KR20150020404A - Natural hair-dye composition using Pomegranate extract, and dyeing method using it - Google Patents

Abstract

The present invention relates to a natural hair-dye composition using a pomegranate extract, and more specifically, to a non-oxidative hair-dye composition which comprises a first agent including at least one among a hot water extract, an ethanol extract and a ferment of the hot water extract of pomegranate flesh powder that is prepared by drying and pulverizing pomegranate fruit, a hair penetration accelerator, an oxidation prevention agent and purified water; and a second agent including iron sulfate as a mordant. The natural hair-dye composition according to the present invention is a natural hair-dye composition with few side effects, which enables dyeing into a natural color, causes less hair damage after dye, and has an equivalent performance to that of non-oxidative hair-dye composition using pyrogallol in the market.

Description

[0001] The present invention relates to a natural hair dye using a pomegranate extract and a dyeing method using the natural hair dye composition,

The present invention relates to a natural hair dye using a pomegranate extract and a dyeing method using the same.

More specifically, the present invention relates to a pesticide composition comprising at least one of a hot-water extract, an ethanol extract, and a hot-water extract of a pomegranate fruit powder obtained by pulverizing pomegranate fruit with a hair penetration promoter, an antioxidant, purified water, And a dyeing method using the non-oxidizing hair dye composition.

The natural hair dyeing agent according to the present invention is a natural hair dyeing agent having little side effects. The hair dyeing agent of the present invention can be dyed in natural colors and has less hair damage after dyeing, and its performance is not inferior to non-oxidizing hair dyeing agents using commercially available pyrogallol.

In general, a hair dye can be distinguished as a temporary hair dye, a semi-permanent hair dye, or a permanent hair dye depending on the durability and durability of the hair color. Among them, permanent hair dye is divided into oxidation hair dye, metal hair dye and vegetable hair dye depending on the dye used. Most of hair dye presently used are oxidation dye precursors and oxidation dye using an oxidation dye such as an amino compound.

However, oxidative dye is a chemical dye containing synthetic dyes. It causes problems such as hair damage, rash and contact skin reaction, and often causes leukemia, bladder cancer, uterine cancer and breast cancer when it is used together with visual impairment. And there is a disadvantage that odor is generated when dyeing.

As a solution to this problem, development of a natural hair dye that is harmless to the human body and environmentally friendly is demanded. The oldest representative natural hair dye is Henna, which is taken from plants native to the tropics of India and the Middle East. It has been used for thousands of years in human hair dyeing. In addition to henna, Walnut, Indigo and Camomile are used. Each color of Henna is red, walnut is brown, ink is black, indigo is indigo, chamomile is yellow Series.

Meanwhile, pomegranate is cultivated in Korea, China, Japan, Taiwan, etc., and it is known that fruit is rich in carbohydrate, amino acid, vitamin, mineral, pectin and tannin and has convergence, blood purification and antioxidant effect. It is known that it has strong anticancer effect, antioxidant effect, suppression of acid secretion and so on. Pomegranate shells are known as pomegranate pills and used as a contraction agent for diarrhea, dysentery, abdominal pain, major depression, and also have effects on skin itching, athlete's foot, ringing, and acne treatment. Especially, it has been reported that pomegranate contains a large amount of polyphenols such as Ellagitannin, Ellagic acid, Gallic acid and Tannic acid which are natural pigments. Figure 1 shows the structural formulas of Ellagic acid, Gallic acid and Tannic acid, including Ellagitannin, a natural pigment of pomegranate.

An example of application of pomegranate as a natural hair dye to human hair is KOKAI Publication No. 2010-30158, but it has a disadvantage in that it has a lower ΔE value than that of a non-oxidative hair dye using commercially available pyrogallol, resulting in low coverage of the claw hair.

The commercially available non-oxidative hair dye containing pyrogallol as a main component has a disadvantage in that hair color at the early stage of dyeing is colored with dark blue with a lot of blue color and is dyed with unnatural color.

It is an object of the present invention to provide a natural hair dye composition which is low in human toxicity and is eco-friendly, and can obtain a hair dyeing effect similar to that of a commercially available non-oxidizing hair dye and a more natural dyeing color and fastness .

