KR100838996B1 - Composition for coloring hair containing extracts of citrus and Method of manufacturing the same - Google Patents

Abstract

The present invention relates to a composition for the hair dye using a natural extract and a manufacturing method, specifically 85 to 93% by weight of the extract obtained from one or more of the leaves, skin and fruit of citrus fruits; 0.5 to 3% by weight of the dye agent; And a first agent comprising at least one selected from the group consisting of perfumes, fungicides, anti-inflammatory agents, preservatives, antioxidants, ultraviolet absorbents, ammonia water, ammonium glycolate, fatty acid alcohols, water and potassium alum. And it relates to a hair dye composition comprising a second agent comprising 85 to 90% by weight of the extract and the remaining amount of the first agent oxidizing agent and pH adjusting agent.

The hair dye composition and preparation method of the present invention alleviate or eliminate side effects due to the chemical component of the hair dye, and show excellent results in terms of hair protection and dyeing effect.

Citrus Extracts, Hair Colorants

Description

Composition for coloring hair containing extracts of citrus and Method of manufacturing the same}

The present invention relates to a hair dye composition comprising an extract from citrus leaves, skin or fruit (hereinafter referred to as "citrus fruit extract"), and a method of manufacturing the same, which has little side effects (skin and eye mucosal irritation) on the human body and is dyed. The present invention relates to a hair dye composition and a method for preparing a hair dye comprising a natural extract having a very soft hair, such as a treatment which is very fast (within 3-15 minutes), and is treated after hair dyeing unlike other hair dyes.

Hair dyes can be classified into permanent hair dyes, semi-permanent hair dyes, and temporary hair dyes depending on the difference in dyeing effects.

Permanent hair dyes are those in which the pigment-forming substance penetrates into the cortex or anhydrous layer inside the hair, causing chemical changes to form insoluble pigments. Semipermanent hair dyes are those in which the pigment itself penetrates into the cuticle layer of the cortex or hair surface and is physically adsorbed. Temporary hair dyes are also those that physically adsorb the pigment only to the cuticle layer, which is the surface of the hair.

The permanent hair dye may be divided into three types, namely, a vegetable hair dye, a metal hair dye, and an oxidative hair dye. Vegetable hair dyes include henna or chamomile and have a low dyeing effect and are difficult to lightly dye. Metallic hair dyes use the principle of blackening when lead is oxidized. Toxic harmful to humans is rarely used at present. Lastly, oxidative hair dyes have excellent dyeing effects and can be dyed in bright colors.

Oxidative hair dyes include the main components of Table 1 (first agent) and Table 2 (second agent) below.

division Characteristic Dye Intermediates It is not a pigment itself, but a substance that turns into a pigment when oxidized, eg p-phenylenediamine, p-aminophenol, p-toluenediamine Dye Modifier Substances that react with dye intermediates to vary color, eg resorcin, m-aminophenol, m-phenylenediamine Alkaline It opens the cuticles and allows the pigmentation reaction to occur quickly. Ex) ammonia, monoethanolamine (MEA) Higher fatty acids Reacts with alkaline agents to form higher fatty acid salts. It facilitates the penetration of dye intermediates or dye modifiers and facilitates cleaning on trituration. Gelling agent When mixed with a second agent it forms a gel. Isocetyl alcohol solvent Helps dissolve dye intermediates, dye modifiers. Ex) isopropyl alcohol

division Characteristic Oxidant Destroys the melanin pigment in the hair, decolorizing the hair and at the same time reacting the dye intermediates and dye modifiers to make new pigments. pH regulator The pH is adjusted to around 4.0 to stabilize hydrogen peroxide.

However, the dye intermediates and dye modifiers of the diamine-based organic dyes of the main components as described above irritate the skin and bind to the skin cells to act as antigens, such as redness, rash, pruritus, heart margin, inflammation, blisters, etc. People with sensitive skin can develop side effects, namely contact dermatitis, and can suffer from contact allergic dermatitis. In addition, the irritation causes harmful effects on the human body, such as when the hair dye enters the eye, which causes a great adverse effect on the eye.

