, the conditioning agent may be at least one selected from a cellulose-based thickener, a cationic polymer, and a polyol.

[0050] In the present invention, the second agent may further include a solvent, a thickener, a pH regulator, an oxidizing agent, a conditioning agent, and / or a metal ion sequestering agent.

[0051] In the present invention, the thickener is carbomer, acrylate / beheneth-25 methacrylate copolymer, acrylate / ceteth-20 itaconate copolymer and acrylate / C. 10 - 30 It may be at least one selected from among alkyl acrylate crosspolymers.

[0052] In the present invention, the thickener may be 1 to 10 parts by weight relative to 100 parts by weight of the second agent.

[0053] In the present invention, the pH adjusting agent may be at least one selected from disodium phosphate, phosphoric acid, and salicylic acid.

[0054] In the present invention, the pH regulator may be present in an amount of 0.01 to 5 parts by weight relative to 100 parts by weight of the second agent.

[0055] In the present invention, the oxidizing agent may be hydrogen peroxide, but is not limited thereto.

[0056] In the present invention, the oxidizing agent may be present in an amount of 2.5 to 12 parts by weight relative to 100 parts by weight of the second agent.

[0057] In the present invention, the conditioning agent may be at least one selected from a cellulose-based thickener, a cationic polymer, and a polyol.

[0058] In the present invention, the metal ion sequestering agent may be at least one selected from EDTA, EDTA-2NA, EDTA-3NA, EDTA-4NA, tetrasodium etidronate, etidronic acid, pentasodium pentitate, sodium stannate, and tetrasodium pyrophosphate.

[0059] In the present invention, the metal ion sequestering agent may be 0.01 to 1 part by weight relative to 100 parts by weight of the second agent.

[0060] As another aspect for achieving the above object, the present invention provides a hair dye comprising the above oxidative hair dye composition.

[0061] In accordance with the present invention, the hair dye may be in one or more formulations selected from the group consisting of cream, gel, liquid, powder, aerosol, and emulsion.

[0062] The hair dye composition of the present invention contains oil in the first agent to prevent contact between the oxidizing dye and oxygen, thereby inhibiting oxidation and providing excellent dye retention, conditioning, and scalp protection effects.

[0063] Figure 1 shows the results of confirming layer separation according to the presence or absence of oil by observing with the naked eye 24 hours and 7 days after manufacturing the first agent of the present invention (Comparative Example 3 and Example 1).

[0064] Figure 2 shows the results of confirming the layer separation speed according to the HLB value of the surfactant by observing with the naked eye after 0 hour, 0.5 hour, and 12 hours of manufacturing the first agent of the present invention (Comparative Examples 4 to 6, Example 10, Example 12, and Example 13).

[0065] Figure 3 shows the results of observing with the naked eye 24 hours after manufacturing the first agent of the present invention (Comparative Example 1, Comparative Example 2, Example 1, Example 8, Example 9, Example 10) to determine the layer separation speed according to the surfactant content.

[0066] Figure 4 shows the results of observing with the naked eye 24 hours after manufacturing the first agent of the present invention (Comparative Example 3, Example 1, Example 2, Example 3, Example 11) to confirm the layer separation speed according to the type of oil.

[0067] Figure 5 shows the results of observing with the naked eye 24 hours after manufacturing the first agent of the present invention (Comparative Example 3, Example 1, and Examples 4 to 7) to determine the layer separation speed according to the oil content.

[0068] Figure 6 shows the results of confirming the scalp protection effect of a hair dye composition manufactured by including each of the first agents of the present invention (Comparative Example 3, Example 1).

[0069]

[0070] Hereinafter, the present invention will be described in more detail through the following examples. However, these examples are intended to exemplify the present invention and the scope of the present invention is not limited to these examples.

[0071]

[0072] Example 1: Preparation of hair dye composition

[0073] 1-1. Manufacturing of the first product

[0074] The first composition containing oil was prepared with the composition ratios shown in Tables 1 and 2 below (Examples 1 to 13). PEG-40-hydrogenated castor oil (coceth-7, PPG-1-PEG-9-lauryl glycol ether, PEG-40-hydrogenated castor oil), cetrimonium chloride, sodium laureth sulfate, disodium cocoamphodiacetate, sorbitan sesquioleate or oleth-2 was applied as the surfactant, and mineral oil, cetyl ethylhexanoate, sweet almond oil or dimethicone was applied as the oil.

