KR100264675B1 - Preparation method of natural indigo from polygoum tinctorlum - Google Patents

Preparation method of natural indigo from polygoum tinctorlum Download PDF

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KR100264675B1
KR100264675B1 KR1019980008599A KR19980008599A KR100264675B1 KR 100264675 B1 KR100264675 B1 KR 100264675B1 KR 1019980008599 A KR1019980008599 A KR 1019980008599A KR 19980008599 A KR19980008599 A KR 19980008599A KR 100264675 B1 KR100264675 B1 KR 100264675B1
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pigment
fermentation
dyeing
natural
indigo
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KR19990074786A (en
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정인모
이용우
우순옥
임수호
김영대
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김강권
농촌진흥청
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B7/00—Indigoid dyes
    • D—TEXTILES; PAPER
    • D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
    • D06P3/58—Material containing hydroxyl groups
    • D06P3/60—Natural or regenerated cellulose

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Coloring (AREA)

Abstract

PURPOSE: A method for preparing natural indigo pigment is provided to readily allow one other than an initiated expert to extract and ferment the pigment, mass-produce it, mass-dye with it, give good color, and enhance article quality. CONSTITUTION: The method comprises adding calcium hydroxide to natural indigo to extract indigo pigments, lyophilizing them to form powder of indigo pigments, adding calcium hydroxide or sodium hydroxide as an alkali agent and starches as fermenting nutrient to the powder, in order to make the water-soluble indigo pigment powder, and fermenting them. Thus, the obtained pigment shows good color. The natural indigo pigment is used to dye silk, ramie, hemp and cotton.

Description

천연쪽 색소의 제조방법Manufacturing method of natural pigment

본 발명은 천연쪽(indigo)색소의 제조방법 및 이를 이용한 명주, 모시, 삼베 및 면의 염색방법에 관한 것이다.The present invention relates to a method for producing natural indigo (indigo) pigment and a method for dyeing silk, ramie, burlap and cotton using the same.

보다 상세히 설명하면 생쪽에서 색소를 우러내어 소석회(消石灰)를 넣고 제조한 후, 쪽 색소를 물에 용해하고 발효시 영양원으로 탄소원과 함께 알칼리제를 첨가하여 발효시킨 후 20-30℃에서 염색하는 방법에 관한 것이다.In more detail, after the pigment is removed from raw raw material, it is prepared by adding calcined lime (消石灰), and then the dye is dissolved in water and fermented by adding an alkaline agent together with a carbon source as a nutrient source during fermentation, followed by dyeing at 20-30 ° C. It is about.

본 발명에 관련된 종래기술은 일본 쪽 염색공방과 국내 전통쪽 염색농가에서 사용하고 있는 전통 천연쪽 색소추출 방법은 쪽풀이 꽃피기 전에 수확하여 용기에 넣고 물을 부어 1-3일 경과후 쪽풀을 건져내고 그 액에 조개껍질 또는 굴껍질 등을 불에 태워 만든 가루를 넣고 교반시켜 용출된 색소액이 연녹색에서 파란색으로 변화되면서 파란침전물이 형성된다.The conventional technique related to the present invention is a traditional natural pigment extraction method used in Japanese dyeing workshops and domestic traditional dyeing farms, harvested before the flowering of prunus, put it in a container, pour water, and extract the puff after 1-3 days In the solution, the powder made by burning shells or oyster shells on fire is stirred, and the eluted pigment solution changes from pale green to blue to form a blue precipitate.

교반을 멈추고 2-3시간 경과후 상등액을 분리하여 침전물을 면포대에서 여과 및 농축시켜 쪽 색소덩어리를 제조한다.After stopping the stirring for 2-3 hours, the supernatant was separated, and the precipitate was filtered and concentrated on a cotton bag to prepare a lump of pigment.

이와 같이 제조된 쪽 색소덩어리는 잿물에 용해하여 굴 또는 조개껍질을 태운 가루를 첨가하여 다시 용기에 넣고 여름철에는 자연상태에서 1-2개월 발효시키고 겨울철에는 따뜻한 실내에서 발효시킨 후 염색한다.The colored pigments prepared in this way are dissolved in lye, added with powdered oysters or shells, and then put back into the container, fermented for 1-2 months in the natural state in summer, and fermented in a warm room in winter and dyed.

