KR101332255B1 - Method of dyeing using Curcumin dye - Google Patents

Abstract

The present invention relates to a dyeing method using turmeric dye, a pretreatment step of removing impurities of a material to be dyed, a dyeing step of dyeing the pretreated material in a salt solution containing turmeric dye, and embedding the dyed material in a mordant solution. It relates to a dyeing method using turmeric dye, including a mordant step, and a flushing step of washing the embedded material in a washing solution.

Description

Method of dyeing using Curcumin dye

The present invention relates to a dyeing method using turmeric dye, and specifically relates to a yellow turmeric dye having an antimicrobial activity as a dye using an extract extracted from turmeric, a manufacturing method thereof and a dyeing method using the same.

In general, dyes have been posed to environmental problems due to environmental pollution caused by industrial wastewater discharged through dyeing process, and toxic, allergic and carcinogenic properties of dyes themselves. This is essential.

The environmentally friendly dyes refer to dyes which do not contain heavy metals or harmful organic substances in the dyes themselves, and are dyes that have high fixation rate but do not emit harmful substances when dyed due to low wastewater generation.

Possible development of the environmentally friendly dyes include reactive dyes, disperse dyes, natural dyes and the like.

In particular, since the natural dyes can be collected in nature and used as natural materials, environmental pollution is low compared to other materials. On the other hand, reactive dyes and disperse dyes are not environmentally friendly by the dye itself, but can be used as an environmentally friendly dye by changing the molecular structure of the dye or reducing waste water during the washing process of the dye. Therefore, the manufacturing technology of environmentally friendly dye is a technology that makes it possible to convert environmentally friendly dyes and disperse dyes, such as natural dyes, which are not environmentally friendly through various manufacturing techniques.

The natural dyes can be obtained by dyeing using pigments from animals and plants existing in nature to obtain a natural, luxurious and emotional color that can not be obtained from chemical dyes, there are no side effects such as allergic reactions occurring in chemical dyes, It has the effect of anti-allergic, antibacterial or deodorant.

In addition, mineral dyes such as ocher, charcoal, jade, and elvan are helpful in circulating blood through the release of far-infrared rays containing negative ions, which has the advantage of obtaining material properties.

In addition to the above advantages, natural dyes can be easily obtained from plants, animals or minerals, can be said to be environmentally friendly dyeing in the dyeing process, even if the same dye can be used to show a variety of dyeing effects.

However, because chemical dyeing is transparent and dark in color, natural dyeing uses natural materials, so there is a disadvantage in that the yield is limited and the color is light. Water pollution caused by wastewater discharged from the process of dyeing and dyeing synthetic dyes has become a serious environmental problem.

Thus, the natural dyes may be widely used not only for textiles, but also for wood, leather, ceramics, cosmetics, toilet paper, paints, food coloring, medicinal coatings, crafts, and clothing, as well as household goods, foodstuffs, housewares, and industrial products.

Particularly, among the natural dyes, the vegetable dye includes a monochromatic dye which can extract only a single color and a polychromatic dye that can give two or more colors, and the monochromatic dye is a direct dye and a material in which the dye and the fiber react directly without intermediate mordant. Mutable dyes that are reacted and dyed depending on the component may be included.

Therefore, in the Republic of Korea Patent No. 311283, which relates to a method for producing silk containing pine needles and mugwort ingredients, absorbs pine needles and mugwort ingredients in raw silk, and dries the glue made from pine needles and mugwort on the outside By making the silk yarn which is made into raw silk, it becomes silk containing pine needles and mugwort ingredients, and it has no moistness, so it is smooth in color, soft to the touch, and silks with pine needles and mugwort fragrance are obtained. There has been proposed a method of manufacturing pine needles wormwood silk by mixing the beneficial substance to the human body to become a good silk for human health.

In addition, according to Korean Patent Laid-Open Publication No. 2003-93176, a method for preparing natural mugwort dyes and a natural fiber dyeing method using natural mugwort dyes is used as a material for producing mugwort natural dyes or mixed with Injin mugwort or cedar mugwort with water or 100 ° C. or more. Boil for 20 to 40 minutes at room temperature (20 to 30 ℃) or use dried or dried iron mugwort to make powder, ferment it to boil for 20 to 40 minutes at 100 ℃ or higher, and pH value of 8 to 9 Preparing weak alkaline water, mixing dye and water in a weight ratio of 2: 1, filtering the mixed salt solution, and fermenting the mixed salt solution at room temperature (20-30 ° C.). Mugwort natural dye production method has been proposed, comprising the steps of filtration, mixing the filtered salt solution and weak alkaline water in a weight ratio of 3: 7, and fermenting the salt solution and the weak alkaline water mixed solution.

