KR20140022604A - Pretreatment method of dyeing of textile materials and dyeing method of textile materials - Google Patents

Abstract

The present invention relates to a dyeing pretreatment method for textile materials and a dyeing method for textile materials using the same, and more specifically, to the invention which increases the persistence of the antimicrobial and antioxidative properties of textile materials by dyeing by improving dyeing fastness by pretreating the textile materials before dyeing the textile materials using lithospermum officinale root extracts. The present invention can provide environmentally friendly products such as diapers and the like.

Description

Pretreatment method of dyeing of textile materials and dyeing method of textile materials}

The present invention relates to a coating material dyeing pretreatment method and a coating material dyeing method using the same, and relates to a dyeing pretreatment method and a dyeing method using the same, which can sustain a dyeing effect of a natural dye.

With the development of technology, traditional dyeing has gradually disappeared with the introduction of chemical dyes instead of conventional dyes. However, in recent years, the public's interest in eco-friendly and eco-friendly products has increased, and pollution-free dyeing processes are comfortable and soft. There is a growing interest in natural dyeing, which can be colored.

Natural dyeing, which has remained at the level of craftsmanship, has recently been applied to various dyeing of various fibers. However, in spite of the advantages of natural dyes, they are not industrialized and practically used due to the low extraction yield. These dyes are expensive compared to synthetic dyes, and the salt instability, complexity of dyeing method, low reproducibility of color and This is why the scientific approach was not made depending on the dyeing method.

Gallnut (Gallnut, Gallapfel) The worm family is caused by the damage to the Rhododendron belonging to the lactose family. The gallant aphids parasitic on red branches or leaves, leaving a hairy tawny or tan-brown pouch-shaped beetle, which usually can be dried for about a week in late September before the gallant aphids penetrate the beetle. The main components of the gall bladder is tannin (50-70%), some glutinous assets, fats, resins, etc. The main component is galallotannin. The gall is mainly produced in Southeast Asia, such as China, Korea, and Japan, and is also used as a major raw material for industry, medicine, and medicine.

Lithospermum erythorhizon , gromwell, root) have been used as a natural wound healing agent for a long time, and shikonin, the main component of the colorant, has been reported to be antimicrobial, anti-inflammatory and anticancer. . In addition, although the dyeing roots have been used by dyeing cloth as a natural purple or red dye, the products dyed with the dyeing roots have a problem of greatly degrading their merchandise because they are discolored by washing.

Accordingly, the present inventors intend to provide a coating material dye pretreatment method and a dyeing method using the same, which can improve dyeing stability of a product dyed with branch root extract.

The present invention for solving the above problem relates to a coating material dyeing pretreatment method,

Modifying the surface of the coating material with a modifier comprising one or both sides of the coating material with a cationic agent; Neutralizing and drying the reformed coating material; And mordenting the dried coating material with a mordant containing a gall bladder extract.

And, the modifier is characterized in that it comprises 0.05 to 0.2% by weight of the cationic agent in the total weight of the modifier.

In addition, in the dye pretreatment method of the present invention, the step of reforming is characterized in that the reforming is carried out by a pad batch (PB) method.

In addition, the PB method is characterized in that performed under 100% wet pickup (wet pickup).

In addition, the cationic agent is characterized in that represented by the formula (1).

In Formula 1, R ¹ to R ³ are independent of each other, and are a hydrogen atom, a methyl group, or an ethyl group, and R ⁴ is a C1 to C5 straight or crushed alkyl group.

In addition, the mordant includes 5 to 15% by weight of the gall bladder extract in the total weight of the mordant, characterized in that the pH 3-4.

Another aspect of the invention relates to a method of dyeing a coating material,

Modifying the surface of the coating material with a modifier comprising one or both sides of the coating material with a cationic agent; Neutralizing and drying the reformed coating material; Mordanting the dried coating material with a mordant containing a gall bladder extract; And dyeing the coated material which has been treated with mordant with a dye including the root extract of borage.

Here, the dyeing agent contains 1 ~ 20% by weight of the root extract and 80 ~ 99% by weight of ethanol, characterized in that the pH 6.5 ~ 7.5.

In addition, the coating material dyeing method of the present invention is characterized in that it can be repeated 1 to 5 times the dyeing step.

In the coating material dyeing pretreatment method and dyeing method of the present invention, the coating material is at least one natural coating material selected from cotton, wool and silk, the natural coating material is characterized in that the fiber, yarn, fabric or knitted fabric. .