위의 과정에서 사용되는 굴껍질가루를 만드는데는 나무에 굴껍질 등을 놓은 다음 그 위를 흙으로 덮어서 5시간 이상 태워야 하는 번잡함이 있고, 또한 사용되는 잿물도 만든 재의 종류별로 성분이 다르고 수소이온농도(pH)가 다르기 때문에 쪽의 발효상태가 불균일하며, 또한 발효작용이 충분하지 못하여 발효가 완료될때까지 1-2개월 정도의 장시간이 걸리며 온도 및 수소이온 농도관리 등에 세심한 주의를 하지 않으면 실패하는 경우가 많아 오랜 경험자 아니면 손쉽게 염색할 수 없다.In order to make oyster shell powder used in the above process, oyster shell is placed on wood and covered with soil and burned for 5 hours or more, and the lye used is different in composition and hydrogen ion concentration. If the fermentation status of the side is different due to different pH, and fermentation is not sufficient, it takes 1-2 months for the fermentation to be completed and fails if you do not pay close attention to temperature and hydrogen ion concentration management. Many people can not dye easily if you have long experience.

또한 자연발효는 쪽 색소자체의 글리코사이드(glucoside)가 가수분해에 의하여 포도당이 되고 다시 공기중의 유산균에 의한 유산발효를 일으킨 후 다시 낙산발효를 하면 수소(H2)와 탄산가스(CO2)가 발생하는데 수소가 쪽색소를 환원시킨 것이다.In addition, the natural fermentation of the glycoside (glucoside) of the side pigment itself becomes glucose by hydrolysis, and again after lactic acid fermentation by lactic acid bacteria in the air, but when the acid is fermented again, hydrogen (H 2 ) and carbon dioxide (CO 2 ) Occurs and hydrogen has reduced the side pigment.

그러므로 전통발효방법은 발효영양원이 부족하게 되기 쉽기 때문에 발효기간이 장시간 필요하며 또한 발효가 충분하지 않은 미발효상태가 될 경우가 많다. 이러한 단점을 개선하기 위하여 발효액에 발효원으로서 글루코사이드를 보충해 주면 아래와 같이 분해되어 발효가 신속하게 된다.Therefore, traditional fermentation methods tend to lack fermentation nutrients, so the fermentation period is required for a long time, and the fermentation is not sufficient. In order to improve these disadvantages, the fermentation broth is supplemented with glucoside as a fermentation source, so that the fermentation is rapidly broken down as follows.

(C6H10O5)n + H2O → C6H12O6(포도당)(C 6 H 10 O 5 ) n + H 2 O → C 6 H 12 O 6 (glucose)

C6H12O6→ 2CH8CH0HCOOH (유산)C 6 H 12 O 6 → 2CH 8 CH0HCOOH (lactic acid)

2C3H6O3→ C3H7COOH + 2CO2+ 2H2(낙산)2C 3 H 6 O 3 → C 3 H 7 COOH + 2CO 2 + 2H 2 (butyric acid)

본 발명은 전통방법에 의한 쪽풀 색소제조시에 조개껍질, 굴껍질가루 대신에 소석회를 사용하며, 발효시에는 발효영양원과 강한 알칼리제를 사용 발효액의 수소이온농도를 조절하여 온도 40-95℃에서 발효가 가능하며, 염색직물의 색상은 전통방법에 비하여 더욱 쪽색을 띈다.The present invention uses calcined lime instead of clam shells and oyster shell powder in the production of green grass pigment by the traditional method, and fermentation at a temperature of 40-95 ℃ by adjusting the hydrogen ion concentration of the fermentation broth using fermentation nutrient source and strong alkali agent during fermentation The color of dyed fabric is more versatile than the traditional method.

일반적으로 쪽풀 색소는 물에 불용성이므로 염색전에 발효에 의하여 발효시켜서 leuco염 형태로 만들어서 염색하여야 하기 때문에 발효제와 수소이온 농도조절이 무엇보다 중요한 요인이다. 이를 위하여 전통발효방법에서는 조개 및 굴껍질가루 등 자연에서 얻은 알칼리제를 사용하지만 이들의 제조공정이 복잡하고, 또한 일반인으로서는 제조가 어렵기 때문에 이를 개선하기 위하여 소석회(Ca(OH)2)나 수산화나트륨(NaOH)를 사용하면 pH조절이 간편하면서 알맞는 수소이온농도를 얻을 수 있다.In general, since the green pigment is insoluble in water, fermentation agent and hydrogen ion concentration control are the most important factors because it must be fermented by fermentation before dyeing to make leuco salt. To this end, traditional fermentation methods use natural alkalis such as shellfish and oyster shell powder, but their manufacturing process is complicated and difficult for the general public to manufacture. Therefore, to improve this, calcined lime (Ca (OH) 2 ) or sodium hydroxide is used. By using (NaOH), it is easy to adjust pH and get proper hydrogen ion concentration.