The hair dyeing agent of the present invention having the above object is characterized by comprising an extract derived from pomeo fruit powder obtained by pulverizing dried pomegranate fruit.

Wherein the extract derived from the pomegranate fruit powder is one of a hot-water extract and an ethanol extract of the pomegranate fruit powder.

In addition, the extract derived from the pomegranate fruit powder is characterized in that the hot-water extract of the pomegranate fruit powder is fermented using a strain (Lactobacillus).

Also, the concentration of the hot-water extract, the ethanol extract, or the fermentation product of the hot-water extract of the pomegranate fruit powder is 10 to 50% by weight after concentration under reduced pressure if necessary.

The hair dyeing agent of the present invention is further characterized by containing at least one additive selected from the group consisting of 1.0 to 20% by weight of Urea as a hair penetration promoter and 0.01 to 10.0% by weight of sodium ascorbate as an antioxidant.

More specifically, the hair dyeing agent of the present invention is a fermented product of a hot-water extract, an ethanol extract, or a hot-water extract of a pomegranate fruit powder; 1.0 to 20% by weight of Urea as a hair penetration promoter, and 0.01 to 10.0% by weight of sodium ascorbate as an antioxidant; And a purified water containing purified water;

1.0 to 10.0% by weight of ferrous sulfate (FeSO ₄ · 7H ₂ O) as a mordant, 0.01 to 10.0% by weight of ascorbic acid as an antioxidant, and purified water as a remaining component.

The pH of the preparation is 7.0 to 8.0.

The dyeing method according to the present invention comprises the steps of uniformly applying the composition 1 to the hair and treating the hair at 20 to 30 ° C for 15 to 30 minutes and uniformly applying the composition 2 to the hair in the same amount as the preparation 1, Is treated at 20 to 30 DEG C for 15 to 30 minutes and then washed with water.

As described above, the present invention uses pomegranate fruit powder pulverized by drying pomegranate fruit, and includes a step of fermenting the extract using a strain to increase the hair dyeing efficacy. In addition, a hair penetration promoter and an antioxidant were added to enhance the hair dyeing effect, and it was characterized in that an aqueous solution of iron sulfate was used as a mordant for controlling natural dyeing color, dyeing effect and fastness for improving fastness.

The first and second formulations of the present invention can be in a liquid phase and a lotion phase or a cream phase. It can be prepared in the form of powders, shampoos, jellies, aerosols and the like.

The amount of the hair dye to be used according to the present invention can be appropriately adjusted according to the condition of the hair, the age of the user, the length of the hair, etc., and the application time can also be appropriately adjusted depending on the individual.

The natural hair dye composition using the pomegranate fruit powder extract of the present invention is basically harmless to the human body and environmentally friendly.

At the same time, it has the same hair dyeing effect and fastness as the non-oxidative hair dyeing agent using pyrogallol which is commercially available.

In addition, it provides a more natural hair dye color than the non-oxidative hair dye using commercially available pyrogallol, and less hair damage when stained.

FIG. 1 shows the structural formula of Ellagic acid, Ellagitannin, Gallic acid and Tannic acid contained in pomegranate,
Fig. 2 is a photograph of the hair using the hot-water extract, ethanol extract, fermented concentrate and pyrogallol from Examples 44 to 46 and Control Example 1,
FIG. 3 is a cross-sectional view of the hair dyed with the hot-water extract, ethanol extract, fermentation concentrate and pyrogallol from Examples 44 to 46 and Control Example 1,
4 is an SEM photograph of the surface of the hair dyed using the hot-water extract, ethanol extract, fermentation concentrate and pyrogallol from Examples 44 to 46 and Control Example 1. Fig.

The natural hair dye composition of the present invention described above is composed of a non-oxidative type hair dye agent composition comprising a pomegranate fruit powder extract obtained by drying a pomegranate fruit and a non-oxidized hair dye agent composition containing an aqueous solution of iron sulfate.

