KR102534978B1 - A Dyeing Method Using Indirobin - Google Patents

Abstract

The present invention relates to a method for extracting and dyeing indirubin from indigo, and more particularly, the time in which pulverized indigo leaves are immersed in water or ethanol and allowed to stand is 24 to 48 hours, which is sufficient time for indirubin to be extracted It relates to a method for extracting and staining indirubin from a side that can produce a red dye with minimized blue color of indigotine by imparting.

Description

Indirubin extraction and staining method from indigo plant {A Dyeing Method Using Indirobin}

The present invention relates to a method for extracting and dyeing indirubin from indigo, and more particularly, the time in which pulverized indigo leaves are immersed in water or ethanol and allowed to stand is 24 to 48 hours, which is sufficient time for indirubin to be extracted It relates to a method for extracting and staining indirubin from a side that can produce a red dye with minimized blue color of indigotine by imparting.

Indigo (scientific name: polygonum indigo) is an annual plant belonging to the dicotyledonous plant Dicotyledonaceae, native to China, and cultivated as a dye resource in the past. The stem stands straight and is 50 to 60 cm tall, with a strong reddish purple color. Fruits are achene, wrapped in calyx, triangular egg shape, about 2mm long, blackish brown.

Plants collectively referred to as indigo are cultivated or grown wild in various varieties throughout the world, including India, China, America, Africa, and Europe. It is represented by such plants, and these plants are used as dyes.

Indigo dyeing and dyeing methods have been with mankind since BC, and even in Korea, information on indigo dyeing methods can be found in ancient literature, and many studies are still being conducted at universities and research institutes.

However, most studies on indigo dyes are focused only on indigotin, which represents indigo, that is, blue-based blue and indigo. However, indigo dye contains not only blue pigment indigotin but also red pigment indirubin, so it is possible to express a reddish indigo color like subblue.

As shown in FIG. 1, indigo leaves contain colorless water-soluble indican, which is a precursor of indigotin, and blue indigotin is produced using this as a starting material. At this time, when indican reacts with oxygen before becoming indigotin, isatin is produced, and when isatin is polymerized with indoxyl, red indirubin is formed. this will be made

Therefore, it is necessary to develop a dyeing method that effectively extracts red indirubin and increases the amount of surface dyeing to the fiber so that it can be dyed in a deep red color.

(patent literature)

Registered Patent Publication No. 10-1689850 (registered on December 20, 2016) "Indigo Dye Manufacturing Method and Indigo Dyeing Method"

The present invention has been made to solve the above problems,

The present invention provides sufficient time for indirubin to be extracted by allowing the pulverized indigo leaves to be immersed in water or ethanol and allowed to stand for 24 to 48 hours, thereby minimizing the blue color of indigotine. It is an object to provide an extraction and dyeing method that can produce a.

An object of the present invention is to provide an extraction and dyeing method that allows dyeing of fibers at room temperature to be dyed at a high concentration when a basic sample is immersed in water to extract dye.

In the present invention, when a basic sample is immersed in alcohol to extract dye, the dye is heated to a certain temperature and then cooled to room temperature to dye the fiber, thereby increasing the concentration of the fiber. It aims to provide

The purpose of the present invention is to provide an extraction and dyeing method that can block the mixing of brown-based colors with fibers by extracting indigo yellow at a high temperature by heating the dye at a temperature of 70 to 90 ° C. .

An object of the present invention is to provide an extraction and dyeing method that can increase the expression rate of indirubin color by adjusting the pH of the dye to be alkaline.

The present invention is implemented by an embodiment having the following configuration in order to achieve the above object.

According to one embodiment of the present invention, the extraction and dyeing method according to the present invention includes a dye extraction step of extracting a dye containing indirubin from indigo leaves, and the dye extraction step is to secrete a basic sample by crushing indigo leaves. A basic sample preparation step, a solvent mixing step of extracting indirubin by mixing the basic sample with water or ethanol, and a stationary step of separating the dye by leaving the solvent mixed with the basic sample for 24 to 48 hours to be characterized

According to another embodiment of the present invention, the extraction and dyeing method according to the present invention is characterized in that it comprises a dyeing step of immersing and dyeing fibers in the dye extracted in the dye extraction step.

