KR101010135B1 - The manufacturing method of the natural dye which used persimmon juice, and the natural dye which used persimmon juice, and the method to dye of the natural dye which used persimmon juice - Google Patents

The manufacturing method of the natural dye which used persimmon juice, and the natural dye which used persimmon juice, and the method to dye of the natural dye which used persimmon juice Download PDF

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KR101010135B1
KR101010135B1 KR1020100042165A KR20100042165A KR101010135B1 KR 101010135 B1 KR101010135 B1 KR 101010135B1 KR 1020100042165 A KR1020100042165 A KR 1020100042165A KR 20100042165 A KR20100042165 A KR 20100042165A KR 101010135 B1 KR101010135 B1 KR 101010135B1
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juice
dye
fabric
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natural dye
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김호영
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이진옥
주식회사 화수목
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B61/00Dyes of natural origin prepared from natural sources, e.g. vegetable sources
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/0001Post-treatment of organic pigments or dyes
    • C09B67/0017Influencing the physical properties by treatment with an acid, H2SO4
    • CCHEMISTRY; METALLURGY
    • C12BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
    • C12PFERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
    • C12P1/00Preparation of compounds or compositions, not provided for in groups C12P3/00 - C12P39/00, by using microorganisms or enzymes
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
    • D06P1/34General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using natural dyestuffs

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Abstract

PURPOSE: Natural dye using persimmon juice is provided to obtain soft fabrics with desired color through one time dyeing and to ensure excellent reproducibility. CONSTITUTION: A method for preparing natural dye using persimmon juice comprises: a persimmon juice preparation step; a fermentation step for forming tannin extract by accelerating fermentation while raising a temperature after protease and amylase enzymes are put into persimmon juice, and decomposing tannin included in persimmon juice; a stirring step for preparing a tannin composition by stirring the tannin extract and injecting alkali; and a pH adjustment step for controlling pH by adding acid to the tannin composition.

Description

감즙천연염료의 제조방법 및 감즙천연염료 그리고 감즙천연염료를 이용한 염색방법{The manufacturing method of the natural dye which used persimmon juice, and the natural dye which used persimmon juice, and the method to dye of the natural dye which used persimmon juice}The manufacturing method of the natural dye which used persimmon juice, and the natural dye which used persimmon juice, and the method to dye of the natural dye which used persimmon juice}

본 발명은 감즙을 이용한 천연염료 제조방법에 관한 것으로서, 더욱 상세히는 감즙을 염료로 제조하여, 피염물에 균일한 염색이 가능하고, 색상의 재현성(再現性)이 우수하며, 1회의 염색처리로 염색공정이 완료될 뿐만 아니라, 피염물이 소프트한 상태로 염색되도록 하는, 감즙을 이용한 천연염료 제조방법에 관한 것이다.The present invention relates to a natural dye manufacturing method using the juice, more specifically, the juice is produced as a dye, it is possible to uniformly dye the stain, excellent color reproducibility (再現 性), one-time dyeing treatment Not only the dyeing process is completed, but also relates to a natural dye production method using the juice, so that the dye to be stained in a soft state.

피륙을 다양한 색조와 문양으로 염색하는 염재(染材)는 주로 화공약품이 원료이기 때문에, 환경오염의 주범이 되고 있고, 상기 염재로 염색된 직물지를 의복으로 재단하여 입었을 때, 피부병을 유발시키는 등 인체에 유해한 문제점이 있었다.Dyestuffs dyeing the skin in various shades and patterns are mainly chemicals, so they are the main culprit of environmental pollution, and when the fabrics dyed with the dyeing materials are cut with clothing, they cause skin diseases. There was a problem that is harmful to the human body.

이러한 문제점을 해결하기 위해, 최근 들어 각광받고 있는 것이 천연염재이다. 상기 천연염재는 전통적으로 사용되어 온 재료들도 있고, 오가닉(organic) 소재로부터 새롭게 발견된 재료들도 있다.In order to solve this problem, it is natural dyes that are in the spotlight in recent years. The natural salts are traditionally used materials, and some are newly discovered from organic materials.