In addition, chemically synthesized materials have problems such as damaging hair or having an irritating odor. And, there is a disadvantage that it takes a long time of about 30 to 40 minutes before hair dye is completed.

An object of the present invention is to solve the above problems, to provide a composition and a method for manufacturing a hair dye comprising a citrus extract having no or harmful action on the human body.

Specifically, the present invention provides a composition for hair dye comprising a citrus extract and a method for producing the same.

In order to achieve the above object, the present invention provides a composition for hair dye comprising an extract obtained from the leaves, peel or fruit of citrus fruits.

Citrus fruits are the fruit trees belonging to the dicotyledonous horticulture and citrus subfamily, and are the generic name of each species belonging to citrus, golden persimmon and tangerine among the citrus subfamily and varieties derived from these three genera. Citrus origins extend to India, Myanmar, Malay Peninsula, Indochina, China, Korea, and Japan, particularly the eastern Himalayas, the Assam, and the upstream of the Yangtze River in China. There is a will. It has been cultivated since ancient times in these provinces.

Citrus fruits are alkaline foods, and they are known to be effective in preventing colds by smoothing metabolism and strengthening skin and mucous membranes.

Citrus fruit extract used in the present invention is used by mixing one or two or more of the leaves, skin and fruit. In addition, the present invention can use extracts of citron, lemon, grapefruit, orange, lime, citron or tanza leaves, skin and fruit belonging to citrus fruits.

Citrus fruit extract of the present invention can be extracted by hot water extraction or solvent extraction method.

The extract may be used in the form of a concentrated extract or powder form hot-air dried it.

To obtain the extract, the leaves, skin or fruit of the citrus fruits are washed well and dried, which are then pulverized, that is, the raw materials are put in water and heated to extract hot water, or a hydrophilic organic solvent, a functional organic solvent or a chin The solvent can be extracted in an oily organic solvent.

Hot water extraction is to put 50 to 150 parts by weight of water with respect to 1 part by weight of citrus fruit raw material is heated for 8 to 12 hours at 100 to 120 ℃.

Solvent extraction is to put 30 to 100 parts by weight of an organic solvent per 1 part by weight of the raw material is extracted for 5 to 10 hours at 40 ~ 50 ℃. Preferably extraction is carried out at 45 ° C. for 8 hours.

The extract thus obtained may be concentrated and used in extract form, or may be powdered and stored.

The hydrophilic organic solvent may be methanol, ethanol, acetone, dioxane, tetrahydrofuran or n-propenol. The hydrous organic solvent may be hydrous methanol, hydrous ethanol or hydrous acetone. In addition, the lipophilic organic solvent may be n-butanol, n-hexane, ethyl acetate or benzene.

In particular, in the case of solvent extraction, the extract is filtered and concentrated to remove the solvent to obtain an extract form of extract. In addition, the organic solvent layer is separated after extraction and dried to obtain a dried product.

The hair dye composition and preparation method of the present invention comprises 85 to 93% by weight of the extract obtained from at least one of the leaves, skin and fruit of citrus fruits; 0.5 to 3% by weight of the dye agent; And a first agent comprising at least one selected from the group consisting of perfumes, fungicides, anti-inflammatory agents, preservatives, antioxidants, ultraviolet absorbents, ammonia water, ammonium glycolate, fatty acid alcohols, water and potassium alum. And a second agent comprising 85 to 90% by weight of the citrus extract and a residual amount of an oxidizing agent and a pH adjusting agent to oxidize the first agent.

In addition, the first agent may further include 0.1 to 5% by weight of the foaming agent.

It is because the first agent and the second agent in the composition for hair dyes of the present invention include the citrus extracts in the above-defined range in view of achieving the effect of the present invention. That is, when the citrus fruit extract is included in the above range, the effect of the present invention cannot be sufficiently achieved, and when the citrus extract is included in the above range, it is no longer expected to improve the effect due to the increase of the extract.