The non-oxidizing type hair dye formulation 1 composition comprises,

- Select one or more of the hot-water extract and the ethanol extract of the pomegranate fruit powder which is pulverized by drying the pomegranate fruit. It is also possible to use a fermentation broth obtained by fermenting the hydrothermal extract in the extract with a strain after concentration under reduced pressure.

- Concentrating the extract solution obtained by the above extraction method under reduced pressure to adjust the concentration to 10 to 50% by weight.

The extract also contains at least one additive selected from the group consisting of a hair penetration promoter and an antioxidant.

- 1 agent is characterized by controlling pH by using acid and base.

Next, the non-oxidizing type hair dye detergent composition contains iron sulfate (FeSO ₄ .7H ₂ O) used as a mordanting agent.

As a specific example of obtaining the hair dye composition of the present invention, first, the composition of the non-oxidizing hair dye formulation of the present invention is constituted as follows.

- 4.5 g of purified water is added to 500 g of pomegranate fruit powder which is pulverized by drying the pomegranate fruit, and the mixture is refluxed for 72 hours at 90-100 ° C., and 900 g of 95% ethanol is added to 100 g of pulverized pomegranate fruit powder And then refluxed at 40-60 ° C for 72 hours.

The extraction solution obtained by the above extraction method is concentrated under reduced pressure to adjust the concentration to 10 to 50% by weight. (Concentration under reduced pressure is carried out if necessary for concentration control).

- Extract the hot water extract from the above extracts to 60 brix under reduced pressure, ferment at 37 ° C for 48 hours using Lactobacillus, sterilize at 80 ° C, centrifuge and concentrate the supernatant to 60 brix.

- At least one of 1.0 to 20.0% by weight of Urea as a hair softening agent or 0.01 to 10.0% by weight of sodium ascorbate as an antioxidant is added to the above extract (fermented product of hot water extract, ethanol extract or hot water extract) as a hair penetration promoter.

- Add pH adjusting agent (KOH, citric acid) to the mixture to adjust the pH to 7.0 ~ 8.0.

- Other items may include more purified water.

Further, the non-oxidizing type hair dye preparation composition contains

- 1.0 to 10.0% by weight of iron sulfate (FeSO ₄ .7H ₂ O) as a mordanting agent;

- 0.01 to 10.0% by weight of ascorbic acid as an antioxidant to prevent the inhibition of efficacy by oxidation of ferrous sulfate (FeSO ₄ · 7H ₂ O); And

- Include purified water.

When hair is dyed using the hair dye of the present invention,

The non-oxidizing hair dye composition of the present invention is applied uniformly to the hair, and then the coated hair is treated at 20 to 30 ° C for 15 to 30 minutes. Then, the nonoxide type hair dye preparation composition is uniformly applied to the hair Then, the coated hair is treated at 20 to 30 ° C for 15 to 30 minutes and then washed with water.

Hereinafter, the present invention will be described in detail with reference to specific examples and experimental examples. It should be understood, however, that the embodiments and examples are provided so that this disclosure will be thorough and complete, and will fully convey the scope of the invention to those skilled in the art.

[Example 1] Obtaining hot water extract derived from pomegranate fruit powder

The pomegranate fruit was dried at 90 to 100 ° C for 72 hours by refluxing at a ratio of 1: 9 of the pulverized pomegranate fruit powder to purified water. The extract was filtered once with Edbentek 5 filter paper. The pH of the obtained stock solution was 3.5.

[Example 2] Obtaining an ethanol extract derived from pomegranate fruit powder

The pomegranate fruit was dried and refluxed at 40-60 ° C for 72 hours at a ratio of 1: 9 pomegranate fruit powder to 95% ethanol. The extract was filtered once with Edbentek 5 filter paper. The pH of the obtained stock solution was 3.5.

[Experimental Example 1]

The hair dyeing effects of the extracts obtained in Example 1 and Example 2 were measured by the following experimental method.

<Experimental Method>

(1) Manufacture of non-oxidizing type hair dye 1

Example 1 10 g of the obtained extract was adjusted to pH 7 ± 0.2 using citric acid, potassium hydroxide and a pH meter.

10 g of the extract obtained in Example 2 was adjusted to pH 7 ± 0.2 using citric acid, potassium hydroxide and a pH meter.

