KR19990007624A - How to dye natural dyes - Google Patents
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- KR19990007624A KR19990007624A KR1019980042834A KR19980042834A KR19990007624A KR 19990007624 A KR19990007624 A KR 19990007624A KR 1019980042834 A KR1019980042834 A KR 1019980042834A KR 19980042834 A KR19980042834 A KR 19980042834A KR 19990007624 A KR19990007624 A KR 19990007624A
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- 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
- D06P1/00—General 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
- D06P1/34—General 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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- 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
- D06P1/00—General 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
- D06P1/0076—Dyeing with mineral dye
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- 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
- D06P1/00—General 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
- D06P1/36—General 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 mordant dyes ; using metallisable dyes
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Abstract
본 발명은 황토나 맥반석분말 등 광물성염료, 치자나 소목 등의 식물성염료 등 천연염료를 직물에 염색함에 있어 견뢰도를 높이고, 천연염료 특유의 기능성을 나타낼 수 있는 새로운 염색방법에 관한 것으로서, 염색하고자 하는 천연염료는 음이온화제로 처리하여 음이온화시켜 천연염료에 의한 직물의 염색에서 이들 간의 정전기적 이온결합에 의하여 천연염료에 의한 염색의 단점이었던 염색견뢰도를 크게 향상시키면서 또한 천연염료 특유의 자연적인 색상의 발현 및 기능성의 부여 등을 그대로 살릴 수 있도록 한 천연염료의 염색방법을 제공함을 특징으로 한다.The present invention relates to a new dyeing method that can increase the fastness in dyeing the natural dyes, such as mineral dyes such as ocher and elvan rock powder, vegetable dyes such as gardenia or joiner on the fabric, and exhibit the unique functionality of natural dyes, The natural dyes are treated with an anionizing agent and anionized to greatly improve dyeing fastness, which was a disadvantage of dyeing with natural dyes by electrostatic ionic bonding between the dyeings of the fabrics with the natural dyes, It is characterized by providing a dyeing method of natural dyes to enable the expression and impartation of functionality.
따라서, 천연염료를 직물에 염색함에 있어 견뢰도를 높이고, 천연염료 특유의 기능성을 나타낼 수 있는 새로운 염색방법을 제공하며, 그에 따라 우수한 염색효과를 갖는 염색직물을 수득할 수 있는 효과가 있다.Therefore, to increase the fastness in dyeing the natural dyes on the fabric, provides a new dyeing method that can exhibit the unique functionality of the natural dyes, there is an effect that can be obtained a dyeing fabric having an excellent dyeing effect.
Description
본 발명은 천연염료의 염색방법에 관한 것이다. 보다 상세하게는 본 발명은 황토나 맥반석분말 등 광물성염료, 치자나 소목 등의 식물성염료 등 천연염료를 직물에 염색함에 있어 견뢰도를 높이고, 천연염료 특유의 기능성을 나타낼 수 있는 새로운 염색방법에 관한 것이다.The present invention relates to a method for dyeing natural dyes. More specifically, the present invention relates to a new dyeing method that can increase the fastness in dyeing the natural dyes, such as mineral dyes such as ocher and elvan rock powder, vegetable dyes such as gardenia or joiner on the fabric, and exhibit the unique functionality of natural dyes. .
