KR101680480B1 - Natural dye with tannin and ecklonia cava and natural dyeing method using the same - Google Patents

Abstract

The present invention provides a natural dying method using persimmon juice dye and Ecklonia cava dye. The method includes: a step of preparing a persimmon dyeing solution by mixing green persimmon juice or persimmon powder with water; a step of preparing an Ecklonia cava dyeing solution by mixing Ecklonia cava steaming liquid or Ecklonia cava powder with water; a step of dyeing a dyeing target material using the mixed persimmon and Ecklonia cava dyeing solution at the same time; and a step of applying sunlight to the dyed material for color expression. The present invention also provides binary complex natural dye obtained by mixing a first component such as green persimmon juice and persimmon powder and a second component such as Ecklonia cava steaming liquid and Ecklonia cava powder.

Description

(Natural dye with tannin and ecklonia cava and natural dyeing method using the same)

The present invention relates to a natural dyeing method, and more particularly, to a new complex dyeing method of imparting flexibility to a galche using a dyestuff dye and a copious dye.

Natural dyeing is a traditional dyeing method that uses vegetable, animal, and mineral dyes obtained from nature to dye fibers. Plant dyes, which have been mainly used as traditional dyes, include plant leaves, flowers, fruits, shells, and roots. Natural dyeing was used as a universal dyeing technique until the chemical dyes were synthesized in Europe. However, due to the development of chemical dyes that can easily produce colorful and diverse colors, natural dyeing was pushed out. Today, only some craftsmen or craftsmen .

Natural dyeing requires a lot of time for pigment extraction and dyeing, and the dyeing process is complicated. In addition, the same dye has a disadvantage in that the dyeing results are different depending on the origin, harvesting time, storage state or extraction method. In addition, there is a limit to the purchase of materials, mass production is difficult, and manufacturing cost is high, and natural dyeing clothes have been ignored by consumers.

Nevertheless, natural dyeing can be natural and elegant coloring due to the raw materials obtained from nature, and even when discolored or discolored, the color is stable and silver is very suitable for manufacturing clothes containing natural beauty. Especially, it is not only harmless to human body but also has antimicrobial properties and has excellent function in terms of health such as being able to protect the body from pests. In addition, it does not destroy the environment in the manufacturing process, and there is room to overcome the limit of raw material supply by utilizing natural materials that are relatively inefficient, and it is positive for the creation of employment, so that industrial value is considerably high.

For industrialization of natural dyeing considering environment and health, it is very important to supply raw materials easily and to simplify the dyeing process and lower the overall manufacturing cost. In addition, it is necessary to increase the durability of color after color development by increasing the fastness to light and washing fastness, and further functions such as antibacterial and disease prevention are required.

Traditionally, botanical materials such as persimmon, persimmon, persimmon, mugwort, onion, and gardenia, minerals such as loess, charcoal and ink have been used as materials for natural dyeing. In order to heal and prevent diseases, As well as the use of it.

Natural dyed fabrics (garments, garments) using dyed materials have been used for a long time due to the lightness and durability of color, but the stiffness of the touch is a big disadvantage that the consumer feels. Unlike other natural dyes, unlike other natural dyestuffs, the stiff tactile feeling is unevenly coated on the fabric surface without absorbing the dye into the fiber. As a result, the flexibility of the fabric is lowered and the surface irregularity is increased, .

In the past, dyeing technology has been used to preserve and quantify dyestuffs by using freeze-dried juice as it is, or by directly freezing and drying powdery juice. In Japan, the juice is fermented in a low-molecular weight by fermentation. On the other hand, in order to improve the fastness of galata, a technique of dyeing with post-process using a sensory dye extracted with hot water after scouring has been proposed (patent application 2008-12402, patent application 2013-155479). However, in this case, it was desired to improve the washing fastness while maintaining the stiffness of the garlic, but it did not improve the flexibility in dying.

In order to accelerate the industrialization of natural dyeing and to provide high-quality and sensitive dyeing materials to the general consumer, it is necessary to improve the existing process of dyeing and develop new dyes.

The present invention has been developed under the technical background mentioned above, and an object of the present invention is to provide a natural dyeing method with improved flexibility.

Another object of the present invention is to provide a bicomponent dyestuff improved in flexibility while maintaining color and functionality as compared to conventional gentle natural dyeing.