그 중에서도 감즙을 이용한 염재는 전통적으로 사용되어 오던 것으로서, 기술의 개발 없이 전래의 방법으로 염색되고 있다. 상기 감즙이 천연염재로 일찍부터 사용된 이유는 주위에서 흔하게 구할 수 있는 재료이고, 타닌(tannin) 성분이 많이 함유되어 있기 때문이다. Among them, the salt material using the juice has been used traditionally, it is dyed by conventional methods without the development of technology. The reason why the juice is used early as a natural salt is because it is a material commonly available in the surroundings, and contains a lot of tannin.

최근에 과학적으로 밝혀지고 있지만, 타닌은 염재로서, 일광(日光), 세탁, 마찰에 대한 견뢰도가 높은 것으로 입증되고 있으며, 천연도료로서 단백질 제거능력 및 자외선 차단능력이 탁월한 것으로 알려져 있다. Although recently discovered scientifically, tannin is a salt material, has been proved to have high fastness to daylight, washing, and friction, and is known to have excellent protein removal ability and UV protection ability as a natural paint.

이처럼 타닌 성분이 많이 함유된 감을 이용한 염색 방법을 살펴보면 다음과 같다.The dyeing method using the persimmon containing a lot of tannin components are as follows.

먼저, 감을 착즙하여 감즙을 추출한다. 그리고 상기 감즙을 물에 희석한후, 상기 감즙이 희석된 물에 피염물을 침지한 후, 햇볕에 건조시킨다. 그런데, 한 번의 침지와 건조 단계로서는 색상이 옅기 때문에 원하는 색상을 얻을 때까지 상기 공정을 다수 회 반복한다.First, persimmon is extracted to extract the juice. Then, after diluting the juice in water, the salts are immersed in the diluted water of the juice, and then dried in the sun. However, since the color is light in one immersion and drying step, the process is repeated many times until the desired color is obtained.

이때, 상기 감즙에 포함된 타닌은 일광과 산소에 의해 갈색으로 변하면서 피염물을 물들이게 된다.At this time, the tannins contained in the juice are changed to brown by sunlight and oxygen to color the chlorine.

상기 배경기술에 의하면 다음과 같은 문제점이 있었다.According to the background art, there are the following problems.

상기 감즙에 포함된 타닌(tannin)은 고분자 타닌 중 축합형 타닌으로서 일광과 산소에 의해 산화되면서 응고되는 성질이 있다. 따라서, 피염물의 섬유와 연착되면서 뻣뻣한 질감을 주게 되는 문제점이 있었다. Tannins contained in the juice are condensed tannins of polymer tannins and have a property of being coagulated by oxidation with sunlight and oxygen. Therefore, there is a problem in that the stiff texture is given while being bonded to the fiber of the blood.

또한, 산소와 일광의 조사량(照射量)에 의해 색상이 점점 검어지기 때문에, 일정한 색상을 표현하기가 어려웠다. 즉, 대기에 노출되는 시간 및 일조량 등에 따라 색상이 변하기 때문에, 작업할 때마다 색상이 상이할 뿐만 아니라, 얼룩이 발생하는 문제점이 있어서, 동일한 색상 및 얼룩 없이 균일하게 염색된 직물지를 대량으로 생산할 수 없는 문제점이 있었다. In addition, since the color gradually became black due to the irradiation amount of oxygen and sunlight, it was difficult to express a constant color. That is, since the color changes according to the time and the amount of sunlight exposed to the atmosphere, not only the color is different each time you work, but also there is a problem that a problem occurs, it is impossible to produce a large amount of uniformly dyed fabric paper without the same color and stain There was a problem.

이러한 원인이 발생하는 이유는 감즙에 포함된 타닌이 폴리페놀류를 성분으로 하는 복잡한 구조의 축합형 타닌으로서, 일광, 산소에 의하여 변색 되면서 응고되는 물질이기 때문이다. 즉, 상기 타닌은 염색 시, 섬유의 분자쇄 사이에서 가교화되어 복합체를 형성함으로써, 섬유가 뻣뻣하게 되어 촉감 불량이 초래되고, 얼룩진 염색의 원인이 되고 있다. 이러한 사실은 학계 및 당업계에 이미 공지된 사실로서, 상세한 설명은 생략하는 바이다.The reason for this is because tannins in the juice are condensed tannins with a complex structure containing polyphenols, which are solidified by discoloration by sunlight and oxygen. In other words, the tannins are crosslinked between the molecular chains of the fibers during dyeing to form a complex, resulting in stiffness of the fibers, resulting in poor touch and staining. These facts are already known in the academic world and the art, and detailed descriptions are omitted.