Another aspect of the present invention is an environmentally friendly product, characterized in that it comprises a coating material dyed by the dyeing method, the eco-friendly product is characterized in that at least one selected from diapers, sanitary napkins, underwear and bedding.

After performing the dyeing pretreatment method proposed by the present invention, the coating material dyed with the branch root extract is very excellent in colorfastness, and the coating material dyed by the method of the present invention is antimicrobial and antioxidant This excellent and sustainable bar can produce eco-friendly products with high marketability.

1 is a UV-Vis absorbance measurement results of the dyeing agents carried out in Experimental Example 1.
2 is a GC-MS measurement result of the dyeing agent carried out in Experimental Example 1.
The graph and photograph of FIG. 3 are the results of the CIELAB color difference measurement experiment conducted in Experimental Example 1, wherein (a) pure cotton fabric, (b) cotton fabric prepared in Comparative Example 5, and (c) cotton fabric prepared in Comparative Example 3 The scanned picture.
The graph and photograph of FIG. 4 are the results of the CIELAB color difference measurement experiment conducted in Experimental Example 1, and (a) pure cotton fabric, (b) cotton fabric prepared in Comparative Example 4, and (c) color of cotton fabric prepared in Example 1. The scanned picture.
FIG. 5 is a FTIR-ATR spectra measurement result obtained in Experimental Example 2, wherein (a) is pure cotton fabric, (b) is Comparative Example 1, (c) is Comparative Example 4, and (d) is Comparative Example 3 and ( e) is the spectra measurement result of the cotton fabric prepared in Example 1.
6 is a surface characteristic test result of the cotton fabric carried out in Experimental Example 3, (a) is a pure cotton fabric, (b) is a cotton fabric prepared in Comparative Example 4, (c) is a cotton fabric prepared in Comparative Example 2 (D) is a SEM measurement photograph of the cotton fabric prepared in Comparative Example 6.
7 is an antioxidant measurement test result carried out in Experimental Example 5, (a) is a cotton fabric prepared in Comparative Example 1, (b) is a cotton fabric prepared in Comparative Example 2, (c) is prepared in Comparative Example 7 (D) is the antimicrobial measurement test results of the cotton fabric prepared in Example 3.

The present invention relates to a dyeing pretreatment method and a dyeing method which can greatly improve the color fastness (dyeing durability) of the coating material dyed with branch root extract, and the present invention will be described in more detail below.

Dyeing pretreatment method of the present invention

Modifying the surface of the coating material with a modifier comprising one or both sides of the coating material with a cationic agent; Neutralizing and drying the reformed coating material; And mordenting the dried coating material with a mordant containing a gall bladder extract.

Here, the modifier is characterized in that it comprises 0.05 to 0.2% by weight of the cationic agent, preferably 0.1 to 0.15% by weight of the cationic agent, specifically 0.05 to 0.2% by weight of the cationic agent and 99.8 to distilled water 99.95% by weight, and may further include a very small amount of impurities. Here, if the cationic agent is less than 0.05% by weight, it may not be possible to see a sufficient modification effect, even when used in excess of 0.2% by weight, there is almost no increase in modification effect according to the increase in use, it is preferable to use within the above range. . In addition, the cationic agent may be represented by the following formula (1), in the following formula 1, R ¹ ~ R ³ are independent of each other, a hydrogen atom, a methyl group or an ethyl group, R ⁴ is a straight line of C1 ~ C5 Chain or crushed alkyl group.

[Formula 1]

In addition, the cationic agent is preferably R ¹ , R ² and R ³ is a methyl group, R ⁴ is an ethyl group or a propyl group, more preferably R ¹ , R ² and R ³ is a methyl group, R ⁴ is It is good to be a profile machine.

In the dyeing pretreatment method of the present invention, the reforming step may use a general method used in the art and is not particularly limited, it is preferable to perform the modification by a pad batch (PB) method, wherein the PB The process is preferably performed under 100% wet pickup.

In the neutralizing and drying step, the neutralizing method may be used a general method used in the art, but is not particularly limited, it is preferable to use an aqueous sodium hydroxide solution as a neutralizing agent. In addition, a drying method may also use a general method used in the art, but is not particularly limited, it is good to dry slowly at a temperature of about 40 ~ 70 ℃.

