KR101298132B1 - Omija dye and a method of preparing the same and a method of dyeing using the same - Google Patents

Abstract

The present invention relates to a Schizandra dye and a dyeing method of preparing a raw material through the collection and washing, grinding, Schizandra; An extraction step of extracting Schisandra chinensis extract by heating the Schizandra chinensis in ethanol; Residue removal step of removing the extracted Schizandra residues; Schisandra dye, characterized in that it comprises an ethanol separation step of separating the ethanol from the extract of Schizandra chinensis, and a method for its preparation and dyeing method using the same.

Description

Omija dye and a method of preparing the same and a method of dyeing using the same

The present invention relates to a Schizandra dye, a method for producing the same, and a dyeing method using the same. Specifically, a dye-based Schizandra dye with antimicrobial activity as a dye using an extract extracted from Schizandra chinensis and its manufacturing method and a dyeing method using the same It is about.

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

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

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

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

The natural dyes can be obtained by dyeing using pigments from animals, plants and minerals existing in nature to obtain a natural, luxurious and emotional color that can not be obtained from chemical dyes, side effects such as allergic reactions that occur in chemical dyes It does not have antiallergic, antimicrobial or deodorant effects.

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

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

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

The natural dyes may be widely used in addition to fibers, such as metals, wood, leather, ceramics, cosmetics, toilet paper, paints, food coloring, medicinal coatings, crafts, such as clothing, household goods, foodstuffs, house products, industrial products.

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

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

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

However, the natural dyes so far developed as natural materials such as pine needles or wormwood is not easy to extract the natural dyes from the natural material, the efficiency is very low, there is a problem inferior in color reproducibility.

In order to solve the above problems, an object of the present invention is to provide an environmentally friendly and antimicrobial Schizandra dye and its manufacturing method by extracting the pigment component from Schizandra.

In addition, an object of the present invention is to provide an environmentally friendly and easy natural dyeing method using the Schizandra dye.

In order to achieve the above object, the present invention provides a raw material preparation step of preparing a raw material by washing, pulverizing, harvesting Schisandra chinensis; An extraction step of extracting the Schizandra chinensis extract by heating the Schizandra chinensis in ethanol for 5-7 hours at 70-95 ℃; Residue removal step of removing the extracted Schizandra residues; The Schizandra chinensis extract provides a method for producing Schizandra chinensis comprising an ethanol separation step of separating ethanol with a rotary vacuum evaporator.

In addition, the Schizandra chinensis provides a method for preparing Schizandra chinensis, characterized in that one or two or more of Schizandra fruit, Schizandra fruit, Schizandra seeds.

In addition, the Schizandra chinensis in the extraction step provides a method for producing Schizandra chinensis characterized in that the extract of Schizandra chinensis extract in 3 to 10 times the weight of Schizandra chinensis.

In addition, there is provided a schizandra dye, which is prepared by the above method.

In addition, the present invention is a dyeing method using a Schizandra dye, comprising: a pretreatment step of removing impurities of a material to be dyed; Dyeing the pretreated material in a salt solution containing Schizandra dyes at 70 to 110 ° C. for 10 to 50 minutes; A embedding step of embedding the dyed material in a mordant for 10 to 30 ° C. for 10 to 30 minutes; It provides a dyeing method using Schisandra chinensis, characterized in that it comprises a washing step of washing the embedded material in a wash solution at 60 to 100 ℃, 20 to 40 minutes.

In addition, the Schizandra chinensis dye provides Schisandra dye using a Schizandra dye, characterized in that the Schisandra chinensis in ethanol and extracted by heating in a hot water, ethanol is separated by a rotary vacuum evaporator.

In addition, the salt solution provides a dyeing method using a Schizandra dye, characterized in that 0.2 to 1.5 parts by weight of Schizandra dye in 100 parts by weight of distilled water.

In addition, the mordant solution provides a dyeing method using Schisandra chinensis characterized in that 1 to 5 parts by weight of alum is mixed with 100 parts by weight of distilled water.