따라서, 상기 타닌의 복잡한 구조를 끊을 경우, 상기 문제점을 해결할 수 있는데, 이를 위해서 감즙을 장기간 저장함으로써 발효를 유발시키는 방법이 사용되고 있지만, 이때 감이 부패하면서 악취를 발생시키고, 균일하게 발효된 감즙을 얻을 수 없으므로 상기 문제점들이 여전히 존재하게 된다.Therefore, when the complex structure of the tannins is broken, the problem can be solved. For this purpose, a method of inducing fermentation by storing the juice for a long time is used, but at this time, the persimmon decays, generates odor and uniformly fermented juice. The problems still exist since they cannot be obtained.

그리고, 일광과 산소에 노출시킴으로써 색상을 조정하기 때문에 침지와 건조 공정을 다수 회 반복해야 함으로써, 시간이 많이 소요되어 생산성이 떨어지는 문제점이 있었다.In addition, since the color is adjusted by exposure to sunlight and oxygen, the immersion and drying processes need to be repeated a plurality of times, resulting in a long time-consuming problem of low productivity.

또한, 감즙을 점성을 구비한 날염용 염료로 사용할 수가 없는 문제점이 있었다.In addition, there was a problem that the juice can not be used as a dye for printing with viscosity.

본 발명에 의한 감즙천연염료 제조방법은, 감즙을 구비하는 감즙구비단계와, 상기 감즙에 프로테아제, 아밀라제 효소를 넣고 온도를 상승시켜가며 발효를 왕성하게 촉진시켜서 감즙에 포함된 타닌을 분해시켜서 고형분이 포함된 타닌추출물이 형성되는 발효단계와, 상기 타닌추출물을 교반하면서 가열하여 알칼리를 투입하여 안정된 타닌조성물을 만드는 교반단계와, 상기 교반단계에 의해 형성된 타닌조성물에 산을 첨가하여 pH를 조정하는 pH 조절단계로 이루어진다. According to the present invention, a method for preparing a natural natural dye is provided with a juice preparation step comprising a juice, and a protease and amylase enzyme are added to the juice to increase the temperature, and vigorously promote fermentation to decompose tannins contained in the juice. A fermentation step in which the tannin extract is formed, a stirring step of heating and stirring the tannin extract to make a stable tannin composition, and a pH to adjust pH by adding an acid to the tannin composition formed by the stirring step. The adjustment step is made.

또한, 상기 발효단계에서 프로테아제, 아밀라제는 상기 감즙 100중량부에 대해서, 0.5∼7중량부이고, 발효가 활성화되도록 온도는 45℃∼90℃로 한다.In addition, the protease, amylase in the fermentation step is 0.5 to 7 parts by weight, based on 100 parts by weight of the juice , the temperature is 45 ℃ to 90 ℃ so that the fermentation is activated.

또한, 상기 교반단계에서 상기 고형분이 포함된 감즙을 20rpm으로 회전하는 교반기에 넣어서 교반하며, 상기 알칼리는 상기 고형분 100중량부에 대해서 0.5∼7중량부의 알칼리를 투입한다. In addition, in the stirring step, the juice containing the solid content is put into a stirrer rotating at 20 rpm and stirred, and the alkali is added 0.5 to 7 parts by weight of alkali based on 100 parts by weight of the solid content.

본 발명에 의한 감즙천연염료는 상기 제조방법에 의해 제조된 것이다.Juicy natural dye according to the present invention is prepared by the above production method.

본 발명에 의한 감즙천연염료를 이용한 염색방법은 원단의 섬유 상에 있는 불순물을 제거하여 중온용 효소로 정련하는 원단전처리단계와, 상기 원단전처리단계를 거친 원단을 상기 청구항 4의 감즙을 물에 희석한 염액에 침지한 후, 온도를 올려가면서 염색하는 염색단계와, 상기 염색단계를 거친 원단을 물로 세척하는 수세처리단계와, 상기 수세처리단계를 거친 원단을 텐터에 장착하여 주름을 제거하는 텐터처리단계가 이루어진다.The dyeing method using a natural natural dye according to the present invention is a fabric pretreatment step of removing impurities on the fibers of the fabric and refining with a medium temperature enzyme, and dilutes the juice of claim 4 with water after the fabric pretreatment step. After immersing in one saline solution, the dyeing step of dyeing while raising the temperature, the washing step of washing the fabric after the dyeing step with water, the tenter treatment to remove the wrinkles by mounting the fabric subjected to the washing step to the tenter Steps are taken.

