KR102002258B1 - Method of dyeing with gardenia extract and natural mordant - Google Patents

Abstract

The present invention relates to a dyeing method using cellulose nanofibers as a natural mordant dye and, more specifically, to a dyeing method for producing a dyeing solution by mixing a gardenia extract with a cellulose nanofiber suspension. Accordingly, the dyeing method is harmless to the human body, and dyeability and the fastness of color are excellent.

Description

METHOD OF DYEING WITH GARDENIA EXTRACT AND NATURAL MORDANT "

The present invention relates to a method for dyeing natural mordants and gardenia extract, and more particularly, to a method for dyeing a cellulose nano fiber harmless to human body as a natural mordant and mixing a gardenia known as a yellow dye directly into a cellulose nanofiber suspension .

As concerns and anxieties about wellness deepen, we consider the functionality of hygiene and health improvement and place high value on eco-friendly and human-friendly functions. Particularly, clothes and bedding products are objects that are always in contact with human beings in everyday life, but may be harmful to human body, and household goods derived from natural materials are attracting attention.

The type of fibers used and the dyes used are almost limited. This is because the mode of bonding between the fibers and the dye that occurs when dyeing is determined by the kind of the fiber and the reaction method of the dye, and it is difficult to obtain a predetermined color due to incomplete dyeing in other methods.

In the case of cellulose fibers, direct dyes, sulfide dyes, Vat dyes, naphthol dyes or reactive dyes are mainly used. In the case of wool or hides, acid dyes, acid mordant dyes, metal complex dyes or reactive dyes are mainly used. The mordant is mainly chemically synthesized, which adversely affects the skin and may cause atopy and the like.

Therefore, although dyeing derived from natural materials has been spotlighted as an alternative, dyeing derived from natural materials has a problem that the durability of the fiber is lowered or characteristics change due to processing or manipulation to increase the durability, .

In addition, mordanting refers to a process of treating dyeing before and after dyeing to help color development and sticking of a salt solution. It enhances the dye-dye binding property, increases dye fastness, promotes dye adsorption, .

The mordant has a mordant before dyeing and a mordant after dyeing. There is also a mordant which simultaneously dye mordant with a mordant in a salt solution, and a mordant which does not mordant depending on the dye. Chromium salts (chromium alum, chromium chloride, chromium chloride, etc.), iron salts (iron sulfate, iron acetate, etc.) and the like are mainly used as mordants. In many cases, the color varies depending on the type of the metal ion. The metal salts combine with the dye to become insoluble rake and adhere to the fiber.

However, most of these mordants are synthetic mordants harmful to human body. Accordingly, there is a continuing need for a mordant comprising a natural substance that is harmless to the human body and can be usefully used as a mordant.

According to one embodiment of the present application, there is provided a harmless dyeing method using a natural mordant agent.

According to one embodiment of the present application, there is provided a dyeing method excellent in fastness.

According to one embodiment of the present application, a dyeing method excellent in functionality is provided.

According to one embodiment of the present application, there is provided a yellow dyeing method using a gardenia extract.

According to one embodiment of the present application, there is provided a dyeing method using a cellulose nanofiber as a natural mordant.

According to one embodiment of the present application, there is provided a dyeing method in which a suspension of cellulose nanofibers is directly mixed with a gardenia extract and used as a dyeing solution.

The present application relates to a method of dyeing with a natural mordant and a gardenia extract.

As an example, preparing a dyestuff; Refining the dyestuff; Dyeing the refined dyed material with a mixture of a cellulose nanofiber suspension and a gardenia extract; Washing the dyed dyed material; And drying the washed dyed matter, wherein the mixture of the gardenia extract and the cellulose nanofiber suspension is mixed at a weight ratio of 1:10 to 30.

As an example, the dyes are either cotton, hemp, rayon, hair and silk.

As an example, the cellulose nanofiber suspension contains 0.5 to 3.5% by weight of the cellulose nanofibers.

In one example, the cellulose nanofibers and the crocin of the gardenia extract form a chemical bond.

As an example, preparing a dyestuff; Refining the dyestuff; Cellulose nanofibers and a gardenia extract in a weight ratio of 1: 5 to 100, dyes the refined dyes at 50 to 110 DEG C for 20 to 100 minutes; Washing the dyed dyed material; And drying the washed dyed material. In the dyeing step, when the dyeing temperature is increased, the dyeing time is reduced.

As an example, the dyeing step is performed at 100 占 폚 for 30 minutes.

As an example, the staining step is carried out at 60 占 폚 for 90 minutes.