Other objects and technical features of the present invention will be more specifically described in the following detailed description.

In order to achieve the above object, the present invention provides a method for preparing a hypochlorite solution, comprising the steps of preparing a hypochlorite solution by mixing water with a putty juice or a reduced powder, preparing a hypochlorite solution by mixing water with the hypochlorite solution or coprecipitated powder, The present invention also provides a method for natural dyeing using a dyestuff dye and a dyestuff dye, which comprises a step of complex dyeing the dyed material in a mixed state with the dyed material mixed with the dyed material, and a step of coloring the dyed material by daylight.

In the complex dyeing, the concentration of the sensitizing dye in the reducing solution is 500 to 900% owf, and the concentration of the filtering dye in the filtering solution is preferably 10% to 70% owf.

The present invention also relates to a composite dye obtained by mixing a first component of a putty juice or pulpy powder and a second component of a pulpy liquor or copepod powder, wherein the first component and the second component are mixed together with water, Wherein the first component and the second component are mixed at a weight ratio of 10: 1 to 20: 1. The two-component complex natural dye according to claim 1, wherein the first component and the second component are mixed at a weight ratio of 10: 1 to 20: 1.

The composite dye has a particle size of 520 nm or less, a catechin content of 90% or more as compared with the exclusive dye, and a lyophilicity of the dyed material can be lowered by 40% or more as compared with the dyed dye.

According to the present invention, it is possible to remarkably improve the feeling of deterioration of the fiber material due to the natural natural dyeing using the juice. Especially, it is possible to acquire color and functionality similar to those of conventional sensitive dyeing through simultaneous compound dyeing of sensory dye and sensory dye or natural dyeing using two-component composite dye.

Therefore, it is expected that the present invention can improve the flexibility of the galchanical products obtained by the pleasure dyeing and improve the touch, thereby enhancing the consumer's preference and contributing to the production of high-quality clothes.

Fig. 1 is a comparative photograph of a combined dyeing sample of persimmon dye and sensation / sensation
Fig. 2 is a graph showing the results of laminarity test
FIG. 3 is a photograph of the lecture test for the combined dyeing of persimmon dye and persimmon /
4A and 4B are graphs showing the catechin content of the common fruit juice powder and the sensory / rheactive two-component dye powder prepared according to the present invention
FIG. 5 is a photograph showing the precipitate for alginate extraction
FIG. 6 is a photograph of a lecture test evaluating the effect of improving the flexibility of dyed dye of two-component /
Figure 7 is a photograph of the surface of a textile material by type of dyeing

The present invention proposes a complex dyeing method using persimmon and cotton.

Brown algae, including mosses, contain polysaccharides such as alginic acid and fucoidan. These components are known to play a role in imparting sticky texture, flexibility and elasticity to brown algae. Specifically, it has various properties such as gel formation and viscosity enhancement ability, water absorption ability, and lubrication ability, and thus industrial use is expanding.

In the present invention, unlike the dyeing of the different dyes sequentially in the conventional natural dyeing, the physical stiffness and tactile sensation after evaluating the simultaneous dyeing of the fiber material with the sensitizing dye and the coprecipitating dye, Which is estimated to be improved. Through the simultaneous dyeing, it was possible to improve the stiffness of the conventional galche by enhancing the flexibility while maintaining the traditional color of the persimmon dye.

On the other hand, there has been no report on the development of bicomponent dyes by mixing other natural substances or pigments with dyes using putty juice when dyeing with impurities. In the present invention, a bicomponent dyestuff mixed with persimmon and menthol and a natural dyeing method using the same are proposed. The complex dyes mixed with the different components of the sensory sensation are respectively removed from the senses and the impurities contained in the senses, and the senses and senses are mixed in a weight ratio of 10: 1 to 20: 1, followed by hot water extraction, followed by drying and pulverization. It was possible to obtain a binary composite dye with finer and uniform particle than the mixture of the dye and the dye before the hot water extraction. As a result of natural dyeing using sensory and sensory bimetallic composite dyes, it was confirmed that the color characteristics and uniformity of the dyeing fabric were better than those of the simultaneous dyeing of the sensitive dye and the sensitive dye. In the simultaneous compound dyeing of the sensitizing dye and the coprecipitating dye, the ratio of the dyed dye or the dyed / dyed composite dye is related to the degree of improvement of the dyed dye due to the dyed dye in the natural dyeing process. When the dyed dye is too small, Improvement is small, and conversely, there is no improvement in flexibility even when excessive. The two-component composite dye of the present invention has a particle size of 520 nm or less and can maintain a catechin content of 90% or more.