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

Hereinafter, preferred embodiments of the present invention will be described in detail with reference to the accompanying drawings. First, it should be noted that, in the drawings, the same components or parts have the same reference numerals as much as possible. In describing the present invention, detailed descriptions of related well-known functions or configurations are omitted in order not to obscure the subject matter of the present invention.

As used herein, the terms "about", "substantially", and the like, are used at, or in close proximity to, numerical values as are indicative of the manufacturing and material tolerances inherent in the meanings mentioned, Absolute figures are used to prevent unfair use by unscrupulous infringers.

The present invention relates to a method for producing a dyeable schizandra dye in Schizandra chinensis and a dyeing method for dyeing with Schizola dye obtained.

Omija (Omija) used in the present invention is a plant belonging to the Magnoliaceae, whose scientific name is recorded as Schizandra Chinensis Baillon, and is an active woody plant in northeastern China, Southeast Asia, Japan, Sakhalin, and the Korean Peninsula. It grows naturally in the forests of the region or is grown for ornamental or herbal medicine in some specific areas.

Schisandra chinensis differs in its natural aroma, taste, and color depending on the variety and cultivation environment. Natural scents are aliphatic and aromatic alkaloids, flavonoids, terpenes, It is represented by components, such as phenols.

Schizandra chinensis consists of pericap, Schizandra fruit, and Schizandra seeds, and the color of Schizandra pericarp changes from purple to red due to photosynthetic action of anthocyanine pigments. The fruit of Schisandra chinensis contains citric acid, malic acid, malic acid, succinic acid, tannic acid, organic acid of vitamin C (ascorbic acid), glucose (g1ucose) or fructose (fructose). ) And various flavors.

Schisandra chinensis contains about 18.5% of lignan and about 1.6% of citral, including schizandrin, schizandran, r-schizandrin, schizandrol, deoxyschizandrin, gormsin-A, B, C, It is reported to contain essential oils such as F, G, angeloylgomisin, and dibenzocyclo-octadiene.

Generally, Schisandra chinensis consists of 80.0% moisture, 1.2% protein, 1.0% fat and other components such as glucose, vitamin C, and organic acids and inorganic salts. Glucose (g1ucose) contained in Schisandra chinensis fruit is fermented by enzymes, and Schisandra liquor can be obtained. Omaza has a unique natural aroma, taste and color, and it has been used since ancient times as a ingredient in various Korean foods such as tea, tea, omiza liquor, omiza drink, omiza noodle and omiza confectionery. However, today, the efficacy of Omara is widely recognized as antibacterial, anticancer, antioxidant, detoxifying, lowering blood sugar, lowering blood pressure, skin whitening and anti-aging, and natural dyeing. , Medicinal cosmetics, natural dyes, pharmacology, chemical new materials are attracting attention.

In particular, cirsimaritin, phenols magnolia and honokinol, and terpenes a-pinene, menthol, camphor and geraniol among the flavonoids, which are aromatic components of Schisandra chinensis, have been reported to have strong physiological activities.

Recently, the research trend of natural schizandra has been recorded in Japan and China to study the antimicrobial and anti-cancer activity of Schizandra chinensis with new materials.In Korea, the physiological activity, hypoglycemic effect of Schizandra chinensis extract and application of cosmetic industry using Schizandra chinensis Is being studied.

1 is a process showing the manufacturing method of the Schizandra dye of the present invention, the method for producing Schizandra dye is prepared including a raw material preparation step, extraction step, residue removal step, ethanol separation step.

The raw material preparation step is prepared by collecting and cleaning the schisandra chinensis. It will be preferable to wash and then crush the Schizandra chinensis.

Generally, Schisandra chinensis can be divided into Schisandra chinensis (pericap), Schisandra chinensis fruit (fruit), Schisandra chinensis (seed) and Schisandra chinensis used in the present invention can be used as Schisandra chinensis, Schisandra chinensis, Schisandra chinensis, or Schisandra chinensis. It is also possible to use a mixture of two or more of Schizandra chinensis fruits and Schizandra chinensis.