As an example, the method further comprises dyeing the dried extracts with the gardenia extract alone.

The present invention provides a natural mordant agent comprising cellulose nano fibers, 0.5 to 3.5% by weight of a cellulose nanofiber, and the balance being water.

As an example, the cellulose nanofibers are included in an amount of 0.5 to 1.5% by weight.

The present application provides dyed dyes dyed with a gardenia extract and dyed by a mixture of a suspension of cellulose nanofibers, which are natural mordants mentioned above, and a gardenia extract.

As an example, the dyes are either cotton, hemp, rayon, hair and silk.

As an example, the mixture is a mixture of a gardenia extract and a cellulose nanofiber suspension in a weight ratio of 1:10 to 30.

According to one embodiment of the present application, a harmless dyeing method can be provided to the human body by using a salt mildew salt.

According to one embodiment of the present application, a method of staining using a cellulose suspension directly can be provided.

In addition, a dyeing method excellent in fastness and functionality is provided. In addition, a yellow dyeing method using a gardenia extract is provided.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a flow chart of a method for dyeing with natural mordants and gardenia extract, an embodiment of the present application.
FIG. 2 is a graph showing the color characteristics measured after dyed with a gardenia extract in the case where the cellulose fiber nanofibers are included or not. FIG.

The terminology used in this application is used only to describe a specific embodiment and is not intended to limit the invention. The singular expressions include plural expressions unless the context clearly dictates otherwise. In the present application, the term "comprises" or "having" is intended to designate the presence of stated features, elements, etc., and not one or more other features, It does not mean that there is none.

Unless defined otherwise, all terms used herein, including technical or scientific terms, have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Terms such as those defined in commonly used dictionaries are to be interpreted as having a meaning consistent with the contextual meaning of the related art and are to be interpreted as either ideal or overly formal in the sense of the present application Do not.

Dyeing refers to dyeing in a dyeing liquid which is transferred to the inside of the dyed materials such as fibers, films, and reversals through a medium such as water, and is bonded to the dyed materials by physicochemical reaction to have a certain degree of fastness. Depending on the combination of fibers and dyes, the dyeing mechanism is changed. Dyeing properties vary depending on dyeing conditions such as concentration, pH, bath ratio, and preparation. The present application provides a method of dyeing a gardenia having an excellent fastness using a cellulose nano fiber which is a natural mordanting agent.

Fastness refers to the degree of durability and resistance to various internal or external conditions of the dyeing dye. It is the fastness of the dyeing, which indicates the degree of resistance and durability to various internal or external conditions, such as light fastness, washing fastness, wash fastness, friction fastness, seawater fastness, chlorine fastness, Fastness or sublimation fastness, but especially light fastness and wash fastness are important. Dyed fiber products are required to have sufficient resistance and durability for performance and usage conditions in the manufacturing process or during use. They are used in various applications such as daylight, washing, weather, sweat, friction, water, chlorine bleaching, If you get it, it will fade or discolor. The color resistance to these external conditions is dye fastness, which is the most important item in evaluating dye performance. The dye fastness varies considerably depending on the nature of the dye, the dyeing state of the dye, the amount of dyeing, the properties of the fiber, the surface state of the dye, and the processing agent in the fiber.

Hereinafter, a method of dyeing using natural mordants and gardenia extract of the present application will be described with reference to the accompanying drawings. The accompanying drawings are illustrative and the scope of the dyeing method using natural mordants and gardenia extract And the like.

BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a flow chart of a method for dyeing with natural mordants and gardenia extract, an embodiment of the present application.

As shown in Fig. 1, first, a dyestuff is prepared (S110). The dyes are available in both animal and vegetable fabrics. Specifically, the dyes are not particularly limited, but are cotton, hemp, rayon, wool, and silk.

Then, the prepared dyestuff is refined (S120). Refining is the preparation process to remove foreign substances and chemical components contained in the fiber and complete bleaching or dyeing. Here, the method of refining the dyed material is not particularly limited, and the refining method used in the art can be used. In addition, the scouring method may be different depending on each dyestuff. In the following Experimental Examples, preferred refining methods and conditions are described. However, the present application is not limited to such refining methods and conditions.

Then, the refined dyed material is dyed using a mixture of cellulose nanofiber and gardenia extract (S130).

Gardenia Jasminoides is an evergreen tree with a temperate coastline, its leaves are shiny, and the white flowers blooming in June have a strong aroma, making them a beautiful landscape gardener. Gardenia fruit is widely used as a non-polluting natural dye or as an industrial and medicinal plant. In particular, gardenia is used for dyeing yellow or yellow, which is caused by crocin. Crocin is represented by the following formula (1).