본 발명에 의하면, 감즙을 통해서 일반 염료처럼 사용할 수 있는 농색의 천연염료이므로, 일반 염료처럼 1회의 염색으로 원하는 색상의 직물지를 얻을 수 있고, 얼룩 없이 고르게 염색될 수 있으므로 재현성이 우수하다. 그리고 종래처럼 침지와 건조를 반복하지 않아도 되기 때문에 신속한 염색 작업이 가능하여 생산효율이 월등하다. 그리고, 날염용 염료로 제조할 경우, 날염용 염료로도 충분히 사용이 가능한 효과가 있다. 따라서, 천연염료로서 대량 생산에 적합한 효과가 있다.According to the present invention, since it is a natural dye of deep color that can be used as a general dye through the juice, it is possible to obtain a textile paper of a desired color by one dyeing like a general dye, and can be dyed evenly without staining, so it is excellent in reproducibility. In addition, since the immersion and drying do not have to be repeated as in the prior art, a rapid dyeing operation is possible, resulting in excellent production efficiency. In addition, when manufacturing with a dye for printing, there is an effect that can be sufficiently used as a dye for printing. Therefore, there is an effect suitable for mass production as a natural dye.

상기 과제를 해결하기 위한 본 발명에 의한, 감즙천연염료의 제조방법 및 감즙천연염료 그리고 감즙천연염료를 이용한 염색방법을 살펴보면 다음과 같다. According to the present invention for solving the above problems, a method of producing a natural natural dye and a natural natural dye and a dyeing method using a natural natural dye are as follows.

상기 과제에서 살펴본 것처럼, 감즙에 함유된 타닌의 문제점들을 해소하기 위해서는 감즙을 저장하여 장기간 발효시킴으로써 가능하다. 이러한 기술은 이미 제주도와 경북 지방에서 예로부터 사용되어 오고 있는 방법으로서 그 효과는 일찌기 알려져 있는 것이다. 그러나, 감즙을 저장하여 발효시킨다고 하더라도 부패가 초래되어 악취가 발생하고 균일하게 발효된 감즙을 얻을 수 없었다. 따라서, 여전히 뻣뻣하고, 얼룩지며, 재현성이 있는 감 염료를 얻을 수 없었다.As discussed in the above problem, in order to solve the problems of tannin contained in the juice is possible by storing the juice for a long time fermentation. This technique has already been used since ancient times in Jeju and Gyeongbuk province, and its effect is known early. However, even when the juice is stored and fermented, decay was caused, and odor was generated, and the fermented juice could not be uniformly obtained. Thus, it was not possible to obtain a sensitizing dye which was still stiff, stained and reproducible.

이에 본 발명에서는 상기 감즙을 효소로 처리하여 축합형 타닌의 복잡한 화학 구조를 깨뜨림으로, 섬유의 분자쇄 사이에서 가교재로서 기능을 못하도록 하고, 미리 농색이 되도록 처리하여 일반 화학염료처럼 1회의 염색 또는 날염으로 제품이 완성되도록 한 것을 특징으로 한다.In the present invention, by treating the juice with an enzyme to break the complex chemical structure of condensed tannins, to prevent the function as a crosslinking material between the molecular chains of the fiber, and to be pre-darkened by one time dyeing or as a general chemical dye It is characterized in that the product is completed by printing.

이를 위하여 본 발명에서는 감즙을 이용한 천연염료 제조방법을 다음과 같이 이루어지도록 한다.To this end, in the present invention, a natural dye production method using the juice is made as follows.