However, the natural dyes developed to date such as pine needles or wormwood is not easy to extract, so the efficiency is very low and there is a problem of poor color reproducibility.

In order to solve the above problems, an object of the present invention is to provide a turmeric dye having an environmentally friendly and antibacterial and extracting method of the pigment component from turmeric.

In addition, an object of the present invention is to provide a dyeing method capable of dyeing fabrics and papers by using natural turmeric dyes, which are environmentally friendly and easy to dye.

In order to achieve the above object, the present invention provides a dyeing method using a turmeric dye, a pretreatment step of removing impurities of the material to be dyed; Dyeing the pretreated material in a salt solution containing turmeric dye for 70 to 110 ℃, 10 to 50 minutes; A embedding step of embedding the dyed material in a mordant for 10 to 30 ° C. for 10 to 30 minutes; And it provides a dyeing method using the turmeric dye, characterized in that it comprises a washing step of washing the buried material in a wash water 60 to 100 ℃, 20 to 40 minutes.

In addition, the salt solution containing turmeric dye provides a dyeing method using turmeric dye, characterized in that 0.02 ~ 0.1 parts by weight of turmeric dye mixed with 100 parts by weight of distilled water.

In addition, the turmeric dye provides a dyeing method using turmeric dye, characterized in that the turmeric is extracted by the ethanol extraction method.

In addition, the mordant provides a dyeing method using turmeric dye, characterized in that 1 to 7 parts by weight of alum is mixed with 100 parts by weight of distilled water.

In addition, the washing liquid provides a dyeing method using a turmeric dye, characterized in that the neutral detergent having a pH of 5 to 8 contains 5 to 15% by weight.

In addition, the present invention provides a fabric characterized in that the dyeing method.

In addition, there is provided a paper characterized in that the dyeing method.

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. First, it should be noted that, in the drawings, the same components or parts have the same reference numerals as much as possible. In the following description of the present invention, a detailed description of known functions and configurations incorporated herein will be omitted so as to avoid obscuring the subject matter of the present invention.

As used herein, the terms "about", "substantially", etc., are used at, or in close proximity to, the numerical values given when manufacturing and material tolerances are inherent in the meanings stated, and are intended to aid the understanding of the present invention. Or absolute figures are used to prevent unfair use of unscrupulous infringers.

1 is a process chart showing a dyeing method of the turmeric dye of the present invention, Figure 2 is a photograph showing a surface dyed with turmeric dye according to the present invention, Figure 3 is a photograph showing a dog dyed with turmeric dye according to the present invention. to be.

The present invention relates to a method of dyeing fabrics using turmeric, and to imparting functions such as antibacterial activity of turmeric to the fabric to be dyed and to an environmentally friendly method of dyeing turmeric.

Curcumin used in the present invention belongs to the genus Zingiber Officinale Roscoe, and its scientific name is known as Curcuma Longa Linne or Tumeric, and its unique scent and taste, natural color and various characteristics. It is classified as a perennial herbaceous plant.

Generally, turmeric, belonging to the ginger family, has been used for tea and beverages, and in India, Aryan people have grown turmeric from 2500 to 1500 BC and used it for medicine and dyes. In Korea, turmeric is grown in Gurye, Haenam, Suncheon, etc. in the early Joseon Dynasty and used as a herbal medicine in the record of Sejong or Dongguk Yeoji.

The turmeric is made of a hard cork layer, and when using it, the inner stem component of turmeric is removed after removing the cork layer. Among the internal stem components of turmeric (100.0%), water 16.0%, starch 50.0%, carbohydrate 12.4%, fibroid 5.0%, arabinose 1.1%, fructose (fractose) ) 1.2%, glucose 2.8%, and other common ingredients, and essential oils (4.5-6.0%) contains curcumin 0.3%, zingiberone (tumiberone), tumeone (cineer), cineol ( It is recorded that trace amounts of cineol) and the like are contained, and trace amounts of phenol and the like are present in the organic components such as kalium (K), sodium (Na), calcium (Ca) and the like. In particular, the chemical molecular structure of curcumin, an anthocyanine-based natural dye having various effects such as antibacterial action, anticancer action, and antioxidant action in the essential oil component of turmeric, is shown in Chemical Formula 1 below.