제1도는 천연쪽 발효액의 pH와 염색물질의 염착농도를 나타낸 것이다.Figure 1 shows the pH of the natural fermentation broth and the dyeing concentration of the dyeing material.

제2도는 천연쪽 염색온도와 염색직물의 염착농도를 나타낸 것이다.Figure 2 shows the natural dyeing temperature and the dyeing concentration of the dyed fabric.

본 발명은 생쪽에서 색소를 추출하여 쪽색소분말을 제조하는 공정, 쪽색소를 류코형 염으로 변화시키는 발효공정, 천연 쪽색소의 최적 염색조건 설정으로 구성되어 있다.The present invention is composed of a process of preparing a pigment pigment by extracting the pigment from raw, a fermentation process of changing the pigment of the pigment to a leuco salt, and setting of optimal dyeing conditions of natural pigment.

쪽 색소분말 제조공정에서는 천연쪽색소를 추출시에 소석회를 첨가하여 작업의 간편성과 추출수율을 높이고, 발효공정에서는 수산화나트륨와 포도당을 첨가하여 강한 쪽색 염료를 얻을 수 있다. 염색조건 설정에서는 쪽 수산화나트륨, 포도당의 사용량에 따른 최적 발효조건을 확립하는 데 있다.In the process of manufacturing the pigment powder, calcined lime is added during the extraction of natural pigment to enhance the simplicity and the extraction yield. In the fermentation process, sodium hydroxide and glucose may be added to obtain a strong pigment. The dyeing condition is to establish the optimum fermentation conditions according to the amount of sodium hydroxide and glucose.

이하, 본 발명을 실시예에 의하여 보다 구체적으로 설명하고자 한다.Hereinafter, the present invention will be described in more detail with reference to Examples.

이들 실시예는 오로지 본 발명을 설명하기 위한 것으로 본 발명의 범위가 이들 실시예에 국한되지 않는 것은 당업계에서 통상의 지식을 가진자에게 있어서 자명할 것이다.These examples are only for illustrating the present invention, it will be apparent to those skilled in the art that the scope of the present invention is not limited to these examples.

[실시예 1]Example 1

[쪽 색소분말 제조][Production of Pigment Powder]

쪽풀이 꽃피기전(8월상순경)에 생잎 80g을 물 1ℓ에 넣고 소석회의 첨가량을 달리하여 4종류의 추출용액을 만들어 하루동안 쪽색소를 추출한 다음 색소추출액을 농축 동결건조하여 각각의 쪽색소 분말을 제조하였다. 이 색소분말의 착색도를 색차계(Color Difference Meter)를 이용하여 조사한 결과 아래표 1에서와 같이 색상은 소석회 첨가량이 30g/ℓ까지는 증가하였으나 그 이상에서는 색상값이 감소하였으며 명도값도 소석회 첨가량 3g/ℓ까지 점차적으로 감소한 것으로 보아 생쪽 색소추출방법에 있어서 소석회량은 3g/ℓ 첨가하는 것이 쪽색소의 착색도가 가장 높다.Put the 80g of fresh leaves in 1ℓ of water before the flowering of the green grass (at the beginning of August) and make 4 kinds of extract solution by changing the amount of added lime, and extract the green pigment for one day. Was prepared. The coloration of this pigment was investigated using a color difference meter. As shown in Table 1 below, the amount of hydrated lime increased up to 30 g / l, but the color value decreased. It was gradually decreased to 1 L, and the amount of calcined lime added in the raw pigment extraction method was the highest in the coloring of the side pigments.

[실시예 2]Example 2

[천연 쪽의 발효][Natural fermentation]

실시예 1에서 3g/ℓ의 소석회를 넣고 제조한 천연쪽 색소는 물에 불용이기 때문에 그래도 섬유에 결합 및 흡착이 안되므로 염색하기 위하여서는 반드시 전 단계로 류코(Leuco)형혐으로 발효시켜서 염색하여야 한다.Since natural pigments prepared by adding 3 g / L of hydrated lime in Example 1 are insoluble in water, they cannot be bound and adsorbed on the fiber, but must be fermented with Leuco mold in the previous step for dyeing.