감즙을 구비하는 감즙구비단계가 이루어지고, 상기 감즙구비단계에서 얻어진 감즙에 프로테아제, 아밀라제 효소를 넣고 온도를 상승시켜가며 발효를 왕성하게 촉진시켜서 감즙에 포함된 타닌을 분해시켜서 고형분이 포함된 타닌추출물이 형성되는 발효단계가 이루어지고, 상기 타닌추출물을 교반하면서 가열하여 알칼리를 투입하여 안정된 타닌조성물을 만드는 교반단계가 이루어지고, 상기 교반단계에 의해 형성된 타닌조성물에 산을 첨가하여 pH를 조정하는 pH 조절단계가 이루어진다. 상기 교반단계에서 알칼리를 투입하는 이유는 발효단계로 인해서 형성된 산을 중화시켜서 안정화시키기 위해서이고, 또한, 타닌의 고분자 연결고리를 끊어서 가교화되는 것을 중단시키기 위해서이다. A juice preparation step comprising the juice is made, put the protease, amylase enzyme in the juice obtained in the juice preparation step to increase the temperature and vigorously promote fermentation to decompose tannins contained in the juice tannin extract containing solid content This is a fermentation step is formed, the stirring is heated to stir the tannin extract while stirring to make a stable tannin composition, the pH is adjusted by adding an acid to the tannin composition formed by the stirring step The adjustment stage is made. The reason for adding alkali in the stirring step is to neutralize and stabilize the acid formed by the fermentation step, and to stop crosslinking by breaking the polymer linkage of tannin.

상기 감즙구비단계는 일례로서, 타닌 성분이 가장 많이 함유된 어린 풋감을 구비해서 구연산을 수용액에 넣어서 살균처리한 후, 파쇄하여 압착기로 착즙한다. 그리고 90 메시(mesh) 스크린으로 여과하여 감즙을 제조하게 된다. 본 발명의 감즙구비단계는 상기 방법에만 국한된 것은 아니고, 감즙을 착즙할 수 있는 방법이면 모두 가능하다. 또한, 시중에 유통되는 감즙을 사용하는 것도 가능하다.As an example, the juice preparation step is provided with a young foot containing the highest amount of tannin, sterilized by putting citric acid in an aqueous solution, and then crushed and juiced by a compress. The juice is then prepared by filtration through a 90 mesh screen. The juice preparation step of the present invention is not limited to the above method, any method can be used to juice the juice. It is also possible to use commercially available juices.

상기 발효단계에서 프로테아제, 아밀라제는 일례로 상기 감즙 100중량부에 대해서, 0.5∼7중량부이고, 발효가 활성화되도록 온도는 45℃∼90℃로 하는 것이 바람직하다. 상기 발효단계를 거치게 되면 감즙은 발효에 의해 감즙 100중량부에 대해서 10.0중량부의 고형분이 발생하게 된다. 상기 교반단계에서는 상기 고형분이 포함된 감즙을 20rpm으로 회전하는 교반기에 넣어서 교반하며, 상기 알칼리는 상기 고형분 100중량부에 대해서 0.5∼7중량부의 알칼리를 투입하도록 한다.Protease and amylase in the fermentation step, for example, with respect to 100 parts by weight of the juice , 0.5 to 7 parts by weight , the temperature is preferably 45 ℃ to 90 ℃ so that the fermentation is activated. After the fermentation step, the juice is 10.0 parts by weight of solids based on 100 parts by weight of the juice by fermentation. In the stirring step, the juice containing the solid content is put into a stirrer rotating at 20 rpm, and the alkali is added to 0.5 to 7 parts by weight of alkali based on 100 parts by weight of the solid content.

따라서, 본 발명에서는 감즙을 부패하지 않고 인위적으로 고르게 발효되도록 함으로써, 타닌의 가교화 기능을 못하도록 하여 피염물이 뻣뻣해지는 현상을 방지할 수 있고, 상기 교반단계에서 농색이 되기 때문에 1회의 염색으로 염색공정이 완료될 수 있다.Therefore, in the present invention, by artificially evenly fermenting the juice without decay, it can prevent the crosslinking function of tannins to prevent the stiffness of the chlorine stiffness, because the color is dark in the stirring step, dyeing by one dye The process can be completed.

상기 본 발명의 과학적 근거는 다음과 같다.The scientific basis of the present invention is as follows.