In the present invention, as a sensitizing dye, generally a dried persimmon can be used, or a dried persimmon powder can be used, which is obtained by mixing and pulverizing a foot sensation with water. In addition, as a captive dye, a hot-water extract of menthol may be used, or a dry powder of a boiled juice obtained in a menthol processing may be used. In case of two-component complex dye, it may be obtained by directly mixing the foot sensation and the sensation with water and extracting with hot water. Alternatively, it may be obtained by mixing the sensory powder with the prepared sensory preparation, mixing the sensory powder with the sensory powder, and extracting with hot water.

For simultaneous dyeing, the concentration of the sensitizing dye may be in the range of 500% owf to 800% owf, and the sensitivity of the dye may be in the range of 10% owf to 70% owf. Also, when natural dyeing is performed with a sensory / bicomponent composite dye, the dye concentration may be in the range of 500% owf to 900% owf. In the natural dyeing according to the present invention, the weight ratio of the fabric and the salt solution may be, for example, in the range of 1:50 to 1: 300, and the dyeing temperature may be, for example, 50 to 80 ° C, For example, from 20 minutes to 50 minutes.

Hereinafter, the technical structure and effects of the present invention will be described in more detail with reference to specific examples.

The sensory / Emotional  Complex dyeing condition

When dyed cotton fabrics were prepared with freeze-dried persimmon extracts, the dyestuffs concentration of 500% and 800% (owf), which is the condition for the color of traditional perspex fabric (galche) (0, 5, 10, 30%) by the following three steps.

Process A: Sensory dyes (sequential dyeing) after subtractive coloring and daylighting

Step B: Staining / coloring of the infection after infection (sequential staining)

Step C: One-bath, which is a mixture of sensory and sensory dyes simultaneously, is dyed and exposed to sunlight (simultaneous dyeing)

The samples of each process were subjected to 10 days (8 hours of daylight exposure / day x 10 days) of daylighting, and the dyeing was completed. The color results of the dyed material are shown in Table 1 (sensitivity 500%) and Table 2 (sensitivity 800%).

The complex dyeing conditions of color difference (ㅿ E) of 3 or less, which is the same color / tone as that of sensory dyes and hardly distinguish color difference from human eyes by conditions of 500% and 800% And a mixed dyeing C process. Therefore, it was concluded that the C process, which is the dyeing of the sensory and temporal patterns simultaneously, is considered to be the best technique for complex dyeing of the senses while maintaining the intrinsic color of the hypothetical dye in the range of 5 ~ 30%

Maintain a unique color of persimmon Moth  Concentration range

As the concentration of the dermatophyte increases, it may change from the inherent color of the dyes. Therefore, it is possible to reproduce the dermatophyte from 5% to 100% (owf) using C process, And the concentration of phlegm which did not deviate greatly. The color results of the sensory / temporal composite staining obtained by the combined dyeing technique of sensation / attenuation are shown in Table 3 (sensitivity 500%) and Table 4 (sensitivity 800%). As a result, it was judged that the dyeing condition was able to maintain intrinsic color up to 50%. As shown in FIG. 1, these results can be confirmed in comparative photographs with the combined dyeing samples of the persimmon dyeing and sensation / attenuation for the 500% and 800% of the sensitizing densities, respectively.

feeling/ Moth  Composite dyeing for improving flexibility of simultaneous composite dyeing materials

The flexibility of the composite dyed fiber fabric was evaluated by using the lecture experiment (KS K 0539).

The specimens were cut into 2.5 × 15 cm pieces (2 pieces each in the warp / weft direction, oblique direction, one piece measured on the surface and one piece measured on the back side) according to the cantilever method. , The test specimen was placed so that the front end of the test specimen came to the end of the flat end and then the test specimen was gently pushed and the length of the specimen pushed until the end reached the slope was checked to the mm level.

The lecture E is calculated by the following equation. The larger the E value, the less flexible and stiff specimens are interpreted.

E (cm.g) = C ³ x W

Where C = D / 2, D: Length (cm) of the specimen pushed up to reach the slope, and W: Average weight of the specimen (g / cm ² ).