[Chemical Formula 1]

Cellulose nanofibers are natural products, and cellulosic nanofibers are nano- or micrometer-sized rod-shaped particles or fibers that are tightly bundled together in a cellulosic chain. Cellulose is represented by the following formula (2).

(2)

In the present application, such cellulose nanofibers are used as natural mordants. The mordant is a process of treating the dyed material before and after dyeing to help the coloration and the fixation of the dye solution. It enhances the binding property between the dyed dye and the dye, increases the fastness to dyeing, promotes the dye adsorption and increases the color of the dyeing fabric. do. Thus, it can be said to be an operation mediating fiber dyeing.

As an example of the present application, a mixture of a cellulose nanofiber suspension and a gardenia extract is used. The cellulose nanofiber suspension contains 2.5 to 3.5% by weight of the cellulose nanofibers, and the balance may be water. Here, it is preferable that a mixture of the gardenia extract and the cellulose nanofiber suspension are mixed at a weight ratio of 1:10 to 30. In the present application, the mixture contained in this proportion is referred to as a suspension.

One of the characteristics of the present application is that such a suspension is used for direct dyeing. Through this, the dyeability can be greatly improved.

In addition, the cellulose nanofibers and the crocin of the gardenia extract form a chemical bond.

As another example of the present application, a mixture of a cellulose nano fiber diluted with a gardenia extract is used. Cellulose nanofibers and gardenia extract in a weight ratio of 1: 5 to 100, and the refined dyed material is preferably dyed at 50 to 110 DEG C for 20 to 100 minutes.

That is, if dyeing is carried out at a high temperature of 100 占 폚, dyeing is preferably performed for 30 minutes, and if dyeing is performed at a low temperature of 60 占 폚, dyeing is preferably performed for 90 minutes.

Then, the dyed dyed material is washed (S140). Here, the method of washing the dyed material is not particularly limited, and a cleaning method used in the art can be used. Cleaning can be carried out until no dye comes out of the dyed material. Particularly, the cleaning can be carried out at 20 to 40 캜, more preferably at 30 캜. In addition, preferred cleaning methods and conditions are described in the following experimental examples. However, the present application is not limited to such cleaning methods and conditions.

If necessary, a plurality of washes, such as one or more times, such as two or three times, may be performed to provide a washed undyed salt intended for the present application.

Then, the washed dyed material is dried (S150). Here, the method of drying the dyed material is not particularly limited, and the drying method used in the art can be used. As one example, it can be naturally dried. In addition, preferable drying methods and conditions in the following experimental examples will be described. However, the present application is not limited to such drying methods and conditions.

In addition, this method may further include a step of dying the dried artichoke extract alone with a gardenia extract. For purposes of this application, dyeing may be performed two or more times. For example, when the staining is performed twice, the first staining method and conditions may be the same as the second staining method and conditions, and some methods and conditions may be different.

The present invention also provides a natural mordant agent comprising a cellulose nanofiber, wherein the natural mordant agent comprises 0.5 to 3.5% by weight of a cellulose nanofiber, and the balance is mixed with water to provide a natural mordant agent. More preferably 0.5 to 1.5% by weight of the cellulose nanofibers.

In addition, the present application provides such a method, specifically a dyed substance produced using a cellulose nanofiber suspension.

Specifically, the present application provides a dyed dyed material by a mixture of a suspension of cellulose nanofibers, which are natural mordants, and a gardenia extract. The dyes are cotton, hemp, rayon, wool, and silk. The gardenia extract and the cellulose nanofiber suspension are mixed in a weight ratio of 1:10 to 30.

Hereinafter, the present application will be described in more detail through an experimental example.

( Experimental Example  One)

To confirm the characteristics of the natural mordant, dyeing was carried out under various conditions. First, rayon and silk were used as dyes. Specific specifications of the fabrics used are shown in Table 1 below.

The rayon was refined using distilled water (600 ml) and soap (0.8 g) at 70 ° C for 30 minutes. Silk, distilled water (100ml), soap (3.2g) and Na ₂ CO ₃ (0.8 g) at 90 캜 for 15 minutes.

The powder of the gardenia was produced from a commercial product manufactured by Anseongri 84 (source: Samhong Molsan), northeast of the Hwasun Gun, South Jeolla Province, Korea. Cellulose nanofiber (CNF) was manufactured by Asian Nano Cellulose Co., Ltd. Specific specifications of CNF are shown in Table 2. Two types of CNFs were used for the B5 and O1 types. The specifications for both types are the same as those shown in Table 2, and CNF O1 is more dilute than B5.