According to another embodiment of the present invention, in the extraction and dyeing method according to the present invention, the dyeing step is a dye separation step of separating the supernatant from the dye solution left in the stationary step, and immersing the fibers in the separated dye It includes an immersion step of dyeing, and the immersion step is characterized in that when water is used in the solvent mixing step, the fiber is immersed in the dye at room temperature.

According to another embodiment of the present invention, in the extraction and dyeing method according to the present invention, the dyeing step is a dye separation step of separating the supernatant from the dye solution left in the stationary step, and a heating step of heating the separated dye And, a cooling step of cooling the heated dye, and an immersion step of immersing and dyeing the fiber in the dye cooled to room temperature, and the solvent mixing step is characterized in that ethanol is used as a solvent.

According to another embodiment of the present invention, in the extraction and dyeing method according to the present invention, the heating step is characterized in that the dye is heated to a temperature of 70 ℃ ~ 90 ℃.

According to another embodiment of the present invention, in the extraction and dyeing method according to the present invention, the dyeing step is characterized in that it comprises a pH adjustment step of adjusting the pH of the dye.

According to another embodiment of the present invention, in the extraction and dyeing method according to the present invention, the pH adjusting step is characterized in that the pH of the dye is adjusted to pH 10 to pH 11.

The present invention can obtain the following effects by combining and using the above embodiments and configurations to be described below.

The present invention provides sufficient time for indirubin to be extracted by allowing the pulverized indigo leaves to be immersed in water or ethanol and allowed to stand for 24 to 48 hours, thereby minimizing the blue color of indigotine. has the effect of enabling the creation of

The present invention has the effect of allowing dyeing of fibers at room temperature to be performed at room temperature when dyeing is performed by immersing the basic sample in water so that dyeing of a deep concentration is achieved.

In the present invention, when the basic sample is immersed in alcohol to extract the dye, the dye is heated to a certain temperature and then cooled to room temperature to dye the fiber, thereby increasing the concentration of the fiber.

In the present invention, when heating the dye, the heating is performed at a temperature of 70 to 90 ° C., so that the indigo yellow extraction at high temperature prevents the brown color from being mixed with the fiber.

The present invention has the effect of increasing the expression rate of indirubin color by adjusting the pH of the dye to be alkaline.

1 is a reference diagram showing the production process of indirubin
2 is a flow chart of a method for extracting and staining indirubin from a side according to an embodiment of the present invention
Figure 3 is a photograph showing the staining result according to the stationary time
Figure 4 is a photograph showing the dyeing state according to the temperature of the dye extracted with water as a solvent
Figure 5 is a photograph showing the dyeing state according to the temperature of the dye extracted with ethanol as a solvent
Figure 6 is a photograph showing the dyeing state according to the pH of the dye

Hereinafter, preferred embodiments of the indirubin extraction and staining method from the side according to the present invention will be described in detail with reference to the accompanying drawings. In the following description of the present invention, if it is determined that a detailed description of a known function or configuration may unnecessarily obscure the subject matter of the present invention, the detailed description thereof will be omitted. Throughout the specification, when a part "includes" a certain component, it means that it may further include other components without excluding other components unless otherwise stated.

Referring to the method of extracting and dyeing indirubin from indigo according to an embodiment of the present invention with reference to FIGS. 1 to 6, the extraction and dyeing method includes a dye extraction step of extracting a dye containing indigo from indigo ( S1) and a dyeing step (S2) of immersing and dyeing the fibers in the dye extracted in the dye extraction step (S1).

The extraction and dyeing method according to the present invention extracts a substance representing color from indigo so that fiber can be dyed. to be extracted and dyed.

In particular, the extraction and dyeing method allows the fiber to be dyed in a deep red color through effective extraction of indirubin, and for this purpose, to ensure sufficient stationary time in the dye extraction step (S1), to adjust the temperature and pH of

The dye extraction step (S1) is a configuration for extracting a dye containing indirubin (C ₁₆ H ₁₀ N ₂ 0 ₂ , mw = 262.26) from indigo, using water (distilled water) or ethanol (EtOH) as a solvent. so that extraction can take place. In the dye extraction step (S1), indigo leaves can be extracted by putting the indigo leaves in water or ethanol. do. To this end, the dye extraction step (S1) may include a basic sample preparation step (S11), a solvent mixing step (S12), and a stationary step (S13).