The extraction step may be a method using a solvent such as water vapor, methanol, ethanol, ether, propylene glycol, supercritical fluid extraction using carbon dioxide, but using ethanol to increase the efficiency and reproducibility of Schizandra chinensis extract. Would be desirable.

In the step of extracting Schisandra chinensis using ethanol, Schisandra chinensis extract was extracted by adding Schisandra chinensis to ethanol for 5-7 hours at 70-95 ° C, which is similar to the boiling point of ethanol.

If less than the above range, there may be a component that remains in trace amounts due to insufficient dissolution of the pigment component of Schizandra, if exceeding the above range, Schizandra extract components may be deteriorated.

The ethanol may be denatured of Schizandra extract or 90% or more of ethanol (C ₂ H ₅ OH) aqueous solution.

In addition, it is preferable to extract the Schizandra chinensis extract into 3 to 10 times the weight of Schizandra chinensis so that Schizandra immersed in ethanol.

The residue removal step is to remove the Schizandra residues from Schizandra extract extracted with ethanol.

In order to completely remove the Schizandra residues, it is preferable to remove Schizandra residues using a 150 ~ 250mesh sieve (sieve)

The ethanol separation step is to obtain a natural Schizandra dye by removing ethanol from the Schizandra extract, the Schizandra extract is separated by ethanol with a rotary vacuum evaporator to obtain Schizandra dye.

The ethanol-separated schizandra dye may be lyophilized to obtain a solid of Schizandra dye.

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

Figure 2 is a process showing the dyeing method of Schizandra dye of the present invention Schizandra dyeing method is dyed in the pre-treatment step, dyeing step, mordant step, washing step.

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

The dyeing step is a step of dyeing the pretreated material in the salt solution containing Schisandra chinensis extract is dyed for 70 to 110 ℃, 10 to 50 minutes.

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

The salt solution is prepared by mixing 0.2-1.5 parts by weight of Schizandra chinensis extract described above with 100 parts by weight of distilled water. When the Schizandra chinensis extract is mixed in less than 0.2 parts by weight, the uniformity of the dye is inhibited, and when mixed in excess of 1.5 parts by weight, the efficiency of dyeing may decrease.

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

The mordant is prepared by mixing 1 to 5 parts by weight of alum in 100 parts by weight of distilled water. When the alum is mixed at less than 1 part by weight, it is not possible to expect mortar, and when it is mixed at more than 5 parts by weight, the efficiency of mortar may be reduced.

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

The washing step is a step of washing off undyed Schizandra dyes, washing with water at 60 to 100 ° C. for 20 to 40 minutes in a washing solution.

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

As described above of the present invention, it is dyed in a pretreatment step, a dyeing step, a mordant step, and a washing step, and the dyeing effect can be further increased by performing a pre-dye treatment using alum and the like before the dyeing step to increase the dyeing effect.

As described above, the present invention has an effect of providing an environmentally friendly and antimicrobial Schizandra dye by extracting Schizandra extract that can be used as a dye in Schizandra chinensis.

In addition, it is effective to provide a natural dyeing method that is easy to dye and environmentally friendly using the Schizandra dye.

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

1 is a process chart showing a method for producing a schizandra dye of the present invention.
Figure 2 is a process chart showing the dyeing method of Schizandra dye of the present invention.

Hereinafter, the Schizandra dye of the present invention and a dyeing method using the same will be described in detail by Examples.

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

1. Manufacture of Schizandra Dyes

Domestic Schizandra chinensis was prepared by washing Schizandra chinensis, Schizandra chinensis fruit, Schizandra chinensis seeds, and crushed with a mortar and pestle to prepare raw materials. 200g of Schizandra chinensis prepared in 800ml of 93% ethanol aqueous solution, heated at 85 ℃ for 6 hours, and extracted Schizandra chinensis extract. It was.