[0075] No. Ingredient name Example 1 Example 2 Example 3 Example 4 Example 5 Example 6 Example 71 Purified water 78.300 78.300 78.300 83.3000 68.300 58.300 48.300 2 Hydroxyethyl cellulose 0.4000 4000 4000 4000 4000 4000 4000 3 Polyquaternium-71 0001 0001 0001 0000 1 0001 0001 0001 000 4 Propylene glycol 2.000 2 000 2 000 2 000 2 000 2 000 2 000 5 Disodium EDTA 0.1000 1000 1 000 1 0000.1000.1000.1006Ascorbic Acid0.5000.5000.5000.5000.5000.5000.5007Sodium Sulfite0.3000.3000.3000.3000.3000.3000.3008Sodium Chloride0.5000.5000.5000.5000.5000.5000.5009Colorant1.2001.2001.2001.2001.2001.2001.2001.20010Fragrance0.2000.2000.2000.2000.2000.20011PEG-40-Hydrogenated Castor Oil 0.5000.5000.5000.5000.5000.5000.5000.50012 Cetrimonium Chloride 13 Sodium Laureth Sulfate 14 Disodium Cocoamphodiacetate 15 Sorbitan Sesquioleate 16 Olethe-2 17 Ethanolamine 5.00005.00005.00005.00005.00005.000018 Mineral Oil 10.000 5.00020.00030.00040.00019 Cetyl Ethylhexanoate 10.000 20 Sweet Almond Oil 10.000 21 Dimethicone

[0076] ※ Indicated as weight % based on 100 parts by weight of the first component

[0077] No. Ingredient name Example 8 Example 9 Example 10 Example 11 Example 12 Example 13 1 Purified water 78.5000 78.0000 77.8000 78.300 77.8000 77.8000 2 Hydroxyethyl cellulose 0.40000 40000 40000 40000 4000 3 Polyquaternium-71 1.0000 1.0000 1.0000 1.0000 1.0000 1.0000 4 Propylene glycol 2.0000 2.0000 2.0000 2.0000 2.0000 2.0000 5 Disodium EDTA 0.10000 10000 1 0000.1000.10000.10006Ascorbic Acid0.50000.50000.50000.50000.50000.50007Sodium Sulfite0.30000.30000.30000.30000.30008Sodium Chloride0.50000.50000.50000.50000.50009Colorant1.2001.2001.2001.2001.2001.2001.20010Fragrance0.20000.20000.20000.20000.200011PEG-40-Hydrogenated Castor Oil 0.30000.8000 1.00000.500 12 Cetrimonium Chloride 1.000 13 Sodium Laureth Sulfate 1.000 14 Disodium Cocoamphodiacetate 15 Sorbitan Sesquioleate 16 Olethe-2 17 Ethanolamine 5.0000 5.0000 5.0000 5.0000 5.0000 5.0000 18 Mineral Oil 10.000 10.000 10.000 10.000 19 Cetyl Ethylhexanoate 20 Sweet Almond Oil 21 Dimethicone 10.000

[0078] ※ Indicated as weight % based on 100 parts by weight of the first component

[0079] In addition, Comparative Examples 1 to 6 were manufactured by changing the composition ratio as shown in Table 3 below.

[0080] No. Ingredient name Comparative example 1 Comparative example 2 Comparative example 3 Comparative example 4 Comparative example 5 Comparative example 6 1 Purified water 78.8000 76.800 88.300 77.8000 77.8000 77.8000 2 Hydroxyethyl cellulose 0.40000 4000 4000 4000 4000 4000 3 Polyquaternium-71 1.0000 1.000 1.0000 1.0000 1.0000 1.0000 4 Propylene glycol 2.0000 2.000 2.000 2.000 2.000 2.000 5 Disodium EDTA 0.10000 1000 100 0.10000.10000.10006Ascorbic Acid0.50000.5000.5000.50000.50000.50007Sodium Sulfite0.30000.3000.3000.30000.30000.30008Sodium Chloride0.50000.5000.5000.50000.50000.50009Colorant1.2001.2001.2001.2001.2001.20010Fragrance0.20000.2000.20000.20000.200011PEG-40-Hydrogenated Castor Oil 0.0000 2.0000 500 12 Cetrimonium Chloride 13 Sodium Laureth Sulfate 14 Disodium Cocoamphodiacetate 1.000 15 Sorbitan Sesquioleate 1.000 16 Olethe-2 1.000 17 Ethanolamine 5.0000 5.0000 5.0000 5.0000 5.0000 5.0000 18 Mineral Oil 10.000 10.000 10.000 10.000 19 Cetyl Ethylhexanoate 20 Sweet Almond Oil 21 Dimethicone