In the step of mordant, the mordant comprises 5 to 15% by weight of the gall bladder extract, preferably 7 to 11% by weight of gall bladder extract in the total weight of the mordant, specifically 5 to 15% by weight gall bladder extract and It may include 85 to 95% by weight of water, and may further contain a trace amount of impurities. Here, if the gall extract is less than 5% by weight morbidity effect is reduced, even when used in excess of 15% by weight is almost uneconomical bar increase effect. And the mordant is pH 3 ~ 4, preferably pH 3.5 ~ 3.7 in order to maximize the mordant treatment effect.

Another aspect of the present invention, the coating material dyeing method

Modifying the surface of the coating material with a modifier comprising one or both sides of the coating material with a cationic agent; Neutralizing and drying the reformed coating material; Mordanting the dried coating material with a mordant containing a gall bladder extract; And dyeing the coated material which has been treated with mordant with a dye including the root extract of borage.

In the coating material dyeing method, the method of reforming, neutralizing and drying, and mordant, and the type and characteristic of the material used in each step are the same as the pretreatment described above.

The dyeing agent may include 1 to 20% by weight of Chichi root extract and 80 to 99% by weight of ethanol, and preferably 4 to 10% by weight of Chichi root extract and 90 to 96% by weight of ethanol. Here, if the boric root extract is less than 1% by weight, the dyeing is too blurry, and even if it is used in excess of 20% by weight, there is almost no dye enhancement effect. And, the dyeing agent is pH 6.5 ~ 7.5, preferably pH 6.7 ~ 7.0.

In addition, in the method for dyeing the coating material of the present invention, repeating the dyeing step 1 to 5 times, preferably 1 to 2 times, is preferable in terms of increasing durability and improving color.

In the above-described coating material dyeing pretreatment method and dyeing method of the present invention, the coating material is at least one natural coating material selected from cotton, wool and silk, the natural coating material is preferably fiber, yarn, fabric or knitted fabric. Preferably, it is cotton fiber and cotton fabric.

As described above, the coating material dyed by the method proposed by the present invention is very suitable for use as an environmentally friendly product, since the branched root extract, which is a dyeing ingredient, has excellent antimicrobial and antioxidant effects, and in particular, as an environmentally friendly product, diapers, sanitary napkins, underwear And very good for use in bedding and the like.

[ Example ]

Preparation Example

(1) Preparation of Dye

100 g of dried roots were dried, pulverized and pulverized, and then the powders were immersed in 1 L of ethanol and left in a shade at 25 ° C. for 2 hours to obtain an extract from the roots of the branched roots. Repeat more times. After the extraction was completed, filtration was carried out to remove insoluble residues from the extract, finally producing a dyeing agent containing the borage root extract. The dyeing agent was prepared containing the root extract of 9% concentration and pH was 6.8.

(2) Preparation of mordant

After drying gall of 100 g, pulverized and powdered, and then put the powder in 1L of distilled water, and boiled for 1 hour. Next, after cooling, filtration was performed to remove the insoluble residue, thereby finally preparing a mordant including a gall bladder extract. The prepared mordant had a concentration of about 5% and a pH of 3.6.

(3) Modifier  Produce

3 g of N- (chloride (3-chloro-2-hydroxypropyl) trimethylammonium chloride) (Dow cornoing, MI, US) as a cationic agent was added to 1 L of water, followed by stirring and dissolving to obtain 0.13% by weight of cationic agent. A modifier comprising was prepared.

Example  One

(One) Reforming process

Cotton fabrics (100% cotton, 52 × 24 cm 2) were modified with a modifier prepared in Preparation Example in a pad-batch process with 100% wet pickup. The modified cotton fabric was then placed in a sealed bag and left at 25 ° C. for 20 hours.

Next, the cotton fabric was taken out, washed sufficiently with distilled water, and then neutralized by adding and stirring the cotton fabric in an aqueous solution of sodium hydroxide at a concentration of about 0.1%.

Next, the cotton fabric was dried in a rotary dryer (60 ° C.) to prepare a modified cotton fabric.

(2) burying process

The modified cotton fabric was prepared using a mordant prepared in Preparation Example using a Lab IR dyeing machine (Lab IR dyeing machine, Manufacturer: Mathis Labomat, trade name: Becatron AG, Swizerland; bath ratio = 1: 20). It was made to be immortalized.