On the other hand, the dye agent of the hair dye composition of the present invention can be adjusted according to the type and color of the hair to be represented, preferably 0.5 to 3% by weight based on the total hair dye composition, more preferably 1 weight % Or less If it is out of the above range, it is because a problem occurs that it is difficult to obtain the desired hair dye effect. That is, the dye agent below the above range does not achieve the hair dye effect, and if it exceeds the above range because the relative amount of the citrus extract in the composition is reduced to achieve the effect of the present invention.

In addition, when the composition for hair dyes of the present invention includes the foaming agent in the above-defined range, the foaming effect cannot be sufficiently obtained when it is included in the above-described range. When the composition is included in the above-mentioned range, foaming occurs excessively and the composition easily flows. It is because it is unpreferable since it becomes a shape which throws away and reduces a hair dye effect.

The foaming agent may be at least one selected from anionic surfactants such as saponin and sodium alkyl sulfate, nonionic surfactants added with alkyl fatty acid polyoxyethylene, and betaine type amphoteric surfactants.

In the hair dye composition of the present invention, the foaming agent forms a fine bubble to facilitate hair dyeing in a short time by promoting oxidation of the oxidizing agent. In addition, by allowing the hair dye to reach the hair roots by the delicate foam, it is possible to achieve a uniform hair without a part that is not dyed. And the hair dye is prevented from flowing out by the delicate foam, and the so-called application of the hair dye is improved.

Citrus extract of the present invention helps to regenerate and strengthen the cuticle layer on the surface of the hair after hair dyeing, thereby preventing hair retention and nutrients. Therefore, it can protect hair, promote activation, and improve hair dyeing effect.

The present invention may be a form in which the first agent and the second agent are each provided in a packaged form and then mixed and used in use.

The hair dye composition of the present invention can be used in a gel form (liquid and cream form) in which the first agent and the second agent are mixed.

The composition for hair dyes of the present invention divides the citrus extracts into the first agent and the second agent because the amount of the citrus extract is overwhelmingly large compared to the amount of the dye agent or the oxidant (the whole composed of the first agent and the second agent) Citrus extract content of 200 wt% of hair dye composition is 180 wt% or more), dye (first agent) and oxidizing agent (second agent) are equally dispersed in the citrus extract, This is to ensure that the mixing process of the oxidant is not disturbed. That is, the citrus extract is to be divided into the first agent and the second agent in the hair dye composition and method for the rapid and uniform mixing of the dye agent and the oxidizing agent, respectively.

The oxidizing agent and the pH adjusting agent may be ones commonly used in the field of hair dyes. Most preferably, hydrogen peroxide water is used as an oxidant and phosphoric acid is used as a pH adjuster.

The hair dye composition and preparation method of the present invention include compounds commonly used in hair dyes, that is, fragrances, bactericides, anti-inflammatory agents, preservatives, antioxidants, ultraviolet absorbers, ammonia water, ammonium glycolate, fatty acid alcohols, water or potassium alum. Can be.

In addition, the dye including the dye in the hair dye composition and method of the present invention is added to exhibit a variety of colors, the type of the dye may include all dyes that can be commonly used in the field of hair dye. As diamine organic dye, p-phenylenediamine, m-phenylenediamine, o-phenylenediamine, p-nitro-o-phenylenediamine, n-phenyl-p-phenylenediamine, 4-ethoxy-m sulfate -Phenylenediamine, toluene sulfate-2.5-diamine and the like can be used.

The oxidation of the contents should be prevented in order to maintain the quality of the hair dye composition and the preparation method of the present invention during storage. Therefore, the composition and the manufacturing method for the hair dye of the present invention may be a packaging material having an oxygen blocking effect, preferably a packaging material in which a synthetic resin and a thin aluminum foil are laminated.

When using the hair dye composition and preparation method of the present invention, the first agent and the second agent are uniformly mixed and used in the form of liquid gel and cream.

The present invention will be described through the following examples. However, it should not be construed that the present invention is limited to the following examples.