The gardenia extract was extracted with Liquid 1:20 at 90 ℃ for 20 minutes. The pH of the extract was 6 and neutral.

1L of the gardenia extract was added with refined cotton and stirred at 80 ° C for 1 hour. Five grams of Gardenia Extract + CNF (B5) and 5g of Gardenia Extract + CNF (O1) were stained with each rayon / silk fabric under the changed conditions. Thereafter, it was rinsed twice with distilled water and then dried. The pH of the saline solution was 6 and neutral.

The L *, a * and b * values of CIE were measured under the conditions of D65-10 light source using a spectrophotometer (COLOR-EYE 3100, Macbeth ^ⓡ , USA) as the color characteristics of the dyed fabric. A turbidity meter (ATAGO, REFRACTOMETER, PAL-1, JAPAN) was used to measure the turbidity before and after dyeing. In addition, a sugar content meter (Lutron, TURBIDITY METER, TU-2016, TAIWAN) was used to measure the sugar content before and after dyeing. Lab, turbidity and sugar content were measured for each, and are shown in Tables 3 to 5, respectively.

As shown in Tables 3 to 5, the L value of CNF (B5) was lower overall, and the color fastness of CNF (B5) was comparatively excellent. In addition, turbidity was increased in gardenia extract + 5 g of CNF (B5) + rayon, but turbidity was decreased after dyeing as a whole, so it was judged that the dye adhered well to the fiber. And, sugar content means g of sugar dissolved in water per 100g. Overall, the sugar content increased after dyeing, so CNF, the sugar component, was likely to remain in the saline solution after staining.

( Experimental Example  2)

For further experiments, cotton, rayon and silk were used as the dyes. Specific specifications of the fabric used are shown in Table 6 below.

The surface was refined using distilled water (400 ml) and NaOH (1 g) at 100 ° C for 30 minutes. The rayon and silk were refined in the same manner as in Experimental Example 1. In addition, the same products as in Experimental Example 1 were used for the germanium powder and CNF. The gardenia extract was also extracted in the same manner as in Experimental Example 1.

The polished surface of 800 mL of gardenia extract was stirred and stained at 80 ° C for 1 hour. Ten grams of Gardenia Extract + CNF (B5) and 10 g of Gardenia Extract + CNF (O1) were stained on each side / rayon / silk fabric. Thereafter, it was rinsed twice with distilled water and then dried. The pH of the saline solution was 6 and neutral.

The Lab, turbidity and sugar content of each dyed fabric were measured in the same manner as in Experimental Example 1 and are shown in Tables 7 to 9, respectively.

As shown in Tables 7 to 9, the L value of CNF (O1) and CNF (B5) was low in silk, and the L value of CNF (O1) and CNF (B5) was high in cotton and rayon. Turbidity increased with cotton and silk in the case of CNF (B5) after dyeing, and rayon decreased. CNF (O1) increased only in plane, and rayon and silk decreased. In the case of CNF (B5), sugar content increased, while rayon and silk decreased. CNF (O1) decreased only in the face and rayon and silk fiber increased.

( Experimental Example  3)

In order to improve the fastness of natural dyeing, additional experiments were conducted to confirm whether CNF (A1, B1 (evaporation), B5, O1) served as a mordant. CNF (A1, B1 (evaporation), B5, and O1) were simultaneously mordantized by using a powder of gummy powder as a dye for natural dyeing, and then the sugar content and turbidity were compared before and after dyeing. Were compared.

The manure was used as the dyed material. Specific specifications of the fabric used are shown in Table 10 below.

(88 g) was dissolved in distilled water (100 ml), soap (30 g) and Na ₂ CO ₃ (60 g) at 100 캜 for 60 minutes.

In addition, the same products as in Experimental Example 1 were used for the germanium powder and CNF. The gardenia extract was also extracted in the same manner as in Experimental Example 1.

The polished surface of 800 mL of gardenia extract was stirred and stained at 80 ° C for 1 hour. Five grams of Gardenia Extract + CNF (A1, B1 (Evaporation), B5, O1) were stained on the cloth. Thereafter, it was rinsed twice with distilled water and then dried. The pH of the saline solution was 6 and neutral.

Lab, turbidity and sugar content of each dyed fabric were measured in the same manner as in Experimental Example 1, and the results are shown in Tables 11 to 13, respectively.