Here, the embedding process was finally carried out at 80 ℃ by raising the bath (bath) temperature by 3 ℃ per minute, the stirring was carried out at a stirring speed of 25 rpm for 30 minutes at this temperature.

Next, after cooling to 30 ° C., the cotton fabric was taken out, dehydrated, washed and dried to prepare a modified and printed cotton fabric.

(3) dyeing process

The modified and immobilized cotton fabrics were prepared using a dye prepared in Preparation Example, and the modified and immobilized cotton fabrics were prepared using a Lab IR dyeing machine (Lab IR dyeing machine, manufacturer: Mathis Labomat, trade name: Becatron AG, Swizerland; (bath ratio) = 1: 20).

Here, the dyeing process was finally carried out at 40 ℃ by raising the temperature of the bath by 3 ℃ per minute, at this temperature was stirred at a stirring speed of 25 rpm for 1 hour (1 cycle).

Next, after cooling the temperature to 30 ℃, the cotton fabric was taken out, dehydrated, washed and dried to prepare a cotton fabric dyed with branch root extract.

Example  2 to 3

In the same manner as in Example 1 to prepare a cotton fabric dyed with Chichi root extract, Example 2 was carried out by repeating the dyeing process 2 cycles to prepare a cotton fabric dyed with Chichi root extract.

In addition, Example 3 was carried out by repeating three cycles of the dyeing process in the same manner to prepare a cotton fabric dyed with Chichi root extract.

Comparative Example  1 to 7

Comparative Example 1 was modified in the same manner as in Example 1 to the pure cotton fabric used in Example 1 to prepare a modified cotton fabric.

In Comparative Example 2, a dyed cotton fabric was manufactured by performing a dyeing process (1 cycle) in the same manner as in Example 1 without performing a modification and embedding process.

In Comparative Example 3, a dyed cotton fabric was manufactured by performing a reforming process and a dyeing process (1 cycle) in the same manner as in Example 1 without performing a mortaring process.

Comparative Example 4 was not carried out the reforming process and dyeing process, was carried out in the same manner as in Example 1 only to produce a cotton-treated cotton fabric.

In Comparative Example 5, only the dyeing process was performed on the pure cotton fabric in the same manner as in Example 1 to prepare dyed cotton fabric.

In Comparative Example 6, a dyed cotton fabric was prepared by performing a mortar and dyeing process without a reforming process on the pure cotton fabric in the same manner as in Example 1.

Comparative Example 7 was a dyeing cotton fabric was prepared by performing a reforming process and dyeing process (3 cycles) in the same manner as in Example 2, without performing a mordant process, Comparative Examples 1 to 6 summarized in Table 1 and same.

division Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Comparative Example 5 Comparative Example 6 Comparative Example 7 Reforming process ○ × ○ × × × ○ Burying process × × × ○ × ○ × Dyeing process × ○
(1 cycle) ○
(1 cycle) × ○
(1 cycle) ○
(1 cycle) ○
(3 cycles)

Experimental Example  1: Measurement of Properties of Dyeing Agent

(1) absorbance measurement experiment

UV-Vis absorbance was performed at 200-800 nm wavelength using a Hitachi U-2000 spectrophotometer (Lambda 950, MA, US). Indicated.

Figure 1 (a) is a dye solution prepared in Preparation Example, (b) is a photograph of a solution diluted 35% of the dye solution prepared in Preparation Example. Referring to the graph of FIG. 1, 520 nm (Chu and Soh 2001; Park et al. 2009), which is a characteristic absorption peak (λ _max ) of shikonin, appears, indicating that the siconin-based material is included in the dye. You can check it.

In addition, the visible light transmittance was shown at 560 ~ 800nm and 380 ~ 489nm, the color was identified as magenta caused by the blue and red wavelengths stronger than the yellow-green wavelength.

(2) GC - MS ( gas chromatograph - Mass spectrohpotometry ) And high performance liquid chromatography ( HPLC Measurement experiment

The dye prepared in Preparation Example was subjected to GC-MS measurement, and qualitative analysis was also performed using a high performance liquid chromatography-Diode Array Detector (HLPC-DAD, trade name: Agilent Technologies 5975C inert XL EI / CI MSD). Here, the HLPC-DAD is equipped with a Hitachi model L-700 pump, a triple-axis detector and a column (250 × 4.6 mm id, 5 μm, trade name: Thermothermoquest C18 HYPURITY). The mobile phase was mixed with acetonitrile and an acetic aqueous solution of pH 2.56 in a 1: 1 volume ratio, and the flow rate was 1.0 mL / _min . And the effluent from the column was monitored at 280 nm.