Extract Preparation Example 1

The washed and dried citrus leaves, peel or fruit 10kg and 2000L of water were put in a tank and heated at 100 ° C for 10 hours to obtain an extract. The extract was heated and concentrated by evaporating water. An extract extract was obtained.

Next, the extract extract was hot-air dried to obtain an extract powder.

Extract Preparation Example 2

Washed and dried citrus leaves, peel or fruit 10kg and 2000L ethanol was put in a tank, and heated to reflux at 40 ~ 50 ℃ for 8 hours to obtain an extract. The extract was heated and concentrated by evaporating ethanol. An extract extract was obtained.

Next, the extract extract was hot-air dried to obtain an extract powder.

Examples 1-8

Using the extract prepared above, according to the formulation of Table 3, the first agent and the second agent of the composition for the hair dye and the preparation method were prepared.

Composition Example One 2 3 4 5 6 7 8 The first p-phenylenediamine 2.250 1.650 1.300 0.750 2.250 1.650 1.300 0.750 m-phenylenediamine 0.115 0.050 1.550 0.060 0.115 0.050 1.550 0.060 m-aminophenol 1.050 0.750 0.800 0.100 1.050 0.750 0.800 0.100 Resorcin 0.900 0.750 0.500 0.600 0.900 0.750 0.500 0.600 EDTA 0.100 0.100 0.100 0.100 0.100 0.100 0.100 0.100 Methylparaben 0.050 0.050 0.050 0.050 0.050 0.050 0.050 0.050 Thioglycolic acid 0.100 0.100 0.100 0.100 0.100 0.100 0.100 0.100 Sodium lauryl sulfate 1.000 1.000 1.000 1.000 1.000 1.000 1.000 1.000 Cocamide Profile Betaine 1.000 1.000 1.000 1.000 1.000 1.000 1.000 1.000 Hydroxyethyl cellulose 2.500 2.500 2.500 2.500 2.500 2.500 2.500 2.500 Monoethanolamine 0.500 0.600 0.700 0.800 0.500 0.600 0.700 0.800 extract 90.435 91.450 90.400 92.940 85.435 91.350 90.300 87.940 Foam 5.000 0.100 0.100 5.000 2nd Hydrogen peroxide * 8.000 8.000 8.000 8.000 8.000 8.000 8.000 8.000 EDTA 0.200 0.200 0.200 0.200 0.200 0.200 0.200 0.200 Stearmonium chloride 0.300 0.300 0.100 0.300 0.300 0.300 0.300 0.300 Liquid paraffin 1.000 1.000 0.500 1.000 1.000 1.000 1.000 1.000 Cetyl alcohol 2.000 2.000 1.000 2.000 2.000 2.000 2.000 2.000 lanolin 1.000 1.000 0.500 1.000 1.000 1.000 1.000 1.000 Phosphoric Acid 0.030 0.030 0.030 0.030 0.030 0.030 0.030 0.030 Sodium pyrophosphate 0.070 0.070 0.070 0.070 0.070 0.070 0.070 0.070 extract 87.400 87.400 89.600 87.400 87.400 87.400 87.400 87.400 Sum 200 200 200 200 200 200 200 200

Unit: weight%

*: Concentration 34.5 ~ 35.5%

Preparation of the first agent

The first agent blended according to the above table was added to a production tank, and stirred at 80 ° C. for 3 minutes at a speed of 2000 rpm and at a speed of 150 rpm for 3 minutes with a paddle mixer. Then, the mixture was cooled to 45 ° C. while stirring with a paddle mixer. Monoethanolamine was added to the mixture and cooled to 25 ° C. The mixture was then filtered and aged for 24 hours in a nitrogen atmosphere.

Preparation of the second agent

On the other hand, the second agent blended according to the above table was added to the production tank and stirred at 80 ° C. for 3 minutes at a speed of 2000 rpm and at a speed of 150 rpm for 3 minutes with a paddle mixer. Then, 8 g, 0.03 g and 0.07 g of hydrogen peroxide, phosphoric acid and sodium pyrophosphate were added thereto, and the mixture was cooled and mixed to 45 ° C. while stirring with a paddle mixer. The mixture was then filtered and aged for 24 hours in a nitrogen atmosphere.