(2) Manufacture of non-oxidizing type hair dye 2

7% by weight of iron sulfate and 0.5% by weight of ascorbic acid were dissolved in purified water, and an appropriate amount of sodium monohydrogenphosphate was added to adjust the pH to 3.0 to 3.5.

(3) Dyeing of hair

1.5 g of each of the non-oxidative hair dye 1 obtained in Example 1 and Example 2 was applied to white moth and the mixture was allowed to stand at room temperature (20-30 ° C) For 20 minutes, 1.5 g of the non-oxidizing type hair dye 2 agent was applied to each white hair and allowed to stand at room temperature (20-30 ° C) for 20 minutes.

(4) Evaluation of salt strength

The colorability (ΔE) between the hair dyed and the untreated hair was measured using a spectrophotometer CM-5. The larger the color difference, the better the dyeability of the hair dye .

The results are shown in Table 1 below.

Table 1 shows that the extracts of Example 1 and Example 2 have similar hair dyeing effects. The value of ΔE ^* ab is about 32, and when it is confirmed by naked eye, both extracts are dyed with dark brown with slight khaki light after staining with white moth, and it seems to cover about 50% of brown hair. As a result of the colorimetric analysis, ΔL ^{*, which} is the brightness index, is -31, which is darker than that of the untreated dye. The color coordinate index Δa ^* is (+) and Δb ^* Color.

[Examples 3 to 6] Concentration of the extract derived from pomegranate fruit powder

The extracts obtained in Example 1 and Example 2 were concentrated under reduced pressure using a vacuum distiller to give a ratio of powder to extract solution of 1: 4 and 1: 1. The pH of the concentrate was 3.0 to 3.5. Details are shown in Table 2 below.

[Experimental Example 2]

The hair dyeing effects of the extracts obtained in Examples 1 to 6 were carried out in the same manner as in Experimental Example 1. The results (ΔE ^* ab) are shown in Table 3 below.

From Table 3, it can be seen that the higher the concentration, the greater the hair dye efficacy.

However, since the ratio of powder: solvent is 1: 4 (20% by weight), the rate of increase in the hair dyeing effect decreases. This is because the aggregation structure between the sugar-dye and the pigment- It seems to be difficult to penetrate.

Actually, in the case of Example 4 and Example 6, the viscosity of the concentrated liquid becomes very high, so that the concentration yield is lowered and the concentrated liquid is hardly taken. Therefore, when the concentration of the extracts is 1: 4 (20% by weight) of the powder: solvent, the yield of the concentrate can be increased along with the optimum hair dyeing effect.

[Examples 7 to 16] Hair hair mobility by addition of hair penetration enhancer

In each of Example 3 and Example 5, 1 to 10% by weight of Urea known to act as a exfoliation agent was added to investigate the possibility as a hair penetration promoter, and the details are shown in Table 4 below. Examples 7 to 11 are obtained by adding Urea to Example 3, and Examples 12 to 16 are obtained by adding Urea to Example 5.

[Experimental Example 3]

The hair dyeing effects of the extracts obtained in Examples 7 to 16 were measured by the same experimental method as in Experimental Example 1, except for the production method of the non-oxidizing hair dye 1 agent.

&Lt; Preparation of non-oxidizing type hair dye 1 >

Examples 7 to 11: Urea was added to the extract concentrate obtained in Example 3 as shown in Table 4, and the pH was adjusted to 7 ± 0.2 using citric acid, potassium hydroxide and a pH meter. Then, 1: 9.

Examples 12 to 16: Urea was added to the extract concentrate obtained in Example 5 as shown in Table 4, and the pH was adjusted to 7 ± 0.2 using citric acid, potassium hydroxide and a pH meter, and purified water was added thereto to adjust the final concentration 1: 9.

The result (? E ^* ab) is shown in Table 5 below.

As shown in Table 5, it can be seen that as the content of Urea is increased, the hair dyeing effect is also increased. As a result, Urea, a keratin softener, has been shown to act as a hair penetration promoter of the non-oxidative hair dye, and its effect increases as its content increases.