현재 효소를 이용하여 직물을 정련하는 방법이 알칼리 섬유나 산성 섬유에 이용되고 있는데, 일례로 단백질 섬유를 효소 정련하는데 사용하는 프로테아제 중에서 온도와 ph가 맞으면 짧은 시간에 단백질, 세리신 성분을 분해시키는 효소가 있고, 아밀라제 중에도 고온(90℃ 이상)에 견디며 짧은 시간에 가수분해시키는 효소가 있다. 따라서, 복잡한 분자 구조를 가지고 있는 감의 타닌성분도 ph, 온도의 조건이 부합되면 상기 효소에 의해서 안정된 분해가 됨은 물론이다. 따라서, 타닌의 가교화 기능을 못하도록 하여 직물이 뻣뻣해지는 현상을 방지할 수 있다.Currently, a method of refining textiles using enzymes is used for alkali fibers or acidic fibers. For example, among proteases used for enzyme refining protein fibers, enzymes that decompose proteins and sericin in a short time when the temperature and ph are correct Among the amylases, there are enzymes that withstand high temperatures (90 ° C. or more) and hydrolyze in a short time. Therefore, the tannin component of the persimmon having a complex molecular structure is also of course stable decomposition by the enzyme if the conditions of ph, temperature is met. Therefore, it is possible to prevent the crosslinking function of tannins and to prevent the fabric from becoming stiff.

또한, 상기 타닌의 경우는 열을 가할 경우, 축합형이 기본 구조인 flavon-3,4diol의 하이드록실기가 고온처리로 케토형으로 변화하면서 적갈색이나 흑갈색으로 변색되어 색조가 농색이 되기 때문에 일광에 건조하지 않고서도 농색으로 제조가 가능하다.In addition, in the case of the tannin, when the heat is applied, the hydroxyl group of flavon-3,4diol, which is a condensation type basic structure, changes to keto form by high temperature treatment, and the color changes to reddish brown or blackish brown, and the color tone becomes dark. It can be manufactured in deep color without drying.

상기 본 발명이 가능하도록 하는 구체적인 실시예를 살펴보면 다음과 같다.Looking at a specific embodiment to enable the present invention as follows.

(제1실시예)(Embodiment 1)

감즙 100중량부를 구비하는 감즙구비단계가 이루어지고, 프로테아제를 감즙의 2중량부, 아밀라제를 감즙의 3.5중량부를 상기 감즙에 투입하고 40∼60℃의 온도로 12시간 효소반응이 일어나도록 하는 발효단계가 이루어진다. 그리고, 수산화나트륨용액(300g/600㎖)과 붕사용액(32g/100㎖)을 상기 발효단계를 거친 감즙에 넣은 후, 교반기로 20rpm으로 회전시키면서 98℃까지 온도를 상승시키는 교반단계가 이루어진다. 상기 수산화나트륨용액과 붕사용액은 수용액으로서 상기 괄호 속의 분모는 물의 양을 표시한다. 또한, 투입량은 상기 고형분 100중량부에 대해서 0.5∼7중량부로 한다. 그리고, 상기 수산화나트륨용액과 붕사용액의 혼합비는 임의로 정할 수 있으며, 둘의 혼합중량이 0.5∼7중량부이면 무방하다.
이때, 색상은 삼베색에서 황토, 소털색, 흑갈색으로 서서히 변해가면서 소털색상에서 잠시 엉겼다가 이내 묽은 점성을 띠게 된다. 상기 교반단계를 거친 후, 방냉시켜서 50℃로 낮춘 후, 구연산을 감즙 대비 4중량부를 넣고, pH를 7로 맞추도록 하는 pH 조절단계로 이루어진다.
A fermentation step consisting of 100 parts by weight of the juice is made, fermentation of the protease 2 parts by weight of the juice, amylase 3.5 parts by weight of the juice into the juice and the enzymatic reaction takes place for 12 hours at a temperature of 40 ~ 60 ℃ Steps are taken. Then, the sodium hydroxide solution (300g / 600ml) and boric acid solution (32g / 100ml) is put into the juice through the fermentation step, and the stirring step of raising the temperature to 98 ℃ while rotating at 20rpm with a stirrer is made. The sodium hydroxide solution and the borax solution are aqueous solutions, and the denominator in parentheses indicates the amount of water. In addition, the injection amount is 0.5-7 weight part with respect to 100 weight part of said solid content. In addition, the mixing ratio of the sodium hydroxide solution and the boring solution can be arbitrarily determined, and the mixing weight of the two may be 0.5 to 7 parts by weight.
At this time, the color is gradually changed from burlap to ocher, bovine hair, and blackish brown, and then tangled in bovine hair for a while and then becomes thin and viscous. After the stirring step, allowed to cool to lower to 50 ℃, put 4 parts by weight of citric acid per juice , and consists of a pH adjusting step to adjust the pH to 7.