[Formula 1]

In general, turmeric has a unique natural aroma, spicy taste, natural color and various characteristics, and since ancient times, it has been used as a folk remedy for turmeric liquor, turmeric tea, turmeric cotton, turmeric drink, turmeric sauce, turmeric curry, Although it has been used in herbal medicines such as turmeric spice and herbal medicines such as cold, fever, cough and digestion, the effects of turmeric today are antibacterial, anticancer, antioxidant, anti-inflammatory, blood pressure lowering, detoxification, and skin aging. Various effects are known for its action, anti-obesity effect, natural dyeing effect, and research on the development of functional products related to herbal medicines, herbal cosmetics, herbal soaps, natural dyeing, and related materials and materials of these products It is becoming.

In addition, among the essential oil components of turmeric, jinbeberon (zingiberone), tumerone (tumerone), cineol (cineol) and the like have an efficacy and effect on antibacterial action, anti-inflammatory action, antioxidant action, etc. Attention has been drawn to these ingredients, and zingiberone is a similar ingredient to ginger ginger (zingerol) and may be deteriorated due to destruction or degradation of active ingredients during long-term storage or processing. Curcumin, an anthocyanin-based curcumin that is yellow in turmeric, is known to be a natural dye for fiber and hair today. Vegetable dyes currently used as natural dyes include safflower, Schisandra chinensis, mugwort, and animal dyes such as scabbard scales, and mineral dyes include mica, titanium, talc, ocher, etc. In general, natural dyes are environmental pollution or human body. While it is advantageous in terms of safety, there is an instability that the color changes during long term storage. Recent studies of turmeric report that curcumin extracted from Curcuma Longa Linne has an effect on anti-inflammatory and anticancer activity when used in the cells of activated receptors.

Turmeric dye used in the present invention may be used turmeric extract or supercritical fluid extraction method using carbon dioxide extracted from the turmeric using a solvent such as steam, methanol, ethanol, ether, propylene glycol, etc. It would be desirable to use ethanol to improve reproducibility.

In the method of preparing turmeric dye using the ethanol, the stem component of turmeric is pulverized, dried, and soaked in ethanol.

Turmeric soaked in ethanol can be heated in a hot bath for 5-7 hours at 70-95 ° C., similar to the boiling point of ethanol, and ethanol can be separated using a rotary vacuum evaporator to obtain solid turmeric dye. .

In order to increase the quality or yield of turmeric dye as the extraction solvent, it is preferable to use 90% or more ethanol (C ₂ H ₅ OH) aqueous solution.

In addition, it is preferable to extract the turmeric extract by putting it in ethanol 3 to 10 times the weight of turmeric so that turmeric may be sufficiently immersed in ethanol.

The natural turmeric dye may be applied to paper in addition to natural fibers such as cotton, hemp, wool, and silk, and synthetic fibers such as polyester, nylon, and acrylic.

1 is a process showing the dyeing method of turmeric dye of the present invention, the turmeric dye dyeing method is dyed in the pre-treatment step, dyeing step, mordant step, washing step.

The pretreatment step is to remove impurities in the material to be dyed, such as paper, fiber, fabric to be dyed can be treated by a general pretreatment method suitable for the material to be dyed, such as paper, fibers, fabric.

The dyeing step is a step of dyeing the pre-treated material in the salt solution containing turmeric extract is dyed for 70 to 110 ℃, 10 to 50 minutes.

If the condition of the dyeing is out of the above range may be stained or unevenly dyed fiber, and if the temperature is exceeded may cause damage such as shrinkage in the material to be dyed.

The salt solution is prepared by mixing 0.02 to 0.1 parts by weight of the turmeric dye described above with 100 parts by weight of distilled water. When the turmeric extract is mixed at less than 0.02 parts by weight, the uniformity of the dye is inhibited. When the turmeric extract is mixed at an amount exceeding 0.1 parts by weight, the efficiency of dyeing may be reduced.

In preparing the salt solution, it may be preferable to first mix the turmeric dye with a small amount of distilled water to dissolve the turmeric dye uniformly in distilled water, and then mix the distilled water again. This is because turmeric dye may not be uniformly mixed when the turmeric dye is mixed with a large amount of distilled water in powder form, so that the turmeric dye may be uniformly mixed in a small amount of distilled water to obtain a uniform salt solution.

The embedding step is to bury the dyeing material in a mordant solution for 10 to 30 ℃, 10 to 30 minutes in the step of increasing the color fastness by treating the chlorine to facilitate the fastening of the coloring and turmeric dye.