[0081] ※ Indicated as weight % based on 100 parts by weight of the first component

[0082]

[0083] 1-2. Secondary manufacturing

[0084] The second agent was prepared with the composition ratio shown in Table 4 below (Examples 14 to 16). Specifically, xanthan gum, carbomer, acrylate / ceteth-20 itaconate copolymer, and acrylate / C10-30 alkyl acrylate crosspolymer were added to purified water and stirred with an Agi mixer, then propylene glycol, disodium EDTA, etidronic acid, disodium phosphate, and phosphoric acid were added, heated to 78°C to dissolve, cooled to 40°C, and hydrogen peroxide was added and stirred to prepare the second agent.

[0085] No. Ingredient name Content (%) Example 14 Example 15 Example 16 1 Purified water 90.9 30 91.7 30 90.7 30 2 Xanthan gum 0.1000.1000.100 3 Carbomer 1.800--4 Acrylates / Ceteth-20 Itaconate copolymer-1.000-5 Acrylates / C10-30 alkyl acrylate crosspolymer--2.000 6 Pr Propylene Glycol 1.000 1.000 1.000 7 Disodium EDTA 0.0500 0500 0508 Etidronic Acid 0.1200 1200 1209 Disodium Phosphate 0.3500 3500 35010 Phosphoric Acid 0.0500 0500 05011 Hydrogen Peroxide 5.600 5.600 5.600

[0086] ※ Indicated as weight % based on 100 parts by weight of the second component

[0087]

[0088] 1-3. Preparation of hair dye composition

[0089] The first agent (Example 1) and the second agent (Examples 14 to 16) were mixed in a weight ratio of 1:1, and the viscosity was measured using an LVDV-II+Pro Brookfield Viscometer (64 pin, 12 rpm, 1 min). The results are shown in Table 5.

[0090] Example 1 Example 1 Example 1 Example 1 Example 1 Example 2 Example 14 Example 15 Example 16 Viscosity (rpm) 21,895 25,447 22,593 Properties No flowability No flowability No flowability

[0091] In addition, the first agent (Examples 1 to 13) and the second agent (Examples 14 to 16) were mixed in different combinations at a weight ratio of 1:1 to prepare an oxidizing hair dye composition, which was used for the evaluation of dye retention, conditioning, and wool and scalp protection effects described below.

[0092]

[0093] Example 2: Evaluation of oxidation power and degree of layer separation of the first agent

[0094] 2-1. Oxidizing power evaluation

[0095] The first compositions of Example 1 and Comparative Example 3 were opened and left at room temperature for 24 hours or one week, respectively, and then the color degree was checked with the naked eye. Example 1 contains mineral oil, and Comparative Example 3 is a first composition that does not contain oil.

[0096] As a result, it was confirmed that the color of Comparative Example 3 became darker than that of Example 1 after one week (Fig. 1), which suggests that the oil layer included in the composition of Example 1 is located on the upper part of the aqueous phase containing the dye, thereby blocking oxygen in the air and preventing oxidation of the dye. In other words, the two-layer hair dye composition including the oil phase (oil layer) on the upper part of the aqueous phase was evaluated to have an oxidation inhibition effect of the dye even without nitrogen filling, and thus has not only long-term storage stability but also economic utility due to the absence of packaging.

[0097] 2-2. Evaluation of layer separation speed according to the HLB value of the surfactant

[0098] By applying different surfactants, the HLB value (Hydrophile-Lipophile Balance,

[0099] Comparative examples 4 to 6, examples 10, 12, and 13, each having a different hydrophilic-lipophilic balance, were left at room temperature and the layer separation was observed visually over time (0 h, 0.5 h, 12 h).

[0100] The separation speed according to the difference in HLB value was compared, and the separation time suitable for use in mass production is when the separation begins gradually about 1 hour after manufacturing and the separation is completely maintained after 12 hours.