As shown in Tables 11 to 13, the color fastness was lower in the case of containing CNF than in the case of dyeing alone as a gardenia extract. Especially, L value of Gardenia extract dyeing + CNF B5 5g was lowest after dyeing. However, the difference in L values in all samples was not large. It was confirmed that turbidity was lowered after dyeing in all the samples, and it was confirmed that the dye was adhered to the fiber. The overall sugar content increased after dyeing, but the sugar content decreased with dyeing of Gardenia extract dyeing + CNF B1 5g.

( Experimental Example  4)

Primary staining was carried out in the same manner as in Experimental Example 3, followed by washing and drying, followed by secondary dyeing with the gardenia extract alone, washing and drying as in primary dyeing.

Lab, turbidity and sugar content of each of the dyed fabrics (before and after the primary dyeing and the secondary dyeing) were measured in the same manner as in Experimental Example 1 and are shown in Tables 14 to 19, respectively.

When CNF was included, it was found that the L value was lower than that of dyed alone. Especially, L value of 5 g of Gardenia extract dyeing + CNF B1 (Evaporation) was lowest after secondary staining. However, L value of Gardenia extract dyeing + CNF B5 5g and Gardenia extract dyeing + CNF O1 5g increased during secondary staining.

In the case of turbidity, the values of Gardenia extract dyeing + CNF B1 (Evaporation) 5g and Gardenia extract dyeing + CNF O1 5g were nearly doubled in the secondary staining. It is presumed that the dye fixed to the fiber during secondary dyeing came back during dyeing.

In the case of Gardenia extract dyeing + CNF O1 5g, sugar content decreased after 1st and 2nd staining. In the case of Gardenia extract dyeing + CNF B5 5g, sugar content increased after 1st and 2nd staining.

( Experimental Example  5)

The paleo-persimmon was used as the dyestuff. Eleven pieces of 25 × 25 cm (cm) puffy mud dogs were prepared, and 1% aqueous solution of Na ₂ CO ₃ and 0.5% aqueous solution of surfactant were heated at 100 ° C. for 60 minutes in a bath ratio of 1:50.

The powdered ginger powder and distilled water were prepared at 1:20, and when the temperature reached 90 ° C, the powder was added, mixed well for 20 minutes, and impurities were filtered out and stained. When 5 g of each of the 800 ml of the gardenia extract and the CNF were heated to about 100 ° C, they were heated for 30 minutes and 60 minutes, respectively. 5 g of each 800 ml of gardenia extract + CNF is heated at about 60 ° C for 30 or 60 minutes to be dyed. After 30 minutes of dyeing, 30 minutes of dyeing, 60 minutes of dyeing and 90 minutes of dyeing were recorded. The color values of the saline solution after 30 minutes of dyeing, 60 minutes of dyeing and 90 minutes of dyeing were recorded, Table 24 (fabric, 100 占 폚 staining) and Table 25 (woven fabric, 100 占 폚 staining), Table 21 (stain, 60 占 폚 staining) 60 ° C).

After 30 minutes dyeing, sugar content decreased except B5, but turbidity increased. After 60 minutes dyeing, turbidity decreased except B1, and sugar content increased in common. After 90 min dyeing, turbidity was mostly reduced, but B5 was still higher than before dyeing. In B1 and O1, turbidity decreased and sugar content increased. In the case of O1, sugar content was the highest. When dyeing the gardenia extract, the turbidity decreased in common, but the sugar content increased. It is presumed that the components of the fabric or CNF are in the saline solution.

When dyeing at 60 ° C, the sugar content and turbidity of B1 are all reduced, and dyeing is expected to be successful. However, as opposed to dyeing at 100 ° C, the turbidity of all samples was reduced.

In the case of the color of the saline solution, when the value of b is high, O1 was the most yellowish dye after 30 minutes dyeing, and O1 was the most saline color after 60 minutes. However, b value decreased after 90 min staining. This was expected to increase the b value of the fabric. After 90 minutes dyeing, B5 was the most saline solution and b value was high. In the case of gardenia extract alone, the color was the strongest, the lowest value a, and the yellow color was very high. When we put the CNF, it was confirmed that the color becomes closer to red.

The color of the salt solution was different from that of the fabric. After 30 minutes, the color of b1 was the strongest and the red-yellow value was also high. After 60 minutes, all of the saline had high a, b value and high L value, and the color was bright and bright.

Compared with the gardenia extract alone, the b value was not improved after 30 minutes when CNF was added together, but after 90 minutes, the a and b values increased by 3 and the red-yellow color appeared, but the difference was insignificant .