[Examples 17 to 24] Hairy hair efficacy upon addition of antioxidants

The addition of 0.1 to 1% by weight of sodium ascorbate, which is used as an antioxidant, to each of Example 3 and Example 5 was examined to determine the effect of adding antioxidants. Examples 17 to 20 were obtained by adding sodium ascorbate to Example 3, and Examples 21 to 24 were obtained by adding sodium ascorbate to Example 5.

[Experimental Example 4]

The hair dyeing effects of the extracts obtained in Examples 17 to 24 were carried out in the same manner as in Experimental Example 3, and the results (? E ^* ab) are shown in Table 7 below.

As shown in Table 7, it can be seen that as the content of sodium ascorbate, which is an antioxidant, increases, the hair dyeing effect also increases. As a result, Sodium ascorbate, which is an antioxidant, is not as effective as Urea, but it has been found to help increase hair salting efficacy.

[Examples 25 to 38] Salting-out effect according to pH change

The pH of each of the extracts obtained in Example 1 and Example 2 was adjusted to 4 to 10 to measure the hair dyeing effect according to the pH. Potassium hydroxide, citric acid and pH meter were used for pH control.

[Experimental Example 5]

The hair dyeing effects of Examples 25 to 38 were measured by the same experimental method as in Experimental Example 1, except for the production method of the non-oxidizing type hair dye 1 agent.

&Lt; Preparation of non-oxidizing type hair dye 1 >

Examples 25 to 31: 10% by weight of Urea and 1.0% by weight of sodium ascorbate were added to the extract concentrate obtained in Example 3, pH was adjusted to 4 to 10, error range ± 0.1 using citric acid, potassium hydroxide and pH meter After the addition of purified water, the final concentration was adjusted to 1: 9.

Examples 32 to 38: 10% by weight of Urea and 1.0% by weight of sodium ascorbate were added to the extract concentrate obtained in Example 5, adjusted to pH 4 to 10 and error range ± 0.1 using citric acid, potassium hydroxide and a pH meter After the addition of purified water, the final concentration was adjusted to 1: 9.

The pH of each example is shown in Table 8 below.

The hair dyeing results (? E ^* ab) are shown in Table 9 below.

As shown in Table 9, it was found that as the pH was increased, the hair dyeing effect was increased, but the hair dyeing effect was lowered at pH 9 after showing the best hair dyeing effect at pH 8. From the above results, it can be seen that the optimum pH for hair dyeing is 7 to 8.

[Example 43] Fermentation of an extract using a strain

The extract obtained in Example 1 was concentrated under reduced pressure to 60 Brix using a vacuum distillation apparatus, and after fermentation at 37 ° C. for 48 hours, 2% by weight of Lactobacillus plantarum , 48% by weight of purified water and 50% After centrifugation and centrifugation, the supernatant was taken and concentrated under reduced pressure to a ratio of pomegranate powder: extraction solvent of 1: 1 (50%) with a vacuum distillation apparatus. The pH of the fermentation concentrate was 3.2.

[Example 44]

10% by weight of Urea and 1.0% by weight of sodium ascorbate were added to the fermentation concentrate obtained in Example 43, the pH was adjusted to 8.0 ± 0.1 using citric acid, potassium hydroxide and a pH meter, and purified water was added thereto to a final concentration of 1: 4 20% by weight).

[Example 45]

10% by weight of Urea and 1.0% by weight of sodium ascorbate were added to the pomegranate hot water extract concentrate (1: 1, 50% by weight) obtained in Example 4, and the pH was adjusted to 8.0 ± 0.1 using citric acid, potassium hydroxide and a pH meter The final concentration was adjusted to 1: 4 (20% by weight).

[Example 46]

10% by weight of Urea and 1.0% by weight of sodium ascorbate were added to the pomegranate ethanol extract concentrate (1: 1, 50% by weight) obtained in Example 6, and the pH was adjusted to 8.0 ± 0.1 using citric acid, potassium hydroxide and pH meter The final concentration was adjusted to 1: 4 (20% by weight).