[0101] As a result, in Comparative Example 4, which used sorbitan sesquioleate (HLB 3.7) as a surfactant, the layer separation speed was too slow, and in Comparative Example 5, which used oleth-2 (HLB 4.9), the water-soluble dye was decomposed as it emulsified in the oil layer. In Comparative Example 6, which used disodium cocoamphodiacetate (HLB 8), the layer separation started quickly even before 0.5 hours after standing, indicating that the layer ratio between products may be non-homogeneous when filling the product. On the other hand, in Example 10, which used PEG-40-hydrogenated castor oil (HLB 13.1) as a surfactant, in Example 12, which used cetrimonium chloride (HLB 21), and in Example 13, which used sodium laureth sulfate (HLB 10.4), an appropriate separation speed was shown (Fig. 2).

[0102]

[0103] 2-3. Evaluation of layer separation speed according to surfactant content

[0104] The effect of the surfactant content in the first agent on layer separation was confirmed. As a result of comparing layer separation by leaving i) Comparative Example 1 without surfactant, ii) Comparative Example 2 with 2% surfactant, iii) Example 1 with 0.5% surfactant, iv) Example 8 with 0.3% surfactant, v) Example 9 with 0.8% surfactant, and vi) Example 10 with 1% surfactant for 24 hours, it was confirmed that Examples 1, 8, 9, and 10 separated well. On the other hand, Comparative Example 1 without surfactant separated layers immediately and the interface was uneven, so the surface was not smooth, and Comparative Example 2 with 2% surfactant showed almost no layer separation (Fig. 3).

[0105]

[0106] 2-4. Evaluation of layer separation speed according to oil type and content

[0107] Comparative Example 3, Example 1 (mineral oil application), Example 2 (cetyl ethyl hexanoate application), Example 3 (sweet almond oil application), and Example 11 (dimethicone application), each containing different types of oil, were left at room temperature for 24 hours, and the degree of separation was observed with the naked eye.

[0108] As a result, it was confirmed that Comparative Example 3, which did not contain oil, did not exhibit layer separation, and that Examples 1, 2, 3, and 11 achieved sufficient separation. However, in the case of Example 3, it was confirmed that the polarity of the oil was somewhat low, so some of it was emulsified in the water portion and appeared cloudy (Fig. 4).

[0109] In addition, the degree of separation was compared after leaving Comparative Example 3, Example 4 (oil content 5%), Example 1 (oil content 10%), Example 5 (oil content 20%), Example 6 (oil content 30%), and Example 7 (oil content 40%), each having a different oil content, at room temperature for 24 hours.

[0110] As a result, it was found that layer separation did not occur well in Examples 6 and 7 with high oil content (Fig. 5).

[0111]

[0112] Example 3: Evaluation of dye retention and hair protection effect of oxidative hair dye composition

[0113] 3-1. Color fastness (dye retention) evaluation

[0114] A hair dye composition manufactured as a first agent in Comparative Example 3 without oil, and a hair dye composition manufactured as Examples 1 to 7 and Example 11 including oil, and a second agent manufactured as Example 14 were each mixed in a ratio of 1:1, and the mixture was evenly applied to a hair sample for testing, left for 30 minutes, and then washed in running water using shampoo. Afterwards, the color was measured using a spectrophotometer (Konica Minolta CM-5) on hair dried using a hair dryer and hair that had been repeatedly shampooed 5 times, to evaluate the dyeing retention (fastness).

[0115] *The larger the + value of *a, the closer it is to red, and the larger the - value, the closer it is to green. The larger the + value of *b, the closer it is to yellow, and the larger the - value, the closer it is to blue. The ΔE*ab value is a standard deviation value that measures the difference from the standard color. A larger value indicates a greater change in color, and a smaller value indicates a smaller change in color.

[0116] The fastness was compared using the ΔE*ab value measured with a spectrophotometer (Konica Minolta CM-5). Dry hair after shampooing once was set as the standard value, and the ΔE*ab value of hair shampooed five times was measured a total of three times to obtain the average ΔE*ab value.

[0117] The smaller the ΔE*ab value, the less color change there is, indicating better dye retention.

[0118] As a result of comparing the fastness, it was confirmed that the dyeing retention of Examples 1 to 7 and Example 11 was significantly superior (Table 6).

[0119]

[0120] 3-2. Evaluation of conditioning effects

[0121] The conditioning effect of the hair dye compositions manufactured by applying the first agent of Comparative Example 3, Examples 1 to 7, and Example 11, respectively, was measured. That is, the frictional force of experimental hair weighing 1.5 g and 100 mm in length was measured using a friction coefficient tester (Neo-Tribo (FCMS 170)), and each of the hair dye compositions containing Comparative Example 3, Examples 1 to 7, and Example 11 was evenly applied to the same hair. After drying the hair, the frictional force was measured again using a friction coefficient tester (Neo-Tribo (FCMS 170)). The smaller the average value of the friction coefficient, the better the hair conditioning effect.