In the Schizandra chinensis extract, Schizandra residue was removed using a 200mesh sieve to obtain 580g of Schizandra chinensis extract.

The 580 g of Schisandra chinensis extract was extracted at 60 rpm using a rotary vacuum evaporator to obtain 158 g of Schisandra chinensis dye.

Yield of the Schizandra dye was calculated as follows.

Yield = (G ₁ / G ₂ ) × 100

G ₁ : weight of Schizandra dye (g)

G ₂ : amount of Schizandra chinensis + ethanol (g)

Ethanol Density 0.780 g / ml

2. ICP / OES Analysis

To confirm the inorganic component of the Schizandra dye, 0.1g of Schizandra dye was diluted and dissolved in 100ml of 5% nitric acid solution, and then measured by Inductively Coupled Plasma / Optical Emission Spectrometry. , Al, As, B, Ba, Be, Ca, Co, Cd, Cr, Cu, K, Li, Fe, Mg, Mn, Mo, Na, Ni, Pb, Sb, Se, Si, Ti, Tl, V And Zn were used for sample measurement.

As a result of analyzing the components of the Schizandra dye, K (107.30 ppm), Na (2.110 ppm), Ca (0.935 ppm), Mg (0.891 ppm), Ti (0.345 ppm), Si (0.281 ppm), and Li (0.270 ppm) ), Cu (0.256ppm), Fe (0.126ppm) and various inorganic components were detected, especially Li, which has recently emerged as an energy source.

3. GC / MSD Analysis

In order to identify the organic components of the Schizandra dye, 0.1g of Schizandra dye was diluted and dissolved in 100ml of diethyl ether, and then analyzed and measured by Gas Chromatography / Mass Selective Detector.

The Schizandra dye component is benzene (10.808), acetic acid (11.289), tricyclo dec-3-ene (12.484), a-pinene (13.996), phenol (14.183), ß-terpene (15.840), benzene methanol (17.506) , a-terpinolene (17.616) and various organic components were detected, especially amipine component a-pinene (l3.996) and β-terpene (15.840) and a-terpinolene (17.616) were detected.

4. Antibacterial Test of Schizandra Dyes

Dilute and dissolve in 0.5 g of Schizandra dye in 100 ml of distilled water, and dissolve 1 ml of this solution in Mueller Hilton Broth medium solution (10 ml), followed by staphylococcus aureus (Example 1) and aspergillus niger (Example 2). Each was inoculated to the antimicrobial experiment of microorganisms. The antimicrobial experiments examined the relationship between the viable cell count and the change according to the culture conditions and time of the strain. Here, without adding Schizandra dye as a control, a certain amount of staphylococcus anreus (Comparative Example 1) and aspergillus niger (Comparative Example 2) was added to the medium solution. The medium used was Mueller Hilton Broth (Difco. Lab. CO., USA).

Table 1 is a table showing the test results of Schisandra chinensis Dye microorganisms depending on the incubation time.

Hours (hrs) Staphylococcus aureus Aspergillus niger Example 1 Comparative Example 1 Example 2 Comparative Example 2 0 + + + + 24 + + + + 48 + + + + 72 - + - + 96 - + - + 120 - + - + Test temperature: 36 ℃
+: Microbial positive reaction
-: Microorganism negative reaction

As shown in Table 1, Example 1 and Example 2 showed a positive reaction in the initial antimicrobial test, but showed a negative reaction after 72hrs (3day) after the microbial culture test. In Comparative Example 1 and Comparative Example 2 in which the microorganism was added to the medium solution without adding the extract, positive reaction was shown in the initial antibacterial test, but the positive reaction was continued even after 72hrs (3day). You can see that appears.

Thus, it can be seen that Schizandra dye has an antimicrobial effect on microorganisms.