The following experiment was conducted with the hair dye composition obtained in Examples 1 to 8.

Experimental Example 1 (Storability Evaluation)

The first agent and the second agent of Examples 1 and 6 were sealed in a laminated packaging material of aluminum foil and synthetic resin, respectively, and left in a constant temperature and humidity chamber at a humidity of 75% and a temperature of 40 ° C. for one month, and then taken out and dyed.

No degradation of quality was observed, such as alteration of the product or degradation of the dyeing effect.

Experimental Example 2 (Evaluation)

For 20 panelists (male 10, female 10), the hair dye was applied to the hair dye composition of Example 5 and a commercial dye (Musgetbing Hair Color, Musgene Co., Ltd.). The experimental method was half head comparison method, that is, half of the hair was dyed with the composition of Example 5 and the other half with a commercial hair dye.

As a feeling of use, mixedness, flowability, spreadability, and hair feel after hair dye were evaluated. The evaluation result was shown according to the number of panels which answered that it was good about each feeling.

division Example 5 Composition Commercial dyes Mixed ◎ ◎ Flow ◎ ○ Application ◎ ○ Hair texture ◎ ×

◎: more than 18

○: 14-18

△: 8-13

×: less than 8

From the above table, the hair dye composition of the present invention showed a very excellent result in terms of the texture of hair after hair dye compared to a commercial dye. In addition, it can be seen that the flowability and spreadability in comparison with the commercial dyes.

Experimental Example 3 (Evaluation of Side Effects)

On the other hand, in the case of three panels showing the symptoms of poisoning on the scalp of the half head using the commercially available dye, the half head using the hair dye composition of Example 5 did not show the above symptoms.

In addition, the hair dye composition of Example 3 was applied to the panel of three heads showing the symptoms of poisoning on the scalp of the half head using the commercially available dye, and left for 10 minutes after application in a circle having a diameter of 3 cm above the cuff. Rinse off after 10 minutes. No allergic symptoms were seen on the skin.

Experimental Example 4 (heavy metal detection rate)

Extracts prepared from Extract Preparation Examples 1 and 2 were commissioned by a chemical test laboratory to evaluate the detection of heavy metals by IPC analysis.

Test Items unit Result Test Methods Pb mg / kg Not detected ICP Analysis CD mg / kg Not detected ICP Analysis Mn mg / kg Not detected ICP Analysis Hg mg / kg Not detected ICP Analysis As mg / kg Not detected ICP Analysis

None of the test metals were detected in the citrus extracts of the present invention.

Experimental Example 5 (wool test)

The black and white wool was dyed with the hair dye composition of Example 8 and a commercially available dye, and the dyeing property, hair conditioning effect, and color fastness were evaluated. After 1 hour after applying the hair dye composition of Example 8 and a commercial dye to the thoroughly washed test wool, shampoo, rinse and dry.

The comparison of the dyeability is based on the color difference, and the comparison of the hair conditioning effect and the color fastness is performed by the 5-point scale (5 = the best effect; 4 = the effect is very good; 3 = the effect is moderate; 2 = the effect is slightly good; 1 = ineffective) and scored 10 sensory evaluation specialists and averaged the scores.

Dyeing

The color difference (ΔE) between the dyed wool and untreated wool was measured using a spectrophotometer. The larger the color difference, the better the dyeing property.

Hair conditioning effect

Dyed wool and untreated wool were compared by hand combing 20 times with hand touch to evaluate the incidence of static electricity.

Dyeing fastness

The dyed wool was immersed in an acid solution similar to the sweat component, and after a certain time, the degree of discoloration was observed.