류코형염으로 변화시키기 위하여서는 강알칼리액과 쪽색소의 발효제가 필요한 데 알칼리제로는 전통방법에서는 굴껍질가루등을 사용하지만 본 발명에서는 간편성과 높은 수소이온농도를 얻기 위하여 수산화나트륨을 사용하고 영양원으로 글로쿠스를 사용하였다.In order to change to leuko salt, strong alkaline solution and fermentation agent of side pigment are required. Alkali is used as oyster shell powder in the traditional method, but in the present invention, sodium hydroxide is used to obtain simplicity and high hydrogen ion concentration. Cous was used.

제1도는 수산화나트륨으로 수소이온농도를 조절한 후 발호시켜 염색한 직물의 염착농도(K/S)관계를 조사한 것이다.1 is to investigate the relationship between the dyeing concentration (K / S) of the fabric dyed by firing after adjusting the hydrogen ion concentration with sodium hydroxide.

발효액의 수소이온농도인 12.8까지는 쪽색소의 염착농도가 증가하지만 그 이상의 수소이온농도인 13.0에서는 감소하였다. 이것으로 보아 수소이온농도는 12.8이 발효에 가장 적당한 것으로 판명되었다.Up to 12.8, the hydrogen ion concentration of fermentation broth, the dyeing concentration of the side pigment was increased, but decreased at the higher hydrogen ion concentration, 13.0. From these results, the hydrogen ion concentration of 12.8 was found to be the most suitable for fermentation.

위 실험에서 수소이온농도가 낮은 경우에는 쪽색소가 밧트(Vat)산에서 류코형혐으로 충분히 변화되지 않으므로 각 섬유상에 흡착이 불량하기 때문이며, 수소이온 농도가 13.0으로 높은 경우에 과발효로 인하여 쪽색소가 뭉쳐서 염착성이 떨어지기 때문이다.In the above experiments, when the hydrogen ion concentration is low, the side pigment is not sufficiently changed from Vat acid due to the leuco form, so that the adsorption is poor on each fiber, and when the hydrogen ion concentration is 13.0, the side pigment is overferred. This is because the coalescing is reduced.

또한 발효액의 온도에 따른 염색직물의 염착농도를 조사한 결과는 아래 표 2와 같다. 즉 발효온도를 60℃, 80℃, 95℃에서 발효후 염색직물의 색채 및 염착농도를 비교한 결과 발효온도 95℃에서 색채와 염착농도가 가장 높아 적당발효온도는 95℃임이 판명되었고, 발효온도를 95℃로 하고 발효시간을 10분에서 60분까지 달리한 염색직물의 색채 및 염착농도를 비교하여 보면 표 3에서와 같이 발효시간 20분에서 색채와 염착농도가 가장 증가되므로 적정시간임이 입증되었다.In addition, the results of examining the dyeing concentration of the dyed fabric according to the temperature of the fermentation broth are shown in Table 2 below. In other words, the color and dye concentration of dyeing fabric after fermentation at 60 ℃, 80 ℃ and 95 ℃ were found to be the highest fermentation temperature at 95 ℃. When comparing the color and dyeing concentration of the dyeing fabric with different fermentation time from 10 minutes to 60 minutes at 95 ℃, it was proved to be the proper time because the color and dyeing concentration increased the most at 20 minutes as shown in Table 3. .

※ 글루코스 3g/ℓ 첨가, 발효온도 : 95℃※ Add glucose 3g / ℓ, fermentation temperature: 95 ℃

제2도는 발효 쪽 색소를 95℃에서 20분간 발효하여 염색온도별 염색직물의 염착 농도를 측정한 결과이다. 즉 쪽 색소의 염색온도가 30℃보다 높을수록 염착농도가 점차 감소됨을 보임으로써 적정 염색온도는 30℃임이 판명되었다.2 is a result of measuring the dyeing concentration of the dyed fabric by the dyeing temperature by fermenting the fermented pigment at 95 ℃ 20 minutes. That is, the dyeing concentration gradually decreased as the dyeing temperature of the side pigment was higher than 30 ℃, it was found that the proper dyeing temperature is 30 ℃.

[실시예 3]Example 3

[천연쪽 염색방법의 확정][Confirmation of Natural Dyeing Method]

실시예 1에서 소석회를 첨가하여 만든 쪽색소 용액에 3g/ℓ의 수산화나트륨 또는 수산화칼슘과 3g/ℓ의 포도당을 첨가하여 발효온도 95℃에서 20분간 발효시킨 본 발명의 방법과 전통발효방법에 따라 발효시킨 액을 30℃에서 염색한 염색직물의 염착농도를 아래 표 4에 나타내었다.Fermentation according to the method of the present invention and the traditional fermentation method of fermentation temperature at 95 ° C. for 20 minutes by adding 3 g / L sodium hydroxide or calcium hydroxide and 3 g / L glucose to the side pigment solution prepared by adding lime in Example 1 The dyeing concentrations of the dyeing fabrics dyed at 30 ° C. are shown in Table 4 below.