The result of measuring the dye extract containing the branched root extract prepared in Preparation Example (1) by GC-MS is shown in Figure 2, and looking at the graph, the main peak of deoxysiconin was observed in about 13.27 minutes. However, this peak was reduced by 16.67% after dyeing the cotton fabric, which indicates that the active deoxysiconin was transferred to the cotton fabric by dyeing, that is, the GC-MS value of the dye before dyeing and the remaining dye after dyeing. As a result of the difference in GC-MS values, it was confirmed that the deoxysiconin peak in the remaining dye was reduced by moving the deoxysiconin main component to the cotton fabric by dyeing.

In addition, the results of the mass spectrometry are shown in a box in the graph of FIG. 2, whereby the main component of the dye is deoxyshikonin represented by the following Chemical Formula 2, which is one of sikonin / alkannins. You can see that.

(3) CIELAB ( Lab color space ) Color difference  Measurement experiment

Using a spectrophotometer (Minolta spectrophotometer (Osaka, Japan)), CIELAB color difference measurement experiments were performed using the cotton fabric prepared in Comparative Examples 3 to 5 and Examples 1 to 3, the results are shown in Figures 3 and 4 Indicated. Here, Figure 3 is for confirming the effect of the reforming treatment, Figure 4 is a color difference measurement experiment for confirming the effect of the mordant treatment, L ^* is the brightness (Luminosity) value, a ^* is a red / green complementary color axis, b ^* is the yellow / blue complementary axis.

3 is a color difference measurement result of the cotton fabric prepared in Comparative Example 3 (1 cycle) and dyed 2 to 3 cycles, and the graph values in FIG. 4 are Examples 1 to 3 (dyeing treatment respectively). Color difference measurement result of the cotton fabric prepared in 1 to 3 cycles).

Since the branched root extract is magenta and has a maximum absorbance at 520 nm, cotton fabrics stained with the branched root extract are generally bluish and reddish. In addition, as the dyeing cycle increases, red, blue, and black may be increased through the graph of FIG. 3. Looking at the graph of FIG. 3, even if the dyeing process is additionally L ^* , a ^* , It can be seen that there is no significant change in the b ^* value. Through this, in the past, when the cotton fabric was dyed with a natural dye, the dyeing process was performed several times, but the process of dyeing the cotton fabric can be minimized. It can be confirmed. In addition, these results can also be confirmed through the graph of FIG. 4.

And, comparing the graphs of Figures 3 and 4, b ^* (yellow / blue complementary color axis) shows a large difference in the value, which is due to the effect of the mordant with a mordant (five pear extract).

The photograph of FIG. 3 shows (a) a pure cotton fabric, (b) a cotton fabric prepared in Comparative Example 5, and (c) a cotton fabric prepared in Comparative Example 3. As a result of the CIELAB color difference measurement experiment, it was confirmed that the dye (c) after the reforming treatment was a blue color system, and (b) only the dyeing treatment was a red system. In addition, it was confirmed that the staining effect of the root extract of Chichi can be enhanced. It is believed that this effect is due to the fact that deoxysiconin, which contains many hydroxyl groups, binds to the ion linkage of the modified cotton fabric.

In addition, the photograph of FIG. 4 shows (a) a pure cotton fabric, (b) a cotton fabric prepared in Comparative Example 4, and (c) a cotton fabric prepared in Example 1. CIELAB color difference measurement results show that the mortar treatment offsets the red color of the dye containing root extract and the cotton fabric adds a yellowish tint. In addition, it can be seen from the graph of FIG. 4 that the staining effect of the root extract is influenced by being maintained without falling off during the dyeing process by the root extract after the mortar treatment by the gall bladder.

Experimental Example  2: of cotton fabric FTIR - ATR  Spectroscopic measurement experiment

FTIR-ATR spectra of cotton fabrics were measured, and the method of measurement was attenuated total reflectance (ATR) at a resolution of 4 cm ^{-1 on} a Nicolet 6700 FTIR (trade name: Thermo electron, WI, US) equipment. Fourier transform infrared spectroscopy (FTIR) was collected using the method and the results are shown in FIG. 5.