The mordant is prepared by mixing 1-7 parts by weight of alum in 100 parts by weight of distilled water. When the alum is mixed at less than 1 part by weight, it is not possible to expect mortar, and when it is mixed at more than 7 parts by weight, the efficiency of mortar may be reduced.

The alum may be pre-treated before the dyeing step.

The flushing step is a step of washing off the unretained turmeric dyes in water wash 60 to 100 ℃, 20 to 40 minutes.

It is preferable that the washing solution contains 5 to 15% by weight of a neutral detergent having a pH of 5 to 8 so as not to damage the dyed material.

The present invention is dyed in a pre-treatment step, a dyeing step, a mordant step, a water washing step as described above, in order to increase the dyeing effect, the dyeing effect can be further enhanced by using alum dyes before the dyeing step.

As described above, the present invention extracts turmeric extract that can be used as a dye from turmeric to provide a dyeing method that can be dyed to a fabric such as paper or fabric, knitted fabric, or nonwoven fabric using turmeric having environmentally friendly and antimicrobial properties. There is.

In addition, there is an effect to provide a natural dyeing method easy to dye using environmentally strong sulfur dyes.

In addition, the turmeric dye of the present invention is applicable to dyeing synthetic fibers and paper as well as natural fibers.

1 is a process chart showing the dyeing method of turmeric dye of the present invention.
Figure 2 is a photograph showing the surface dyed with turmeric dye according to the present invention.
Figure 3 is a photograph showing a dog dyed with turmeric dye according to the present invention.

Hereinafter, the dyeing method using the turmeric dye of the present invention will be described in detail by Examples.

The following examples illustrate the present invention, but the scope of the present invention is not limited to the following examples.

◈ Example

The turmeric extract of domestic B company extracted only with the stem of natural turmeric was used as turmeric dye.

The strengthening dye was mixed with distilled water to prepare an aqueous turmeric dye solution containing 1.0% turmeric dye.

After neutralizing cotton (Example 1) and silk (Example 2), which are natural fibers for dyeing with the prepared turmeric dye, at 95 ° C. for 30 minutes, the pretreatment step of removing impurities by boiling at 95 ° C. for 10 minutes is performed. Done,

The cotton and nuts were dyed at 90 ° C. for 30 minutes in a salt solution in which 0.5 g of turmeric dye solution and 100 ml of distilled water were mixed.

After the dyeing, the solution was embedded in 100 parts by weight of distilled water in a mordant solution mixed with 4 parts by weight of alum for 15 minutes at 20 ° C., and after washing, water was washed at 80 ° C. for 30 minutes with a washing solution containing 10 wt% of a neutral detergent having a pH of 7. To obtain a cotton (Fig. 2) and a silk (Fig. 3) stained with turmeric dye.

Comparative Examples 1,2

As in Examples 1 and 2, cotton (Comparative Example 1) and silk (Comparative Example 2) were dyed with turmeric dye, but were dyed without performing a mordant step.

◈ Dyeability evaluation

After dyeing, the dyeing brightness, color direction, and color difference were measured using a color difference meter.

division DL * Da * Db * DE *  if Example 1 90.920 -0.200 62.460 2.520 Comparative Example 1 89.780 -0.070 55.760 0  Dog Example 2 90.920 -2.760 51.680 0.410 Comparative Example 2 90.650 -2.900 50.690 0

DL ^* in Table 1 is the brightness of color, Da ^* and Db ^* stands for direction of color and DE ^* stands for color difference, where the brightness of cotton (90.920) and dog (90.920) are the same when DL ^* is processed by printing method. , Da ^* and When Db ^* was used as a mordant method, the measured values of cotton (-0.200, 62.460) and silk (-2.760, 51.680) appeared in the direction of weak red color and stronger yellow color. The direction of the color is yellowish color, slightly darker in cotton than silk. DE ^* is the color difference based on the printing method and is calculated by the following equation (1).

2 and 3 are photographs showing the cotton and the silk stained with turmeric dye according to the present invention, as shown in Figures 2 and 3, the brightness of the cotton (90.920) and the shoulder (90.920) is very bright, and the direction of color The yellow color system showed that the cotton was slightly darker than the silk, and the color difference was higher in the cotton (2.520) than the silk (0.410). Therefore, this dyeing experiment confirmed that Curcumin extract can be used as a natural dye.