5. Dyeing with Schizandra Dyes

Example  3,4

Pretreatment step of neutralizing cotton (Example 3) and silk (Example 4), which are natural fibers for dyeing with Schizandra dye prepared above, at 95 ° C. for 30 minutes, and then boiled in boiling water at 95 ° C. for 10 minutes to remove impurities.

The cotton and silk were dyed at 90 ° C. for 30 minutes in a salt solution mixed with 100 g of distilled shoe in 0.5 g of Schizandra dye.

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

Comparative example  3,4

Cotton and silk were dyed with Schisandra dye as in Examples 3 and 4, but were dyed without performing a mordant step.

◈ Dyeing Experiment

After dyeing, the dyeing brightness, color direction, and color difference were measured using a color difference meter, and the results are shown in Table 2.

division DL * Da * Db * DE *  if Example 3 87.310 2.240 12.540 0 Example 4 87.690 1.660 12.490 0.800  Dog Comparative Example 3 89.870 2.800 12,000 0 Comparative Example 4 84.910 2.580 13.270 1.340

In Table 2, DL * stands for brightness (brightness of color), Da * and Db * for color direction, and DE * for color difference, where DL * stands for dogs (84.910) in a mordant state (84.910). 87.690) was lighter and brighter and lighter when dyed.

In addition, Da * and Db * showed the color of ivory color when dyed in the direction of color, and DE * was the color difference of the sheet which is based on the no-border state, and was calculated by the following equation.

As a result of the dyeing experiment, the brightness was bright and light, and it was found that the kite appeared darker than the dog when dyed. In addition, when the dyeing method was used, the direction of the color appeared in ivory color system. It was higher in silk (1.340) than cotton (0.800). Therefore, it was confirmed that it can be used as a natural dye as a Schizandra dye containing Schizandra components.

Claims (9)

In the manufacturing method of Schizandra dyes,
A raw material preparation step of preparing raw materials by collecting and washing schisandra chinensis;
An extraction step of extracting the Schizandra chinensis extract by heating the Schizandra chinensis in ethanol for 5-7 hours at 70-95 ℃;
Residue removal step of removing the Schizandra residues from the Schizandra extract;
Schizandra dye production method, characterized in that it comprises an ethanol separation step of separating the ethanol with the Schizandra extract rotary vacuum evaporator. The method of claim 1,
The Schisandra chinensis, Schisandra chinensis fruit, Schisandra chinensis fruit, Schisandra chinensis Seed production method of Schisandra chinensis characterized in that the mixture of two or more. The method of claim 1,
In the extracting step, Schisandra chinensis method, characterized by extracting Schisandra chinensis extract into ethanol of 3 to 10 times the weight of Schisandra chinensis. Schizandra dye, which is prepared by the method of any one of claims 1 to 3. In the dyeing method using Schisandra dye,
A pretreatment step of removing impurities of the material to be dyed;
Dyeing the pretreated material in a salt solution containing Schizandra dyes at 70 to 110 ° C. for 10 to 50 minutes;
A embedding step of embedding the dyed material in a mordant for 10 to 30 ° C. for 10 to 30 minutes;
The dyeing method using a Schizandra dye, characterized in that it comprises a washing step of washing the embedded material in a wash solution at 60 to 100 ℃, 20 to 40 minutes. The method of claim 5,
The Schizandra dye is a dyeing method using Schisandra dye, characterized in that the Schisandra chinensis in ethanol and extracted by heating in a hot water, ethanol is separated by a rotary vacuum evaporator. The method of claim 5,
The salt solution is a dyeing method using a Schizandra dye, characterized in that 0.2 to 1.5 parts by weight of Schizandra dye in 100 parts by weight of distilled water. The method of claim 5,
The mordant is dyeing method using Schisandra chinensis, characterized in that 1 to 5 parts by weight of alum is mixed with 100 parts by weight of distilled water. The method of claim 5,
The washing solution is a dyeing method using Schisandra chinensis characterized in that the neutral detergent having a pH of 5 to 8 contains 5 to 15% by weight.

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