천연염료는 식물성염료, 동물성염료 및 광물성염료들로 대별되며, 자연적으로 수득할 수 있는 것들로서 고래로부터 염료로 널리 사용되어 왔던 것들이다. 천연염료들은 염색물의 색상이 자연스럽고, 합성염료에 비하여 염색물이 인체에 미치는 악영향이 적으며, 환경오염을 덜 유발하고, 폐수처리에 과다한 비용이 소요되지 않는다는 점 등 많은 장점이 있음에도 불구하고, 염료의 생산량이 제한적이고, 염색물의 견뢰도가 불량하며, 염색얼룩이 생기기 쉬운 점 등을 이유로 하여 합성염료의 발전에 따라 점차 그 이용이 줄어들어 현재는 특수한 용도 이외에는 거의 찾아보기 어려운 지경에 이르렀다. 더욱이, 천연염료에 의한 염색은 염료의 산지, 생육환경, 영양상태, 채취시기 등 여러가지 환경변화에 따라 색소성분의 함량이 달라지며, 색소를 추출하는 방법, 염색방법 등에 따라서도 염색물의 색상이 달라지는 등 현대산업이 요구하는 대량생산에는 부적합한 면들이 많아 더욱 공업화가 부진하였다.Natural dyes are roughly divided into vegetable dyes, animal dyes and mineral dyes, which are naturally obtainable and have been widely used as dyes from whales. Natural dyes have many advantages, such as natural color of the dye, less adverse effects on the human body than synthetic dyes, less environmental pollution, and no excessive cost for wastewater treatment. Due to the limited production of dyes, poor fastness of dyes, and easy staining, the use of dyes gradually decreased with the development of synthetic dyes. In addition, the dyeing with natural dyes varies the content of the pigment components according to various environmental changes such as the origin of the dye, growth environment, nutritional status, and harvesting time, and the color of the dyeing material also varies depending on the method of extracting the dye and dyeing method. Many industrial productions were sluggish due to the unsuitable aspects of mass production required by modern industries.
특히, 염색물의 낮은 견뢰도는 가장 극복하기 어려운 문제점으로서 천연염료에 의한 염색의 현대화에 가장 큰 걸림돌이 되고 있다.In particular, the low fastness of the dye is the most difficult problem to overcome is the biggest obstacle to the modernization of dyeing with natural dyes.
그러나, 최근 과학기술이 발달하고, 생산력이 비약적으로 증가하여 섬유제품이 풍부해짐에 따라 최근에 들어 기능성을 중시한 제품, 위생적인 제품 및 건강지향적인 제품들에 대한 요구가 증대하였으며, 이를 위한 부단한 연구결과, 각종 천연염료들 중 기능성을 갖는 염료들이 존재함이 밝혀졌다.However, with the recent development of science and technology and the rapid increase in productivity, the abundance of textile products has increased the demand for functional, hygienic and health-oriented products in recent years. As a result, it was found that there are dyes with functionalities among natural dyes.
예를 들면, 정향, 소목, 석류, 황벽, 울금 등으로 염색한 직물은 향균, 소취성이 우수하다는 결과가 나타나는 것으로 밝혀졌다(섬유기술과 산업, 제 2 권, 제 2 호, 1998년).For example, textiles dyed with clove, joiner, pomegranate, yellow wall, turmeric, etc. have been found to have excellent antibacterial and deodorant properties (Textile Technology and Industry, Vol. 2, No. 2, 1998).
그러나, 천연염료의 염색은 앞서 지적한 바와 같이, 단순히 염액에 염재를 1회 함침시키는 것 또는 수회 반복적으로 함침시키는 것으로 이루어지는 종래의 염색방법으로는 염색이 어렵고, 염색된 염색물의 견뢰도가 낮다는 등의 문제점이 있었으며, 그에 따라 염색의 정도를 직접 관찰하면서 수작업으로 반복하는 것에 의존하여야만 하였으며, 공업화에 커다란 장애가 되었다.However, as mentioned above, the dyeing of the natural dyes is difficult to dye by the conventional dyeing method of simply impregnating the salt solution in the salt solution once or repeatedly repeatedly impregnating, and the fastness of the dyed dye is low. There was a problem, and therefore had to rely on manual repetition while observing the degree of dyeing directly, which was a major obstacle to industrialization.