전통 : 4g/ℓ쪽 + 1ℓ의 잿물과 3g의 굴껍질가루 + 40㎖/ℓ 막걸리Tradition: 4g / ℓ side + 1ℓ of lye and 3g oyster shell powder + 40ml / ℓ rice wine

개발 1 : 4g/ℓ쪽 + 3g/ℓ NaOH + 3g/ℓ 포도당Development 1: 4g / ℓ side + 3g / ℓ NaOH + 3g / ℓ glucose

개발 2 : 4g/ℓ쪽 + 3g/ℓ Ca(OH)2+ 3g/ℓ 포도당Development 2: 4g / ℓ + 3g / ℓ Ca (OH) 2 + 3g / ℓ Glucose

즉, 전통 쪽 염색방법보다 본 발명들의 염색방법인 견, 모시 및 삼베 모두에서 염착농도(K/S)가 약간 증가함을 보였으며 표 5에서와 같이 이들 염색의 세탁, 땀 및 일광에 대한 염색견뢰도에서는 본 발명과 전통방법간에 큰 차이 없이 모두 우수하였다. 이와 같이 본 발명 쪽 염색방법은 전통방법에 비하여 색상이 우수하고 염색 견뢰도에 차이가 없어 실용성이 없다.That is, dyeing concentration (K / S) was slightly increased in both silk, ramie and burlap, which are the dyeing methods of the present invention, compared to the traditional dyeing method. In fastness, all were excellent without significant difference between the present invention and the traditional method. As described above, the dyeing method of the present invention is superior in color compared to the traditional method, and there is no difference in color fastness, so there is no practical use.

전통적인 쪽색소의 제조방법은 전수에 의존한 숙련자만이 할 수 있으나 본 발명은 천연쪽 색소의 추출 및 발효를 간편하고 용이하게 대량생산과 염색을 가능하게 하고 우수한 색상의 쪽 염색방법을 제공한다. 쪽풀을 재배하여 전통의류에 염색하면 상품성을 증대시켜 소득증가에도 기여할 수 있다.The conventional method of producing the color pigments can be made only by those skilled in the art, but the present invention enables easy and easy mass production and dyeing of natural color pigments, and provides a method of dyeing the color of excellent color. Growing grass and dyeing it in traditional clothing can increase the merchandise and contribute to income growth.

Claims (5)

전통 쪽염료의 제조방법에 있어서, 생쪽에 소석회를 첨가하여 쪽색소를 추출하고 동결건조하여 쪽색소 분말을 제조하는 단계와, 쪽색소 분말을 수용성으로 하기 위하여 알칼리제로 수산화칼슘(Ca(OH)2) 또는 수산화나트륨(NaOH)과 발효영양원으로 전분당류를 첨가하여 발효하는 단계로 구성된 것을 특징으로 하는 천연쪽색소의 제조방법.In the traditional method of producing a dye, the step of adding calcined lime on the raw side to extract the side pigment and freeze-dried to prepare the side pigment powder, calcium hydroxide (Ca (OH) 2 ) as an alkali to make the side pigment powder water-soluble Or sodium hydroxide (NaOH) and a fermentation nutrient source to add starch sugars to fermentation. 제1항에 있어서, 전분당류는 포도당, 말토스, 과당인 것을 특징으로 하는 천연쪽색소의 제조방법.The method of claim 1, wherein the starch sugar is glucose, maltose, fructose production method of natural pigment. 제1항에 있어서, 염색용 쪽색소는 쪽 4g/ℓ, 알칼리 3g/ℓ, 전분질 3g/ℓ로 구성된 배지에서 제조된 것을 특징으로 하는 천연쪽색소의 제조방법.The method of claim 1, wherein the dyeing side pigment is prepared in a medium consisting of 4g / l, 3g / l alkali, 3g / l starch. 제1항 또는 제3항에 있어서, 발효조건은 발효온도 90℃에서 발효시간 20분인 것을 특징으로 하는 천연쪽색소의 제조방법.4. The method of claim 1 or 3, wherein the fermentation conditions are 20 minutes of fermentation at a fermentation temperature of 90 ° C. 제1항에 있어서, 염색대상직물이 견, 모시, 삼베 및 면인 것을 특징으로 하는 천연쪽색소의 제조방법.The method of claim 1, wherein the fabric to be dyed is silk, ramie, burlap and cotton.
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