Hair dye composition of Example 8 Commercial dyes Color difference (ΔE) 73 41 Hair conditioning effect 4.6 2.3 Color fastness 4.5 2.0

Example 8 hair dye compositions according to the present invention showed superior results compared to commercially available dyes in terms of dyeability, hair conditioning effect and color fastness.

As described above, the hair dye composition of the present invention by using a natural vegetable material harmless to the human body not only reduces the side effects due to chemicals in the conventional hair dye, but also has excellent effects in terms of dyeing, hair conditioning effect and color fastness.

In addition, the hair dye composition of the present invention has the advantage of shortening the hair dyeing time.

Claims (11)

85 to 93% by weight, 0.5 to 3% by weight of the extract obtained from at least one of the leaves, skins and berries of citrus fruits, and the remaining amount of fragrances, fungicides, anti-inflammatory agents, preservatives, antioxidants, ultraviolet absorbers, ammonia water, glycolic acid A first agent comprising one or more selected from the group consisting of ammonium, fatty alcohols, water and potassium alum; And The composition for hair dyes comprising a second agent comprising 85 to 90% by weight of the extract and the remaining amount of the first agent oxidizing agent and pH adjusting agent. In claim 1, The first agent is a hair dye composition, characterized in that further comprises 0.1 to 5% by weight of the foaming agent. In claim 1, The extract is a hair dye composition, characterized in that obtained by hot water extraction or solvent extraction. In claim 3, The solvent used in the solvent extraction method is composed of methanol, ethanol, acetone, dioxane, tetrahydrofuran, n-propenol, hydrous methanol, hydrous ethanol, hydrous acetone, n-butanol, n-hexanoic acid, ethyl acetate and benzene A composition for hair dyes, characterized in that at least one selected from the group. In claim 2, The foaming agent is a hair dye composition, characterized in that at least one selected from anionic surfactants, non-ionic surfactants to which the alkyl fatty acid polyoxy ethylene is added, and betaine type amphoteric surfactant. In claim 1, The hair dye composition, characterized in that the first agent and the second agent is provided separately to be gel form when mixed when used. In claim 1, The dyeing agent is p-phenylenediamine, m-phenylenediamine, o-phenylenediamine, p-nitro-o-phenylenediamine, n-phenyl-p-phenylenediamine, 4-ethoxy sulfate m- At least one diamine-based organic dye selected from the group consisting of phenylenediamine and toluene sulfate 2.5-diamine. 85 to 93% by weight of an extract obtained from at least one of the leaves, skin and fruit of the citrus fruits; 0.5 to 3% by weight of the dye agent; And at least one selected from the group consisting of perfumes, fungicides, anti-inflammatory agents, antiseptics, antioxidants, ultraviolet absorbers, aqueous ammonia, ammonium glycolate, fatty acid alcohols, water and potassium alum in 70 to 90 ° C. Stirring; Cooling and stirring to 40 to 50 ° C; Adding 0.5 to 1% by weight of alkali agent based on the total weight of the mixture and cooling to 20 to 30 ° C; And The first agent of any one of claims 1 to 7 is prepared by filtration and ripening in a nitrogen atmosphere, Adding an oxidizing agent and a pH adjusting agent to oxidize 85 to 90% by weight of the extract obtained from at least one of citrus leaves, skins and fruits and the remaining amount of the first agent to a production tank and stirring at 70 to 90 ° C; Adding 5 to 10% by weight of hydrogen peroxide, 0.01 to 0.05% by weight of phosphoric acid, and 0.05 to 0.1% by weight of sodium pyrophosphate, followed by cooling and stirring to 40 to 50 ° C with stirring; And A method for producing a composition for hair dyes, characterized in that the second agent of any one of claims 1 to 7 is prepared by filtration and aging in a nitrogen atmosphere. In claim 8, The alkaline agent is a method for producing a composition for hair dyes, characterized in that the monoethanolamine. In claim 8, The oxidizing agent is a method for producing a composition for hair dyes, characterized in that the hydrogen peroxide solution. In claim 8, The pH adjusting agent is a method for producing a composition for hair dyes, characterized in that the phosphoric acid.