[0122] As a result, as shown in Table 7, the friction coefficient values ​​of Examples 1 to 7 and Example 11 containing oil were lower than those of Comparative Example 3 containing no oil, confirming that when the hair dye composition contained oil, it exhibited a better conditioning effect than when it did not.

[0123]

[0124]

[0125] 3-3. Wool Effect Evaluation

[0126] The hair growth effect was evaluated when the first agent of Comparative Example 3, Example 1, Examples 3 to 5, and Example 7 was applied. The hair growth effect is a measure of how thick and healthy hair can grow. The hair dye composition prepared for each experimental group was applied to hair samples and dried. Then, the gloss band, which appears as light scattering on the hair surface under a constant light, was photographed and analyzed for evaluation. The photographed image was used to extract the gloss band using an analysis program, and the pixel value of the area occupied by the gloss band compared to the total area was calculated. As the area of ​​the gloss band increases, the glossiness increases.

[0127] As a result, as shown in Table 8, it was confirmed that the area of ​​the Gloss band significantly increased in Examples 1, 3, 5, and 7 containing 10 to 40% oil compared to Comparative Example 3 containing no oil. However, Example 4 containing 5% oil showed an area value similar to that of Comparative Example 3.

[0128]

[0129]

[0130] 3-4. Evaluation of scalp protection effect

[0131] Ten adult men and women without skin diseases were tested, and 20 μl of the hair dye composition of Comparative Example 3 and the hair dye composition of Example 1 were applied to the skin of the arm area, respectively, and then fixed with an ECODERM IQ Ultra Patch and applied for 8 hours.

[0132] The visual evaluation by the tester was conducted according to the following criteria (Table 9) reflecting the Frosch & Kligman and The Cosmetic, Toiletry, and Fragrance Association (CTFA) guidelines (* 4 subjects were excluded from the experiment due to contact dermatitis at the patch contact area).

[0133] Symbol Score Criteria +1 Slight erythema, spotty or diffuse ++2 Moderate uniform erythema +++3 Severe erythema with edema +++4 Severe erythema with edema and blisters

[0134] As a result, when the first agent containing oil (Example 1) was applied, it was confirmed that the irritation value was lower than that of the first agent not containing oil (Comparative Example 3), indicating that it was effective in alleviating skin irritation (Fig. 6). From the above description, those skilled in the art will understand that the present invention can be implemented in other specific forms without changing the technical idea or essential characteristics thereof. In this regard, it should be understood that the embodiments described above are exemplary in all aspects and not restrictive. The scope of the present invention should be interpreted as including within the scope of the present invention all changes or modifications derived from the meaning and scope of the claims described below and their equivalent concepts rather than the above detailed description.

Claims

1. A first agent comprising oil and an oxidizing dye; and An oxidizing hair dye composition comprising a second agent comprising an oxidizing agent.

2. In paragraph 1, An oxidizing hair dye composition, wherein the first agent is formed of a plurality of layers, including an upper layer including the oil, and a lower layer formed below the upper layer and including the oxidizing dye.

3. In paragraph 1, An oxidizing hair dye composition, wherein the oil is at least one selected from the group consisting of ester oil, hydrocarbon oil, silicone oil, and vegetable oil.

4. In paragraph 1, An oxidizing hair dye composition, wherein the oil is contained in an amount of 5 to 30 parts by weight, based on 100 parts by weight of the first agent.

5. In paragraph 1, An oxidizing hair dye composition, wherein the first agent comprises a surfactant.

6. In paragraph 5, An oxidizing hair dye composition, wherein the HLB value (Hydrophile-Lipophile Balance) of the surfactant is 10 to 30.

7. In paragraph 5, A giant, oxidizing hair dye composition, wherein the surfactant is contained in an amount of 0.1 to 1.5 parts by weight based on 100 parts by weight of the first agent.

8. A hair dye comprising the oxidizing hair dye composition of paragraph 1.

9. In paragraph 8, The above hair dye is a hair dye having at least one formulation selected from the group consisting of a cream, a gel, a liquid, a powder, an aerosol, and an emulsion.

Citation Information

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