The difference in dyeability after 30 minutes and after 90 minutes was not large overall. Therefore, it is considered that dyeing for 30 minutes is more efficient than dyeing for 90 minutes. Specifically, after 90 min staining, b value increased by 2 ~ 4, but there was no difference between L value and a value.

The most probable dye was B5, and it was confirmed that dyeing 5g of B5 for 30 minutes is most appropriate.

The difference of b value is not great, but after 30 minutes, the color value of O1 was the best. After 60 minutes, the b value was improved in common and the dyeability of O1 was the best. At 60 ℃ than 100 ℃, dyeability was better and O1 was found to be most suitable for 30 minutes.

( Experimental Example  6)

For further experiments, cotton, hemp, rayon, hair and silk were used as the dyes. Specific specifications of each fiber are shown in Table 26.

The refining method for each fiber was carried out by using 5% NaOH for 30 minutes at 100 ° C. The reaction was carried out at 100 ° C for 30 minutes using 5% NaOH. The rayon was made with 5% NaOH at 70 캜 for 30 minutes. 0.04% of a neutral detergent was used and dried at 60 DEG C for 20 minutes. The silk was heated in water at 30 ° C for 10 minutes, and then soaked in Na ₂ CO ₃ at 90 ° C for 15 minutes. Ten grams of CNF was added to 800 ml of the prepared gardenia extract, and the mixture was stained at 80 ° C for 60 minutes. When CNF was not added, dyeing was carried out at 80 캜 for 60 minutes without CNF. After dyeing, washing was carried out at 30 캜 until no more color appeared with distilled water, and naturally dried for about one day. The Lab, turbidity and sugar content of each dyed fabric were measured in the same manner as in Experimental Example 1 and shown in FIG. 2 and Table 27 and Table 28, respectively.

As shown in Figs. 2 and 27 and Table 28, when CNF was added, the sugar content of cotton and rayon in the vegetable fiber was increased and the sugar content of the rice was decreased. The sugar content of animal fibers increased but the sugar content of silk decreased. Also, when CNF was added, the turbidity of cotton in the vegetable fiber decreased, but turbidity of hemp and rayon increased. The turbidity of the silk in the animal fibers decreased but the turbidity of the silk increased. Also, when CNF was added, the L *, a * and b * values of both parent and silk increased.

(Experimental Example 7)

Additional experiments were performed to determine the dyeability of the cellulosic suspension (3%) (CNF H). 3% cellulosic suspension and gardenia extract were stained. Specific specifications of the fabrics used are shown in Table 29 below.

First, refine the view. Specifically, when the temperature exceeds 90 ° C , an aqueous 1% sodium carbonate solution and a 0.5% aqueous solution of a surfactant (Tween 80) are mixed at a bath ratio of 1:50 and mixed well. When the temperature reached 100 占 폚, cut slices were put in and then heated to maintain the temperature for 60 minutes. After 60 minutes, the refined artificial leaves were washed in running water for 10 minutes or more for 10 minutes to remove the residue. The washed dogs were dried in a desiccator preheated to 60 ° C for about 10 minutes.

Then, a gardenia extract was obtained from the gardenia powder. Specifically, the distilled water and the germanium powder were prepared at 1:20, and the distilled water was heated. When the temperature of the distilled water reached 90 ° C, the germanium powder was placed in the heated distilled water, stirred for 20 minutes, and heated to maintain the temperature . After 20 minutes, it was filtered out more than 3 times using a sieve to remove impurities as much as possible.

As the first staining method, when the temperature of 800 ml of the gardenia extract (Liquid 1:80) reached 80 ° C, 5 g of CNF H was added, and the eyes were stained for 60 minutes. After dyeing, the water was washed with running water until the salt solution did not come out for about 15 minutes, and dried in a desiccator preheated to 60 ° C.

As a second staining method, 800 ml of CNF H (Liquid 1:80) was sprinkled with a powder of gardenia powder, and when the temperature reached 80 ° C, the pups were stained for 60 minutes. After dyeing, the water was washed with running water until the salt solution did not come out for about 15 minutes, and dried in a desiccator preheated to 60 ° C. This process was repeated three times to obtain respective stained strains

As the third staining method (staining with the remaining salt solution), the second staining method was carried out and stained with the remaining CNF H salt solution. The collected CNF H salt solution was divided into 700 mL portions, and 700 mL of CNF H salt solution was added at 80 ° C., and the mixture was stained for 60 minutes. After dyeing, the water was washed with running water until the salt solution did not come out for about 15 minutes, and dried in a desiccator preheated to 60 ° C. This process was repeated three times to obtain each stained image.