상기 프로테아제(protease)는 일례로 Novozymes사(社)의 Alkalase, Esperase International사(社)의 Purfect 4000G, E에서 선택된 1종을 감즙 대비 2중량부를 투입한다. 또한, 상기 아밀라제는 Basillus 알파-아밀라제(seq-id NO;1∼3)군에서 선택된 1종을 감즙 대비 3.5중량부를 투입함으로써 감즙을 이용한 천연염료가 완성된다.Protease (protease) is an example of Novozymes Inc. Alkalase, Esperase International Inc. Purfect 4000G, E one selected from 2 parts by weight compared to the juice. In addition, the amylase is a natural dye using the juice by adding 3.5 parts by weight of one selected from the group of Basillus alpha-amylase (seq-id NO; 1 to 3) juice.

상기 본 발명에 의해 제조된 천연염료에 의하면, 감즙을 통해서 일반 염료처럼 사용할 수 있는 농색의 천연염료이므로, 일반 염료처럼 1회의 염색으로 원하는 색상의 직물지를 얻을 수 있고, 얼룩 없이 고르게 염색될 수 있으므로 재현성이 우수하다. 그리고 종래처럼 침지와 건조를 반복하지 않아도 되기 때문에 신속한 염색 작업이 가능하여 생산효율이 월등하다. 그리고, 날염용 염료로 제조할 경우, 날염용 염료로도 충분히 사용이 가능한 이점이 있다. 따라서, 천연염료로서 대량 생산에 적합한 특징이 있다.According to the natural dye prepared according to the present invention, since it is a natural dye of deep color that can be used as a general dye through the juice, it is possible to obtain a textile paper of the desired color by one dyeing as a general dye, since it can be dyed evenly without stains Excellent reproducibility In addition, since the immersion and drying do not have to be repeated as in the prior art, a rapid dyeing operation is possible, resulting in excellent production efficiency. In addition, when manufacturing with a dye for printing, there is an advantage that can be sufficiently used as a dye for printing. Therefore, there is a characteristic suitable for mass production as a natural dye.

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본 발명에서는 상기 제조방법에 의해 제조된 감즙천연염료도 본 발명의 권리에 속함은 물론이다. In the present invention, of course, the natural sucrose dyes produced by the above-mentioned manufacturing method also belong to the rights of the present invention.

다음으로 본 발명의 감즙천연염료를 이용한 염색방법을 살펴보면 다음과 같다.Next, look at the dyeing method using a natural dye of the present invention.

원단의 섬유 상에 있는 불순물을 제거하여 중온용 효소로 정련하는 원단전처리단계가 이루어진다. 그리고, 상기 원단전처리단계를 거친 원단을 상기 제조방법에 의한 감즙을 물에 희석한 염액에 침지한 후, 온도를 올려가면서 염색하는 염색단계가 이루어진다. 그리고, 상기 염색단계를 거친 원단을 물로 세척하는 수세처리단계가 이루어지고, 상기 수세처리단계를 거친 원단을 텐터에 장착하여 주름을 제거하는 텐터처리단계가 이루어진다. The fabric pretreatment step is performed by removing impurities on the fabric of the fabric and refining it with a medium temperature enzyme. Then, the fabric after the fabric pretreatment step is immersed in a salt solution diluted in water to the juice by the manufacturing method, the dyeing step of dyeing while raising the temperature is made. Then, a washing step is performed to wash the fabric that has undergone the dyeing step with water, and a tenter treatment step of removing the wrinkles is performed by mounting the fabric that has undergone the washing step in the tenter.