Table 5 and Fig. 2 show the results of the laminating properties of the fiber materials which were simultaneously dyed at a concentration range of 0 to 100% for an 800% concentration.

In the trend of E-value of the lecture, it was found that the sample with 800% sensitivity and 0% sensitivity showed 2.43 lattice. The samples with simultaneous complex staining showed a gradual decrease in lattice constant Respectively. In the case of 100% concentration of complex staining, the result showed that the stiffness was higher than that when the stain was stained alone. This means that if the stain concentration is too high, the stiffness becomes higher due to the increase of the weight of the fabric . Therefore, it can be concluded that the optimal concentration of the senses which can improve the flexibility of 800% single dyeing material by 50%

As a result, when treated with a composite dyeing dye, which is known to have a flexibility imparting substance such as algin, and persimmon dyeing which is traditionally stiff, the lyophilicity is reduced by about 30% It is expected that it will be possible to give a more flexible touch to the consumer, which will further enhance the satisfaction of the consumer in the dyeing fashion material.

FIG. 3 shows a photograph of a lecture test evaluating the flexibility improvement effect on the sensitivity (800% of concentration) and the complex staining (800% of sensory score, 50% of sensory score) simultaneously. The dampened material of 800% damping alone has a longer length (D) until it touches the slope of the test equipment, and the overall shape of the damping material is more curved when the damping material is touched, indicating that the material is stiff and more rigid. However, the composite dyed material with the sensation-sensation shortens the length (D) until it reaches the slope and the spatial difference with the slope becomes smaller, which makes the material much more flexible.

feeling/ Moth Heterosexual  Manufacture of composite dyes

After the result that the flexibility of the fiber material is improved when the composite stain of the senses and the senses are simultaneously obtained, the powdered bicomponent dye powder is mixed with the persimmon / horticultural components to enhance the industrialization and commercialization of the sensory / Respectively.

Specifically, the mixture was mixed with 15: 1 to prepare an aqueous solution of about 9%. After heating for 2 hours, the mixture was filtered to remove impurities such as sugar components, followed by lyophilization and pulverization.

The strengths and functionalities of two - component complexes were evaluated by measuring dye particle size, catechin content, fiber lacquer luster, surface color uniformity, and color strength.

i) Dye Particle Size Analysis

The particle size of the bicomponent dyestuff prepared according to the present invention was compared with the particle size of the lyophilized powder and freeze-dried powder of the lyophilized powder, respectively. Table 6 shows the results of measuring the particle size of the three powders by Electrophoretic Light Scattering (ELS-8000: Photal).

The pulverized powder showed an average particle size of 590 nm, the pulverulent powder showed a particle size of 855.1 nm, and the size of the sensory / bicomponent composite dye had a particle size of 519.4 nm, The size was much smaller. It is expected that when used as a dye of a fiber material, the dyeability of the dye is better, and the uniformity of the color is exhibited, so that the overall dyeability is better.

ii) Content of catechin and alginic acid components

In traditional dyeing, catechin is identified as a major component of the dye. Since it is presumed that the main cause of the functional and physical properties of the dyed fiber material is also the action of the catechin, the content of the catechin in the binary dyes having flexibility improved while retaining the traditional subduction color and functionality proposed in the present invention Should be compared with the content of common juice powder.

The content of the catechin component was measured using HPLC (High Performance Liquid Chromatography, LABOGENE ILC3300 HPLC system (UV-VIS), GER), and the common juice powder collected from the same fruit number at the same time, / Catechin composite dye powder are shown in Figs. 4A and 4B, respectively.

The catechin content of the common juice powder was found to be 10.167 μg / mg, and the catechin content of the sensory / bicomponent composite dye powder was 9.127608 μg / mg. The catechin contents of the binary dye powders were slightly lower than those of the catechins except for the catechins which could be lost when filtering the composite dyes. In other words, catechin, which is reported to determine various characteristics of persimmon dyeing as the intrinsic component of persimmon, can be maintained without any significant change in sensory / bivalent composite dyes.

Next, the content of alginic acid component was confirmed. Since alginic acid is a polysaccharide, measuring the exact content requires a high level of technical expertise. Therefore, in this embodiment, the alginic acid precipitate was obtained in a general alginic acid extraction step, and the alginate retention and maintenance state of the ginseng / gentle bimetallic dyes were examined.