In addition, in order to compare the dyeability obtained by the above-described dyeing method with that obtained by the above-mentioned dyeing method, except for putting CNF H in the first dyeing method, the rest of the flowers were dyed alone as a control (control) Respectively.

Using a colorimeter (KONICA MINOLTA, Color Reader, CR-10, Japan), a sugar meter (ATAGO, REFRACTOMETER, PAL-1, Taiwan) and a turbidimeter (TURBIDITY METER, TU-2016, Japan) , Lab, turbidity and sugar content were measured and shown in Tables 30 to 32, respectively.

As shown in Table 30, when 5 g of CNF H was compared with the result of the only dyeing of the gardenia, the L value slightly increased and the b value slightly decreased in the case of staining using 5 g CNF H.

As shown in Table 31, when the CNF itself was used for staining, there was no significant difference in the L value of the dyed artifacts, but the value b was slightly increased.

As shown in Table 32, when dyeing was repeated three times in the remaining salt solution after the dyeing experiment, the color value was not significantly different from 800 mL. L value and b value tended to be slightly increased due to the residual dye after dyeing, and b value was slightly increased or similar to control.

(Experimental Example 8)

In addition, the same method as the first staining method of Experimental Example 7 was repeated three times to perform staining. Six wash samples obtained through the repeated processes were subjected to the washing process three times, and the wash fastness, the fastness to washing, the fastness to perspiration and the antibacterial property were measured and the results are shown in Table 33 below.

number Condition Wash fastness
KSK ISO 105-C06: 2014
A1S method Light fastness
KS K ISO 105-B02: 2014
Xenon arc method Sweat fastness
KS K ISO 105-E04: 2013
Perth pyrometry Antimicrobial activity
KS K 0693: 2011
2 test species One CNF H 3 repetition same experiment / 2 / / 2 CNF H 3 repetition same experiment / 2 / / 3 CNF H 3 repetition same experiment / 1-2 / / 4 CNF H 3 Repeat The same experiment (cotton) / 1-2 / / 5 CNF H 3 Repeat The same experiment (cotton) / 1-2 / / 6 CNF H 3 Repeat The same experiment (cotton) / 1-2 / /

(Experimental Example 9) Additional experiments were carried out in order to confirm the dyeability of the human eye according to temperature and time using cellulose diluted to various concentrations. Specific specifications of the fabrics used are shown in Table 34 below.

For each sample, 1% aqueous solution of sodium carbonate and 0.5% aqueous solution of surfactant (Tween 80) were added at a bath ratio of 1:50, and the mixture was stirred well. When the temperature reached 100 ° C , the cut slices were added and heated to maintain the temperature for 60 minutes. After 60 minutes, the refined artificial leaves were washed with flowing water for 10 or more times for 10 minutes to remove the residue. The washed dogs were dried in a desiccator preheated to 60 ° C for about 10 minutes.

To extract the gardenia extract from the gardenia powder, distilled water and gardenia powder were first prepared at 1:20. When distilled water is heated and the temperature of the distilled water reaches 90 ° C. The germanium powder was placed in distilled water, stirred for 20 minutes, and heated to maintain the temperature. After 20 minutes, it was filtered out more than 3 times to remove impurities as much as possible.

When the temperature of 800 ml of the gardenia extract (liquid 1:80) reached 60 ° C , 5 g of each CNF 3 was added, and the mixture was dyed for 30, 60 and 90 minutes. When the temperature of 800 ml of the gardenia extract (Liquid 1:80) reached 80 ° C , 5 g of each of CNF 3 was added, and the mixture was dyed for 30, 60 and 90 minutes. When the temperature of 800 ml of the gardenia extract (Liquid 1:80) reached 100 ° C , 5 g of each CNF was added, and the mixture was dyed for 30, 60 and 90 minutes.

Each sample was dyed and then washed with running water until the salt solution did not come out for 15 minutes and dried in a desiccator preheated to 60 ° C.

In order to compare the dyeability obtained by the above-mentioned dyeing method with that of the human eye, the remaining portion was dyed with the gardenia extract alone in the same manner and used as a control.

L, a, b, C, and h were measured under D65-10 light source using CCM (Computer Color Matching, Macbeth, Color - Eye 3100, USA) Also, the K / S value is the highest K / S value within the range of 400-700 nm. Specifically, the colorimetric apparatus itself was initialized by inserting a white tile into the apparatus described above, and the sample was folded twice and then the colorimetric sections were measured five times in total. After storing the measured data 5 times, necessary data such as color value and K / S value were calculated from the colorimetric data in the program, and the values are shown in Tables 35 to 37, respectively.