[Control 1]

5% by weight of pyrogallol powder, 10% by weight of Urea and 1.0% by weight of sodium ascorbate, adjusted to pH 8.0 ± 0.1 with citric acid, potassium hydroxide and pH meter, and then adjusted to 100 g with purified water. Pyrogallol is the major component of non-oxidative hair dye used in the pharmacy.

[Experimental Example 6]

Each of Example 44 to Example 46 and Comparative Example 1 was used as a non-oxidative type hair dye 1 agent, and the hair dyeing effect was measured by the hair dyeing and salt strength evaluation method of Experimental Example 1.

The result (? E ^* ab) is shown in Table 10 and FIG. 2 below.

As shown in Table 10, it can be seen that the hair dyeing effect is further increased by the fermentation using the strain than the ordinary extraction. In addition, it shows a hair dyeing effect which is not far behind that of Control Example 1 in which pyrogallol used as a main component of a commercially available non-oxidative hair dye is added.

To determine the degree of dye penetration into the hair of the dyed hair, the cross section of the dyed hair was measured using a Microtome (Leica Microsystems CM1850) and a microscope (Olympus BX51, 500x) Respectively.

As can be seen from FIG. 3, it can be seen that the fermented concentrate, in contrast to the hot-water extract or the ethanol extract, penetrates the hair dye into the inside of the hair, and thus the hair-dyeing effect and washing fastness are superior to the hot- do.

In order to evaluate the washing fastness of the dyed hair, it was immersed in a 5% solution of sodium lauryl sulfate (SLS), allowed to stand at 25 ° C for 2 hours and then washed with water. The results are shown in Table 11 below.

As shown in Table 11, the decolorization by the surfactants of Examples 44 to 46 was evaluated to be excellent in washing fastness of about 3 to 3.5% as compared with the dyeing hair.

Particularly, the fermentation concentrate has a lower discoloration rate than the hot water or ethanol extract, as shown in FIG. 3, due to penetration of the dye into the hair. In Control Example 1, the ΔE ^* ab value was higher after the washing fastness test, which is due to the color change from dark blue to black after the experiment.

[Experimental Example 7]

In Experimental Example 6, dyed hair was stained using a scanning electron microscope (SEM SX-40A, 1000 times) to determine the degree of hair damage after dyeing, and the results are shown in FIG. 4 .

In FIG. 4, it can be seen that the pre-stained hair is damaged hair, and the hair surface after staining shows that the hair damage is not further progressed in Examples 44 to 46. On the contrary, in the case of the hair dye using the pyrogallol of Control Example 1, hair damage after dyeing was more advanced.

Claims (8)

And a pomegranate fruit powder-dried extract obtained by pulverizing pomegranate fruit. The method according to claim 1,
Wherein the extract derived from the pomegranate fruit powder is any one of a hot-water extract and an ethanol extract of a pomegranate fruit powder. The method according to claim 1,
Wherein the extract of pomegranate fruit powder is obtained by fermenting a hot-water extract of pomegranate fruit powder with a strain (Lactobacillus). The method according to claim 2 or 3,
Wherein the concentration of the fermentation product of the hot-water extract, the ethanol extract or the hot-water extract of the pomegranate fruit powder is 10 to 50% by weight after concentration under reduced pressure if necessary. 5. The method of claim 4,
1.0 to 20% by weight of Urea as a hair penetration promoter, and 0.01 to 10.0% by weight of sodium ascorbate as an antioxidant. A composition comprising the component of claim 5 and purified water;
1.0 to 10.0% by weight of ferrous sulfate (FeSO ₄ · 7H ₂ O) as a mordant, 0.01 to 10.0% by weight of ascorbic acid as an antioxidant, and remaining purified water. The method according to claim 6,
1 &lt; / RTI &gt; is in the range of 7.0 to 8.0. Uniformly applying the composition of claim 1 comprising the ingredients of claim 5 to hair and treating at 20 to 30 DEG C for 15 to 30 minutes;
A method for producing hair comprising the steps of: applying the composition of claim 6 uniformly to the hair in the same amount as that of the first agent; and treating the hair after treating the hair at 20 to 30 DEG C for 15 to 30 minutes,
Hair dyeing method.

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