For this purpose, the aqueous solution (B) of 0.5% owb dye (A) and 8.5% owb compound (850% owf based on 1 g owf of fabric) CaCl ₂ 15% aqueous solution at a ratio of 1: 1 and left for 20 minutes. It is assumed that the amount of precipitate settling downward is proportional to the amount of alginic acid. FIG. 5 shows precipitates for extracting alginic acid. The color of the precipitates was somewhat different, but the sediment heights of the precipitates were almost similar (A: containing a sensitizing / heterotopic binary compound;

These results indicate that the alginic acid contained in the sensory / bicomponent composite dye of the present invention has an amount similar to that of alginic acid contained in the sensory dyestuff powder. Therefore, the sensory / bicomponent composite dyes proposed in the present invention not only maintain the catechin component of persimmon but also maintain the inherent alginic acid, thus directly contributing to improvement of the flexibility of the dyeing material.

iii) Improved flexibility of dyed / dyed bicomponent dye materials

The flexural strength (E value) of the cotton fiber dyed with the sensitizing / dyed bicomponent dyestuff (concentration 850%, owf) was measured by the same method as above, and the flexibility improvement effect was evaluated when compared with the dyed single dye dyeing.

The results of Table 7 show that the E value of the lacquer is 1.43 cm · g, which is lower than the laminating value of 1.77 at the time of simultaneous dyed dye preparation. Compared with the E value of 2.45, which is a single stain with the pulverized powder, the liner degree is reduced by about 42%, and the stiff feel, which is a disadvantage of the dyed fiber material, can be significantly improved.

Fig. 6 shows a photograph of the lapping test in which the effect of improving the flexibility of the fiber material dyed with the dyed / dyed bicomponent dye was evaluated. As compared with the 800% dyed material alone, the single dyed material has a longer length (D) until it reaches the slope of the test apparatus, and the overall shape at the side is further curved, indicating that the material is stiff and more rigid . However, in the case of the materials dyed with the composite / dyed bicomponent dyes, the length (D) until the contact with the slope was shorter and the spatial difference with the slope was smaller, which made the material much more flexible. In particular, the weft direction of the material dyed with bicomponent dyes becomes more relaxed and approaches the slope of the test apparatus.

iv) Improvement of color uniformity of dye / dyed composite dye materials

The color intensity and color uniformity of the two - component composite dye were evaluated by the color difference (K) between color intensity (K / S), Munsell 's HV / C, PCCS tone, The results are shown in Table 8.

Compared to the case of single dyeing of the powdered persimmon dyes, the sensory and sensory powders were prepared and simultaneously dyed and the dyed / dyed bicomponent dyes were stained with the same color and tone. . However, when staining with a bicomponent dyestuff, the color intensity K / S value was closer to that of the traditional persimmon dyeing, and the color difference (E) value was very close to 1.23, It is anticipated that dye production and process control will be possible to develop colors that are close to the color of traditional dyes.

v) Evaluation of color intensity uniformity

The uniformity of the color intensity K / S value was evaluated by 10 standard deviations of the measured values, and the results are shown in Table 9. [Table 9] < tb > < TABLE >

The standard deviations of the K / S values of the dyed materials of the sensory / dyed composite dyes are smaller than those of the dyed materials of the dyed / dyed composite dyes.

These results can be seen in FIG. 7 which shows the surface color of the actual dyed material according to the dyeing method. (C) The surface of the fibrous material is dyed with a composite dye of a sensory / afferent two component, while the specific dyeing (a) and sensory- It can be seen that the colors feel uniform.

Therefore, it is expected that the difficulty of color quality control in the natural dyeing process which has been pointed out as a disadvantage so far can be improved much more.

Claims (5)

delete delete A composite dye obtained by mixing a first component of a dried persimmon juice or pulp powder with a second component of a pulpy liquor or copepod powder,
The first component and the second component are mixed together with water, the mixture is subjected to hydrothermal extraction and dried, and the first component and the second component are mixed in a weight ratio of 10: 1 to 20: 1,
Characterized in that the composite dye has a particle size of 520 nm or less and a catechin content of 90% or more of a sensitizing dye
Binary complex natural dyes including senses and senses.
delete The method of claim 3,
Wherein the composite dye reduces the lattice property of the dyed material by 40% or more relative to the dyed dye.

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