As shown in Table 35, the color of fabric (L value decrease, b value increase, K / S value increase) became darker in 60 minutes when CNF was put in the salt color except for the gardener alone. The color of the salt solution was also lightened when CNF was added, indicating that the dye was adhered to the fabric. In the case of the gardenia dyed alone, the dyed color was the most intense for 90 minutes. However, it was confirmed that when the CNF was added, the color was thickened for 60 minutes and the time could be shortened by simultaneous mordanting of CNF.

As shown in Table 36, at 80 占 폚, no tendency similar to 100 占 폚 was observed. The value of b was increased with longer time in the case of gardenia alone but it was the best dyeing in 60 minutes when K / S value was centered. The highest K / S value was observed at 80 ℃ in the case of gardenia dyeing alone, but the color value was higher and darker at 100 ℃ when K / S value was lower than 80 ℃. When the CNF is inserted, the K / S value decreases as a whole. In the case of the b value, the b value slightly increases except for o1.

As shown in Table 37, there was no clear tendency at 60 ° C. At 60 ℃, the L value decreased, the b value increased, the K / S value increased and the dyeability was good at 90 minutes except for B5 even when CNF was added. The b value and K / S value were higher at 100 ℃ than at 100 ℃ regardless of the input of CNF. Therefore, the color itself shows the deepest color at 60 ° C, but time does not decrease and an exception is made in B5.

From these results, it is more preferable to dye for 60 to 90 minutes, and it is more preferable to dye at 50 to 110 ° C.

Various experiments were conducted through the above-described various experimental examples. As a result, it was confirmed that CNF could be fully utilized as a natural mordant, though the results were somewhat different according to experimental conditions.

It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit and scope of the present invention as defined by the following claims It can be understood that it is possible.

Claims (13)

Preparing a dyestuff;
Refining the dyestuff;
Dyeing the refined dyed material with a mixture of a cellulose nanofiber suspension and a gardenia extract;
Washing the dyed dyed material; And
Drying the washed soil to be washed,
The mixture is dyed with a natural mordant and a gardenia extract in which a mixture of a gardenia extract and a cellulose nanofiber suspension is mixed at a weight ratio of 1:10 to 30. The method according to claim 1, wherein the dyestuff is dyed with a natural mordant and a gardenia extract, either cotton, hemp, rayon, hair or silk. The method according to claim 1, wherein the cellulose nanofiber suspension is dyed with a natural mordant and a gardenia extract containing 0.5 to 3.5% by weight of a cellulose nanofiber. The method according to claim 1, wherein the cellulose nanofibers are mixed with a natural mordant and a gardenia extract, wherein the crocin of the gardenia extract is chemically bonded. Preparing a dyestuff;
Refining the dyestuff;
Cellulose nanofibers and a gardenia extract in a weight ratio of 1: 5 to 100, dyes the refined dyes at 50 to 110 DEG C for 20 to 100 minutes;
Washing the dyed dyed material; And
Drying the washed soil to be washed,
Wherein said dyeing step is a step of staining with natural mordants and a gardenia extract wherein the dyeing time is reduced when the dyeing temperature is increased. 6. The method of claim 5, wherein the staining is performed with a natural mordant and a gardenia extract wherein the staining is performed at 100 DEG C for 30 minutes. 6. The method according to claim 5, wherein the staining is performed with a natural mordant and a gardenia extract wherein the staining is carried out at 60 DEG C for 90 minutes. 6. The method according to claim 5, wherein the method further comprises dyeing the dried artichoke extract with a gardenia extract alone. As a natural mordant for cellulose nanofibers,
Wherein the natural mordanting agent is used in a mixture of 0.5 to 3.5% by weight of cellulose nanofibers and the balance water. The natural mordanting agent according to claim 9, wherein the cellulose nanofibers are contained in an amount of 0.5 to 1.5% by weight. As a dyed dyed with gardenia extract,
Dyed dyed with a mixture of a suspension of cellulose nanofibers of 0.5 to 3.5% by weight and a gardenia extract, which is a natural mordant. 12. The dyestuff according to claim 11, wherein the dyestuff is any one of cotton, hemp, rayon, wool, and silk. 12. The dyestuff according to claim 11, wherein the mixture is a mixture of a gardenia extract and a cellulose nanofiber suspension in a weight ratio of 1:10 to 30.

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