◈ Component Analysis of Turmeric Dye

1. ICP / OES Analysis

To identify the inorganic component of the turmeric dye, the turmeric dye solution (including 1.0% of turmeric dye) is diluted and dissolved in a ratio of 1: 100 100% by weight with 5% nitric acid solution, and then inductively coupled plasma spectrometer is inductively coupled plasma spectrometer. Measured by spectrometry, standard elements for inorganic analysis are Ag, Al, As, B, Ba, Be, Ca, Co, Cd, Cr, Cu, K, Li, Fe, Mg, Mn, Mo, Na, Ni, Pb , Sb, Se, Si, Ti, Tl, V, Zn were used for sample measurement.

Analysis of turmeric material showed K (53.300 ppm), Na (1.150 ppm), Ca (0.711 ppm), Ti (0.351 ppm), Li (0.256 ppm), Cu (0.233 ppm), Zn (0.087 ppm), Fe (0.078). Various inorganic components such as ppm), Mg (0.199ppm), and Al (0.140ppm) were detected, and in particular, the detection of Li, which has recently emerged as an energy source, has been confirmed.

2. GC / MSD Analysis

The turmeric dye solution (containing 1.0% turmeric dye) was diluted and dissolved in a ratio of 1: 100 100 with diethyl ether [(C ₂ H ₅ ) ₂ O] and then analyzed by Gas Chromatography / Mass Selective Detector. .

In the turmeric dye, various organic components such as ethane (1.674), ethyl ether (1.700), propanoic acid (1.859), benzene (10.813), and phenol (14.194) were detected. Detection of benzene (10.814), phenol (14.194), etc., showing various aromatic properties, was confirmed.

◈ Antibacterial test of turmeric dye

0.5 g of turmeric dye solution (containing 1.0% turmeric dye) and 100.0 mL of distilled water were diluted and dissolved with 0.5% sample solution, 1.0 mL of which was mixed and mixed with Mueller Hilton Broth medium solution (10.0 mL). Microorganisms were tested by inoculating microbial staphylococcus aureus (Example 3) and aspergillus niger (Example 4) in the medium solution. The results of microbial test were examined for the number of microorganisms and their relationship with the culture conditions and incubation time. Here, without adding turmeric dye as a control, a certain amount of staphylococcus anreus (Comparative Example 3) and aspergillus niger (Comparative Example 4) was added to the medium solution. The medium used was Mueller Hilton Broth (Difco. Lab. CO., USA).

Table 2 shows the test results of turmeric dye on the microorganisms according to the incubation time.

Hours (hrs) Staphylococcus aureus Aspergillus niger Example 3 Comparative Example 3 Example 4 Comparative Example 4 0 + + + + 24 + + + + 48 + + + + 72 - + - + 96 - + - + 120 - + - + Test temperature: 36 ℃
+: Microbial positive reaction
-: Microorganism negative reaction

As shown in Table 2, Example 3 and Example 4 showed a positive reaction in the initial antibacterial test, but showed a negative reaction after 72hrs (3day) after the microbial culture test. In Comparative Example 3 and Comparative Example 4 in which the microorganism was added to the medium solution without adding the extract, positive reaction was shown in the initial antibacterial test, but the positive reaction was continued even after 72hrs (3day). You can see that appears. As shown in Table 2, it can be seen that the turmeric dye of the present invention has an antimicrobial effect on microorganisms.

Claims (7)

In the dyeing method using turmeric dye,
A pretreatment step of removing impurities of the material to be dyed;
Dyeing the pretreated material in a salt solution containing turmeric dye for 70 to 110 ℃, 10 to 50 minutes;
A embedding step of embedding the dyed material in a mordant for 10 to 30 ° C. for 10 to 30 minutes; And
The method of dyeing using turmeric dye, characterized in that it comprises a washing step of washing the embedded material in a wash solution 60 to 100 ℃, 20 to 40 minutes. The method of claim 1,
The dye solution containing the turmeric dye dyeing method using turmeric dye, characterized in that 0.02 ~ 0.1 parts by weight of turmeric dye mixed with 100 parts by weight of distilled water. The method of claim 1,
The turmeric dye is a dyeing method using turmeric dye, characterized in that the turmeric is extracted by the ethanol extraction method. The method of claim 1,
The mordant is a dye method using turmeric dye, characterized in that 1 to 7 parts by weight of alum is mixed with 100 parts by weight of distilled water. The method of claim 1,
The washing solution is a dye method using a turmeric dye, characterized in that the neutral detergent having a pH of 5 to 8 contains 5 to 15% by weight. Fabric characterized in that the dyeing method according to any one of claims 1 to 5. Paper characterized in that it is dyed by the dyeing method of any one of claims 1 to 5.

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