In the graph of Figure 5 (a) is pure cotton fabric, (b) is Comparative Example 1, (c) Comparative Example 4 ,, (d) Comparative Example 3 and (e) is a cotton fabric prepared in Example 1 Spectroscopic measurement results.

Referring to Figure 5, all cotton fabrics exhibit a bending vibration 1,317 cm ^-1 band of hydrocarbon structure, and also 1,370 cm ^-1 band and 1,430 cm ^- associated with symmetrical stretching of carboxylates derived from cellulose compounds. ¹ band was shown.

It is determined that the characteristic peak of deoxysiconin having a peak around 1630 cm ⁻¹ due to the quinine structure overlaps with the characteristic peak of the cellulose compound around 1635 cm ⁻¹ . The characteristic peak is related to the -OH band of water absorbed by the cellulose molecules of cotton fabrics stained with branch root extracts ((d), (e) of FIG. 5). That is, IR spectrum of the dye only staining agent comprising a root extract cotton is exhausted eopeotneunde the IR spectrum and the difference of the pure cotton fabric, which the main peak of the quinone structure which can be characterized by a peak of a non Francisco appears at 1,630 cm ^-1 This seems to be indistinguishable because it overlaps with the base peak of cotton fibers.

After the mordant, while the treatment, a hydroxyl group peak of 1,635 ㎝ ^-1 around the cellulose is, two peaks respectively divided in 1,710 ㎝ ^-1 and 1,615 ㎝ ^-1 in two peaks ((e) of FIG. 5 (c),) Each may be due to vibration of the carbonyl group double bond (C = O) and the aromatic group double bond (C = C) of gallic acid.

Thus, as the main component of the gall, gallotannin, a hydrolyzable tannin, is easily hydrolyzed by gallic acid and glucose in weak acid.

And it is judged that gallic acid is absorbed well by a cotton fabric by esterification of the cellulose hydroxyl group of a cotton fabric, and the carbonyl group of gallic acid. However, the stretching peak of ester (CO) did not coincide with the FTIR spectrum, which is This is believed to be due to overlapping ether (COC) stretching peaks (1,000 to 1,300 cm ⁻¹ ).

Experimental Example  3: Experiment of Surface Shape Measurement of Cotton Fabric

Cotton fabric surface shape was observed by scanning electron microscope (Scanning electron microscope, Hitachi S-3000N, Tokyo, Japan) and the results are shown in Figure 6 (a) ~ (d).

The weight change of the cotton fabric (not modified) which was treated with pure cotton fabric in the same manner as in Example 1 was increased by 10.8%, which was due to the absorption of a part of the gall bladder extract into the cotton fabric by means of SEM. Is shown in Figure 6 (b).

In addition, the weight change of the cotton fabric (without modification and mordification) after the pure cotton fabric was dyed in the same manner as in Example 1 was reduced to -0.42% on average, which means that when the cotton fabric was dyed, the oil was changed by ethanol solvent. This is because the component material is melted, and when looking at (C) of FIG. 6, it can be seen that the fiber spacing becomes sparse and the fiber diameter is somewhat reduced.

However, looking at (d) of Figure 6 of the cotton fabric prepared in Example 1, it can be seen that the roughness of the fiber surface is very low compared to Figure 6 (b) and (c), which is modified Through treatment and mordant treatment, it was determined that the dyeing was improved in stability and durability.

Experimental Example  4: Antimicrobial Test of Dyed Cotton Fabrics

The measured antibacterial experiments according to the JIS L 1902 method test Fabrics antimicrobial, Aru Staphylococcus aureus (Staphylococcus aureus , ATCC 6538P, Gram-positive bacteria) and Klebsiella pneumonia , ATCC 4352, Gram negative group bacteria).