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상기 원단전처리단계에서는 2∼6% OWF(on the weight of fiber), 액비 20∼50배의 상태에서 처리한다. 또한 염색단계에서는 액비 20∼50배로 상기 제조방법에 의한 감즙을 혼합하고, 25∼95℃로 온도를 올려가면서 20∼60분간 염색한다. In the fabric pretreatment step, 2-6% OWF (on the weight of fiber), the liquid ratio of 20 to 50 times. In addition, in the dyeing step, the juice of the manufacturing method is mixed at a liquid ratio of 20 to 50 times and dyed for 20 to 60 minutes while raising the temperature to 25 to 95 ℃.

상기 수세처리단계는 일례로 5회 정도로 반복하여 수세하는 것이 바람직하다.The washing step is preferably repeated washing with about five times.

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Claims (5)

감즙을 구비하는 감즙구비단계와,
상기 감즙에 프로테아제, 아밀라제 효소를 넣고 온도를 상승시켜가며 발효를 촉진시켜서 감즙에 포함된 타닌을 분해시켜서 고형분이 포함된 타닌추출물이 형성되는 발효단계와,
상기 타닌추출물을 교반하면서 가열하여 알칼리를 투입하여 타닌조성물을 만드는 교반단계와,
상기 교반단계에 의해 형성된 타닌조성물에 산을 첨가하여 pH를 조정하는 pH 조절단계로 이루어지는 것을 특징으로 하는 감즙천연염료 제조방법.
Juicy nine stages with a juice,
A fermentation step in which a protease and amylase enzyme are added to the juice, the temperature is increased, and the fermentation is promoted to decompose tannins contained in the juice to form tannin extract containing solids;
Stirring and heating the tannin extract while stirring to make a tannin composition;
Juicy natural dye production method characterized in that the pH adjustment step of adjusting the pH by adding an acid to the tannin composition formed by the stirring step.
제1항에 있어서,
상기 발효단계에서 프로테아제, 아밀라제는 상기 감즙 100중량부에 대해서 0.5∼7중량부이고, 발효가 활성화되도록 온도는 45℃∼90℃로 하는 것을 특징으로 하는 감즙천연염료 제조방법.
The method of claim 1,
Protease, amylase in the fermentation step is 0.5 to 7 parts by weight with respect to 100 parts by weight of the juice, the temperature of the succulent natural dye production method, characterized in that the temperature is set to 45 ℃ to 90 ℃.
제1항 또는 제2항에 있어서,
상기 교반단계에서 상기 고형분이 포함된 감즙을 20rpm으로 회전하는 교반기에 넣어서 교반하며, 상기 알칼리는 상기 고형분 100중량부에 대해서 0.5∼7중량부의 알칼리를 투입하는 것을 특징으로 하는 감즙천연염료 제조방법.
The method according to claim 1 or 2,
In the stirring step, the juice containing the solid content is put into a stirrer to rotate at 20rpm and stirred, wherein the alkali is a method of producing a natural natural dye, characterized in that 0.5 to 7 parts by weight of the alkali is added to 100 parts by weight of the solid content.
상기 청구항 1 또는 청구항 2에 의해 제조된 것을 특징으로 하는 감즙천연염료.Juicy natural dye, characterized in that prepared by claim 1 or 2. 원단의 섬유 상에 있는 불순물을 제거하여 중온용 효소로 정련하는 원단전처리단계와,
상기 원단전처리단계를 거친 원단을 상기 청구항 4의 감즙을 물에 희석한 염액에 침지한 후, 온도를 올려가면서 염색하는 염색단계와,
상기 염색단계를 거친 원단을 물로 세척하는 수세처리단계와,
상기 수세처리단계를 거친 원단을 텐터에 장착하여 주름을 제거하는 텐터처리단계가 이루어지는 것을 특징으로 하는 감즙천연염료를 이용한 염색방법
A fabric pretreatment step of removing impurities on the fabric of the fabric and refining it with a medium temperature enzyme;
A dyeing step of immersing the fabric, which has undergone the fabric pretreatment step, in a saline solution of diluting the juice of claim 4 in water, and then raising the temperature to increase the temperature;
Washing treatment step of washing the fabric after the dyeing step with water,
Dyeing method using a natural succulent dye, characterized in that the tenter treatment step of removing the wrinkles by mounting the fabric subjected to the water washing step in the tenter
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KR101386987B1 (en) 2012-07-04 2014-04-21 주식회사 화수목 kakitannin(sibuol) based on the method for preparing an adhesive resin
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