The basic sample preparation step (S11) is a process of preparing a basic sample using indigo leaves, and the indigo leaves can be separated, washed, and then refined, and the indigo leaves can be pulverized to be mixed with a solvent.

The solvent mixing step (S12) is a process of mixing the pulverized side leaves with a solvent, and indirubin can be extracted by mixing with water (distilled water) or by mixing ethanol in addition to water. In addition, the process of the dyeing step (S2) may be set differently depending on whether or not ethanol is included in the solvent mixing step (S12).

The stationary step (S13) is a process of providing sufficient time for the dye and precipitate to be separated by leaving the solvent mixed with the basic sample for a certain period of time in the solvent mixing step (S12). In particular, indirubin is extracted. Make sure to give it enough time. At the beginning of the stationary step (S13), indicotin is mainly produced, resulting in blue color when dyeing the fiber, and in the case of dyeing with the conventional indigo extract, the stationary time is generally reduced so that blue color can be effectively dyed. On the other hand, it was confirmed that the generation of indirubin becomes active when time elapses in a state in which the solvent is mixed. It can be made, and when 48 hours elapsed, a significant increase in concentration could not be confirmed. Therefore, in the stationary step (S13), the extraction rate of indirubin can be increased by mixing the divided leaves with a solvent and allowing them to undergo a stationary process for 24 hours or more and 48 hours or less.

The dyeing step (S2) is a process of dyeing the fiber using the dye extracted in the dye extraction step (S1), and dyeing is performed using a dye containing indirubin. In particular, in the dyeing step (S2), the temperature and pH of the dye are adjusted in order to dye the fiber in a deep red color, and the process can be made differently depending on the type of solvent. The dyeing step (S2) may include a dye separation step (S21), a pH adjustment step (S22), and an immersion step (S25), and when the solvent is ethanol, a heating step (S23) before the immersion step (S25). ) and a cooling step (S24).

The dye separation step (S21) is a configuration in which the dye is separated from the mixture through the stationary step (S13), and a part of the supernatant is separated, and additional filtration may be performed.

The pH adjusting step (S22) is a configuration for adjusting the acidity (pH) of the dye, and preferably, the pH can be adjusted through the introduction of K2CO3, NaOH, and the like. In the pH adjusting step (S22), the surface adhesion of indirubin to fibers increases when it has alkalinity, and preferably has an acidity of pH 10 to pH 11.

The heating step (S23) is a configuration of heating the dye, and may be subjected to a heating process only when ethanol is used as a solvent. In the heating step (S23), it is preferable to heat the dye at a temperature of 70 to 90 ° C. When the temperature exceeds 90 ° C., indigo yellow is dyed to the fiber due to the high temperature, so that the fiber turns brown.

The cooling step (S24) is a process of cooling the dye heated in the heating step (S23), so that it is cooled to room temperature. When ethanol is used as a solvent, when the heated dye is cooled to room temperature to immerse the fiber rather than immersed in the heated dye, the dyeing rate of indirubin is increased and dyeing with a deeper concentration is achieved. Therefore, when ethanol is used as a solvent, in the cooling step (S24), dyeing is performed by immersing the fiber in a state in which the dye is cooled to room temperature.

The immersion step (S25) is a configuration in which dyeing is performed by immersing the fiber in the dye containing indirubin. When water is used as a solvent, the fiber is immersed in the dye at room temperature without heating, , When ethanol is used as a solvent, the fiber is immersed in the dye cooled after heating.

Hereinafter, various experimental examples and embodiments of the present invention will be described, but such embodiments are only one embodiment for implementing the technical idea of the present invention, and any changes or modifications may be made as long as the technical idea of the present invention is implemented. It should be construed as falling within the scope of the invention.

<Example 1> Preparation of dye for evaluation of dyeing according to standing time

1) A basic sample was prepared by pulverizing 100 g of raw indigo leaf with a general blend (800W) for 60 seconds, mixing the basic sample with 1000 mL of water, allowing it to stand for 1 hour, and separating the supernatant to prepare dye 1.

2) A basic sample was prepared by pulverizing 100 g of raw indigo leaf with a general blend (800W) for 60 seconds, mixing the basic sample with 1000 mL of water, leaving it for 4 hours, and separating the supernatant to prepare dye 2.

3) 100 g of fresh indigo leaf was ground with a general blend (800 W) for 60 seconds to prepare a basic sample, and the basic sample was mixed with 1000 mL of water, allowed to stand for 8 hours, and the supernatant was separated to prepare dye 3.