All experimental samples and controls in Table 2 below were inoculated with bacteria and then left under the same ambient condition (25 ° C.) for 8 hours. Next, each experimental sample and the control were put in a container containing 100 ml of distilled water (quenching solution), and shaken well so that the bacteria fell from the cotton fabric into distilled water.

division Cotton fabric types Control group Pure cotton fabric Sample Comparative Example 1 In the same manner as in Example 1 on a pure cotton fabric
Cotton fabrics only modified by cationic agents Comparative Example 2 Without performing the reforming and embedding process,
Cotton fabric prepared by performing the dyeing process (1 cycle) by the tooth in the same manner as in Example 1 Comparative Example 3 In the same manner as in Example 1 without performing a mordant
Reforming process through cationic agent and
Cotton fabric produced by dyeing process (1 cycle) Comparative Example 7 Without carrying out the burial process,
The reforming process through the cationic agent in the same manner as in Example 2 and
Cotton fabric produced by dyeing process (3 cycles) Example 2 Modification process through cationic agent in the same manner as in Example 1 and
After carrying out the burial process
Cotton fabric produced by dyeing process (1 cycle)

Next, take 0.1 ml of the bacterial suspension in the container, dilute it with 10 ¹ , 10 ² , and 10 ³ times with distilled water, respectively, take 100 µl of the diluted bacterial suspension from each diluted sample, and then agar plate it (agar). plate) and incubated for 18 hours at 37 ℃.

Next, the bacterial reduction rate was confirmed, and the reduction rate was calculated based on Equation 1 below, and the results are shown in Table 3 below.

[Equation 1

Bacteria Reduction (%) = (B-A) / B × 100

Here, each of A and B is the number of viable microbial cells per ml ⁻¹ after inoculating bacteria into the samples and controls of Table 1, and then culturing them.

division Staphylococcus aureus
Decrease (%) Klebzilla Newmonia
Decrease (%) Control group - - Comparative Example 1 83.0 24.6 Comparative Example 2 99.9 29.2 Comparative Example 3 99.8 98.9 Comparative Example 7 99.8 97.2 Example 2 > 99.9 > 99.9

Looking at the results of the experiment in Table 3, in the case of Comparative Example 2 it can be seen that the antimicrobial effect on the gram negative group bacteria Klebzilla pneumoniae is very low, which is the active ingredient of the original Chichiin or its derivatives are Gram-negative bacteria The results are consistent with the report that there is almost no effect, and these results can be seen in Comparative Example 3 that the results are somewhat compensated by the cationic agent treatment.

And, in the case of Comparative Example 3 and Comparative Example 7, although high antimicrobial properties were shown even if not carried out the mordant process, after performing the dyeing pretreatment method (modification and mortaring process) according to the present invention, the dyed cotton fabric (execution Lower antimicrobial effect than Example 2)

Experimental Example  5: Antioxidant Measurement of Dyed Cotton Fabrics

Antioxidant measurement experiments were performed by measuring the change in absorbance of DPPH solution using DPPH radicals (purchased from Aldrich, MO, US). DPPH is a well-known radical and free radical promoter for other radicals. (scavenger, trap). The method for measuring by DPPH radicals is 50 mg of cotton fabric (Comparative Example 1, Comparative Example 3, Comparative Example 7, Example 2, and control group of 50 mg in a container containing 20 ml of 0.0001 M DPPH / methanol solution). ) Were added and soaked, and then left in the dark for 1 hour, and then the change in absorbance was measured at 517 nm using a UV-vis spectrometer.

division Cotton fabric types Control group Pristine cotton Sample Comparative Example 1 In the same manner as in Example 1 on a pure cotton fabric
Cotton Fabrics Modified by Cationic Agents Comparative Example 3 Without carrying out the burial process,
Modification process by cationic agent in the same manner as in Example 1 and
Cotton fabric produced by dyeing process (1 cycle) Comparative Example 7 Without carrying out the burial process,
Modification process by cationic agent in the same manner as in Example 2 and
Cotton fabric produced by dyeing process (3 cycles) Example 2 Through cationic agent in the same manner as in Example 1
After reforming process and burial process
Cotton fabric produced by the dyeing process (3 cycles)

Low absorbance of the reaction mixture means higher DPPH scavenging activity, which was determined by Equation 2 below and the results are shown in FIG. 7.

&Quot; (2) "

DPPH Free Radical Activity (%) = (C-S) / S × 100

Here, S and C are respectively measured values of the absorbance after the DPPH / methanol solution treatment in the sample and control of Table 2.

Looking at the measurement results of Figure 7, it is confirmed that only the reforming process (Comparative Example 1), or if the burying process was not carried out (Comparative Example 3 and Comparative Example 7) is very low DPPH free radical promotion activity of Example 2 Through this, it was confirmed that the antioxidant effect of the cotton fabric prepared by the dyeing method of the present invention is very excellent.

Experimental Example  6: of dyed cotton fabric Color fastness ( colorfastness Measurement experiment

Color fastness measurements of cotton fabrics were performed according to the American Association of Textile Chemists and Colorists (AATCC) test method, and the results are shown in Table 4 below. In Table 5 below, the color fastness rating was visually observed by the expert group of the color change, and the color fastness rating was compared with the gray scale, and was expressed in the range of 1 to 5 grades.

division Control group Comparative Example 1 Example 1 Color fastness
(Light fastness) 1 rating 1.5 ratings 3 ratings Color fastness
Washing fastness 1.5 ratings 4 ratings 4 ratings Sweat fastness
(Perspiration
Fastness) 2 ratings 2 ratings 3.5 ratings Control: Pure Cotton Fabric
Comparative Example 1: A cotton fabric subjected to only a modification process in the same manner as in Example 1 on a pure cotton fabric
5 stars: no change, 4 stars: slight change, 3 stars: normal,
Level 2: Severely Changing, Level 1: Severely Changing

Looking at the color fastness measurement results of Table 5, Example 1 dyed by the method proposed by the present invention showed a light fastness, wash fastness and sweat fastness of all three or more grades, but not control and mordant treatment Comparative Example 1, which was not, had very low light fastness and sweat fastness.

Through the examples and experimental examples, it was confirmed that the dyeing treatment after the natural dyeing (branch root extract dyeing agent), the dyeing treatment and the dyeing treatment greatly improved the color fastness, that is, the dyeing durability. In addition, the improvement of dyeing durability affects the persistence of antimicrobial and antioxidant properties, thereby confirming that it is possible to manufacture high-quality cotton fabric products.

Therefore, the coating material prepared by the dyeing method of the present invention can be applied to various eco-friendly products, and is not particularly limited, but is very suitable for use in diapers, sanitary napkins, underwear and beddings, which are textile products directly in contact with the skin. Do.

Claims (15)

In dyeing the coating material,
Modifying one or both sides of the coating material with a modifier comprising a cationic agent;
Neutralizing and drying the reformed coating material; And
Embedding the dried coating material with a mordant containing a gall bladder extract;
Coating material dyeing pretreatment method comprising a. The method of claim 1, wherein the modifier
Coating material dyeing pretreatment method characterized in that it comprises 0.05 to 0.2% by weight of the cationic agent in the total weight of the modifier. The method of claim 1, wherein the reforming step
Coating material dyeing pretreatment method characterized in that performed by PB (pad batch) method. The method of claim 3, wherein the PB method
A coating material dye pretreatment method characterized by performing under 100% wet pickup. The method of claim 1, wherein the cationic agent is
A coating material dye pretreatment method characterized by the following formula (1);
[Chemical Formula 1]

In Formula 1, R ¹ to R ³ are independent of each other, and are a hydrogen atom, a methyl group, or an ethyl group, and R ⁴ is a C1 to C5 straight or crushed alkyl group. The method of claim 5,
R ¹ , R ² and R ³ are methyl groups, and R ⁴ is an ethyl group or a propyl group. According to claim 1, wherein the mordant is
Coating material dyeing pretreatment method characterized in that it comprises 5 to 15% by weight of gallnut extract in the total weight of mordant. According to claim 1, wherein the mordant is
Coating material dyeing pretreatment method characterized in that the pH 3 ~ 4. 9. The method according to any one of claims 1 to 8,
And the coating material is at least one natural coating material selected from cotton, wool and silk, and the natural coating material is fiber, yarn, woven or knitted fabric. Modifying one or both sides of the coating material with a modifier comprising a cationic agent;
Neutralizing and drying the reformed coating material;
Embedding the dried coating material with a mordant containing a gall bladder extract; And
Dyeing the mordant coating material with a dye including the root extract;
Coating material dyeing method comprising a. The method of claim 10, wherein the dyeing agent
Covering material dyeing method comprising 1 to 20% by weight of branched root extract and 80 to 99% by weight of ethanol. The method of claim 10, wherein the dyeing agent
Coating material dyeing method characterized in that the pH 6.5 ~ 7.5. The coating material dyeing method according to claim 10, wherein the dyeing step is repeated 1 to 5 times. Eco-friendly product comprising a coating material dyed by the dyeing method of any one of claims 10 to 13. The eco-friendly product of claim 14, wherein the eco-friendly product is at least one selected from diapers, sanitary napkins, underwear, and bedding.

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