4) A basic sample was prepared by pulverizing 100 g of raw indigo leaf with a general blend (800W) for 60 seconds, mixing the basic sample with 1000 mL of water, leaving it for 24 hours, and separating the supernatant to prepare dye 4.

5) 100 g of raw indigo leaf was ground with a general blend (800 W) for 60 seconds to prepare a basic sample, and the basic sample was mixed with 1000 mL of water, allowed to stand for 48 hours, and the supernatant was separated to prepare dye 5.

<Experimental Example 1> Dyeing evaluation according to standing time

1) The silk fabric was immersed in dyes 1 to 5 at room temperature and dyed for 40 minutes. The results of the dyeing were as shown in FIG. 3, and FIGS. The results of staining with dye 5 are shown.

2) As can be seen in FIG. 3, it can be seen that blue and green indicotins are dyed on the fibers in less than 8 hours of standing time (dye 1, 2), and even in the case of 8-hour dyeing (dye 3), very light concentration Le dyed red. As shown in FIG. 3(d), the red color appeared clearly only after 24 hours, and as shown in FIG. 3(e), the deepest red color concentration was shown at 48 hours. Therefore, it can be confirmed that indirubin is sufficiently dyed and dyed with a deep red color after 24 hours or more.

<Example 2> Preparation of dye for dyeing evaluation according to the temperature of the dye (solvent: water)

1) A basic sample was prepared by pulverizing 150 g of raw indigo leaves with a general blend (800W) for 60 seconds, and the basic sample was mixed with 1500 mL of water, allowed to stand for 48 hours, and the supernatant was separated to prepare dye 5 at room temperature.

2) A basic sample was prepared by grinding 150 g of fresh indigo leaves with a general blend (800W) for 60 seconds, and the basic sample was mixed with 1500 mL of water, left for 48 hours, and the supernatant was separated to prepare dye 6 heated to 70 ° C. .

3) Prepare a basic sample by grinding 150g of raw indigo leaves with a general blend (800W) for 60 seconds, mix the basic sample with 1500mL of water, leave it for 48 hours, separate the supernatant, heat it to 70℃, and cool it to room temperature. Dye 7 was manufactured.

<Experimental Example 2> Dyeing evaluation according to the temperature of the dye (solvent: water)

1) Dyeing was performed for 40 minutes by immersing the silk fabric in dyes 5 to 7, and the results of the dyeing were shown in FIG. 4, FIG. 4 (a) to (c) are dyes 5 to 7, respectively The results of staining are shown.

2) As shown in FIG. 4 (a), when the solvent is water, it can be seen that the silk sample is dyed in the brightest red color in dye 5 at room temperature, and in the case of dye 6 where the dye is heated to a high temperature, indigo yellow is dyed As it was dyed, a brown color was dyed, and in the case of dye 7 cooled after heating, it was confirmed that the dyeing concentration was very light. Therefore, it can be confirmed that when the solvent is water, it can be dyed with the most reddish color at room temperature and with the highest concentration.

<Example 3> Preparation of dye for evaluation of dyeing according to the temperature of the dye (solvent: ethanol)

1) A basic sample was prepared by pulverizing 150 g of fresh indigo leaves with a general blend (800W) for 60 seconds, and the basic sample was mixed with 1500 mL of water and 500 mL of ethanol, allowed to stand for 48 hours, and the supernatant was separated to prepare dye 8 at room temperature. .

2) Prepare a basic sample by pulverizing 150g of raw indigo leaves with a general blend (800W) for 60 seconds, mix the basic sample with 1500mL of water and 500mL of ethanol, leave it for 48 hours, separate the supernatant, and heat it at 70℃ Dye 9 was manufactured.

3) Prepare a basic sample by pulverizing 150g of fresh indigo leaves with a general blend (800W) for 60 seconds, mix the basic sample with 1500mL of water and 500mL of ethanol, leave it for 48 hours, separate the supernatant, heat it to 70℃, and bring it to room temperature. Chilled Dye 10 was prepared.

4) Prepare a basic sample by pulverizing 150g of raw indigo leaves with a general blend (800W) for 60 seconds, mix the basic sample with 1500mL of water and 500mL of ethanol, leave it for 48 hours, separate the supernatant, heat it to 100℃, and bring it to room temperature. Chilled dye 11 was prepared.

<Experimental Example 3> Dyeing evaluation according to the temperature of the dye (solvent: ethanol)

1) Dyeing was performed for 40 minutes by immersing the silk fabric in dyes 8 to 11, and the results of the dyeing were shown in FIG. 5, and FIG. The results of staining are shown.

2) When the solvent is ethanol As shown in FIG. 5(c), it can be confirmed that dye 10, which is heated to 70° C. and then cooled at room temperature, dyes the silk sample in the deepest red color. In addition, in the case of dye 11 in which the dye was heated and cooled to 100° C., it can be confirmed that the dye is dyed brown according to the dyeing of indigo yellow according to the high temperature. Therefore, when the solvent is ethanol, it can be confirmed that heating to an appropriate temperature is important because overheating to an excessively high temperature prevents dyeing in a vivid red color.

<Example 4> Preparation of dye for evaluation of staining according to pH

1) Prepare a basic sample by grinding 200g of raw indigo leaf with a general blend (800W) for 60 seconds, mix the basic sample with 1500mL of water and 500mL of ethanol, leave it for 48 hours, separate the supernatant, and add K ₂ CO ₃ and prepared with an acidity of pH 11, and dye 12 was prepared with a pH of 7 using citric acid (C ₆ H ₈ O ₇ ).

2) Prepare a basic sample by grinding 200g of fresh indigo leaves with a general blend (800W) for 60 seconds, mix the basic sample with 1500mL of water and 500mL of ethanol, leave it for 48 hours, separate the supernatant, and add K ₂ CO ₃ Then, dye 13 was prepared at pH 9 using citric acid (C ₆ H ₈ O ₇ ).

3) Prepare a basic sample by pulverizing 200g of fresh indigo leaves with a general blend (800W) for 60 seconds, mix the basic sample with 1500mL of water and 500mL of ethanol, leave it for 48 hours, separate the supernatant, and add K ₂ CO ₃ Then, the dye 14 was prepared at pH 10 using citric acid (C ₆ H ₈ O ₇ ).

4) Prepare a basic sample by pulverizing 200g of raw indigo leaves with a general blend (800W) for 60 seconds, mix the basic sample with 1500mL of water and 500mL of ethanol, leave it for 48 hours, separate the supernatant, and add K ₂ CO ₃ Dye 15 was prepared with an acidity of pH 11.

<Experimental Example 4> Dyeing evaluation according to pH

1) Dyeing was performed for 40 minutes by immersing the silk fabric in dyes 12 to 15, and the results of the dyeing were shown in FIG. 6, FIG. 6 (a) to (d) are dyes 12 to 15, respectively The results of staining are shown.

2) As shown in FIG. 6, it can be seen that the higher the alkalinity, the thicker the red color concentration, and when the pH is higher than 10, it can be confirmed that a sufficiently vivid red color can be dyed.

In the above, the applicant has described various embodiments of the present invention, but such embodiments are only one embodiment for implementing the technical idea of the present invention, and any changes or modifications are made according to the present invention as long as the technical idea of the present invention is implemented. should be construed as falling within the scope of

S1: Dye extraction step
S11: basic sample preparation step S2: solvent mixing step S3: stationary step
S2: staining step
S21: dye separation step S22: pH adjustment step S23: heating step
S24: cooling step S25: immersion step

Claims (7)

A dye extraction step of extracting a dye containing indirubin from the side, and a dyeing step of dyeing the fiber by immersing the dye in the dye extracted in the dye extraction step,
The dye extraction step,
A basic sample preparation step of crushing indigo leaves to secrete a basic sample, a solvent mixing step of mixing the basic sample with ethanol to extract indirubin, and separating the dye by leaving the solvent mixed with the basic sample for 24 to 48 hours including the political stage of
The dyeing step is
A dye separation step of separating the supernatant from the dye solution left in the stationary step, a heating step of heating the separated dye, a cooling step of cooling the heated dye, and an immersion step of dyeing the fiber by immersing the dye in the dye cooled to room temperature. including,
The solvent mixing step uses ethanol as a solvent,
The heating step is to heat the dye at a temperature of 70 ℃ ~ 90 ℃, extraction and dyeing method, characterized in that to dye the fiber in a vivid red color. delete delete delete delete delete delete

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