한편, 섬유와 유기안료 사이에 이온성을 부여하기 위한 이온화제들이 개발되어 상용적으로 공급되고 있으며, 이들 이온화제들은 이온성에 따라 양이온화제(Cationic Agent)와 음이온화제(Anionic Agent)로 대별되며, 양이온화제는 섬유, 특히 면섬유를 구성하는 섬유의 주성분인 셀룰로오스(Cellulose)의 음이온성 관능기와 정전기적으로 결합하여 강한 양이온성을 부여하는 역할을 하며, 음이온화제는 유기안료와 결합하여 역시 강한 이온성을 부여하는 역할을 하며, 이들 양이온화제와 음이온화제들 간의 상호 정전작용에 의하여 섬유와 유기안료간의 결합을 강화시키는 기능을 이용하고 있으나, 이러한 이온화제들의 사용에 의한 섬유의 유기안료 염색방법이 (1) 염색하고자 하는 섬유가 들어있는 제1염욕조내의 약 40℃로 가열된 물에 약 5 중량%의 양이온화제를 투입하고, 약 70℃ 정도로 승온시켜 적어도 10분 이상 유지시킨 후, 냉수로 세정하는 양이온화단계 ; (2) 양이온화제로 처리된 상기 섬유가 들어있는 제2염욕조내의 약 40℃로 가열된 물에 약 12 중량%의 유기안료와 약 1.2 중량%의 음이온화제를 가하고, 적어도 5분 이상 유지한 후, 약 60℃로 가열하고, 약 5분간의 간격으로 4 중량%의 황산마그네슘과 빙초산(pH = 4.5)을 가한 후, 더 가열하여 90℃로 승온시켜 적어도 15분간 유지시킨 후, 수세하는 염색단계 ; (3) 염색처리된 섬유가 들어있는 제3염욕조내의 물을 약 40℃로 가열한 후, 약 2.5 중량%의 포름산나트륨(Formic acid sodium salt)을 가하고, 약 5분의 경과 후 바인더(Binder)를 더 적가하고, 약 10분간 유지하는 고착단계 ; (4) 유기안료가 염색된 섬유를 제3염욕조로부터 인출하여 수세하고, 건조하는 건조단계 ; 및 (5) 욕비가 1 : 5 내지 20 이 되도록 하여 물을 받은 욕조내의 물의 온도를 50 내지 55℃로 조절한 후, 통상의 산-분해효소를 가하여 20 내지 30분간 처리한 후, 열탕처리하여 효소를 비활성화시켜 섬유를 마모처리하고, 계속해서 유연제처리를 하고 건조시키는 후처리단계로 이루어져 있으며, 이러한 종래의 유기안료 염색방법은 3개 또는 그 이상의 염욕조를 사용하여야 하므로 염색에 요구되는 물의 양이 증대되어 폐수의 발생량이 많아지고, 온도를 최고 90℃까지 승온시켜야 하며, 그럼에도 불구하고 견뢰도가 높지 않은 제품을 수득하게 되어 겨우 지스 엘 0801(JIS L 0801), 지스 엘0803(JIS L 0803), 지스 엘0805(JIS L 0805) 및 지스 엘0849(JIS L 0849) 등에 따른 건식 및 습식마찰견뢰도실험에서 지스규격으로 2 내지 3 등급을 나타내는 것으로 밝혀졌다.On the other hand, ionizers for imparting ionicity between fibers and organic pigments have been developed and commercially supplied, and these ionizers are roughly classified into cationic agents and anionic agents depending on the ionicity. The cationic agent electrostatically bonds with the anionic functional group of cellulose (Cellulose), which is the main component of the fibers constituting the fiber, especially cotton fiber, and imparts strong cationicity. It is used to strengthen the bond between the fiber and the organic pigment by mutual electrostatic action between these cationic and anionic agents, but the organic pigment dyeing method of the fiber by the use of these ionizing agents ( 1) First dye bath containing the fibers to be dyed It was added to the cationic agent of about 5% by weight in the heated to about 40 ℃ in the water, and maintained for at least 10 minutes the temperature was raised to about 70 ℃, cationized step of cleaning with cold water; (2) About 12% by weight of organic pigment and about 1.2% by weight of anionic agent are added to the water heated to about 40 ° C. in the second salt bath containing the fiber treated with the cationic agent, and maintained for at least 5 minutes. Thereafter, the mixture was heated to about 60 ° C., and 4% by weight of magnesium sulfate and glacial acetic acid (pH = 4.5) were added at intervals of about 5 minutes, further heated to a temperature of 90 ° C., maintained for at least 15 minutes, followed by step ; (3) After heating the water in the third salt bath containing the dyed fibers to about 40 ℃, about 2.5% by weight of sodium formate (Formic acid sodium salt) is added, after about 5 minutes the binder (Binder) ) Is further added and the fixing step is maintained for about 10 minutes; (4) a drying step of removing the organic pigment-dyed fiber from the third salt bath, washing with water and drying; And (5) the bath ratio is 1: 5 to 20 to adjust the temperature of the water in the bath receiving water to 50 to 55 ℃, and after treatment for 20 to 30 minutes with the addition of a common acid-degrading enzyme, the hot water treatment It consists of a post-treatment step of abrasion treatment of fibers by deactivation of enzymes, subsequent softening treatment, and drying. Since the conventional organic pigment dyeing method requires three or more salt baths, the amount of water required for dyeing This increases the amount of waste water generated, increases the temperature up to 90 ° C., and nevertheless yields a product with low fastness. Only JIS L 0801 and JIS L 0803 In dry and wet friction fastness test according to JIS L 0805 and JIS L 0849 Standards in Scotland was found to exhibit a 2 to 3 star.
더욱이, 이러한 종래의 섬유의 유기안료 염색방법에 의하면, 유기안료들이 섬유의 조직내로 깊숙히 침투하여 표면에서의 염색효과가 저하되고, 충분한 견뢰도를 유지하지 못하며, 마찰견뢰도가 약한 문제점이 있었으며, 따라서 이온화제들을 사용하여 유기안료에 적용되는 방법으로는 천연염료를 염색하는 데에는 적절치 못하여, 천연염료의 염색에는 전혀 활용된 바 없다.Moreover, according to the conventional method of dyeing the organic pigment of the fiber, organic pigments penetrate deeply into the tissue of the fiber, so that the dyeing effect on the surface is lowered, there is a problem that does not maintain sufficient fastness, and has a low friction fastness, thus ions The methods applied to organic pigments using agents are not suitable for dyeing natural dyes, and have never been used for dyeing natural dyes.
따라서, 천연염료를 사용하여 견뢰도가 우수하고, 천연염료 특유의 기능성을 나타낼 수 있는 새로운 염색방법의 개발이 요구되고 있다.Therefore, the development of a new dyeing method that is excellent in color fastness using natural dyes, and can exhibit the unique functionality of natural dyes.
본 발명의 목적은 염색보조제로서 양이온화제와 음이온화제를 사용하여 양이온화제로는 염색될 직물을 처리하고, 음이온화제로는 천연염료를 처리하여 이온결합에 의하여 염색견뢰도를 크게 증대시키도록 한 천연염료의 염색방법을 제공하는 데 있다.An object of the present invention is to treat a fabric to be dyed with a cationic agent using a cationic agent and an anionic agent as a dyeing aid, and a natural dye to treat the natural dye as an anionic agent to greatly increase the color fastness by ionic bonds To provide a method of dyeing.
도 1은 본 발명에 따라 천연염료로서 황토(실시예 1)와 맥반석분말(실시예 2)을 사용하여 염색한 염색직물의 적외선 방사율을 대조군으로서 무처리한 직물(비교예)과 비교하여 나타낸 그래프이다.Figure 1 is a graph showing the infrared emissivity of the dyed fabric dyed using ocher (Example 1) and elvan rock powder (Example 2) as a natural dye according to the present invention compared to the untreated fabric (Comparative Example) as a control to be.
도 2는 본 발명에 따라 천연염료로서 황토(실시예 1)와 맥반석분말(실시예 2)을 사용하여 염색한 염색직물의 적외선 방사율을 대조군으로서 무처리한 직물(비교예)과 비교하여 나타낸 그래프이다.Figure 2 is a graph showing the infrared emissivity of the dyed fabric dyed using ocher (Example 1) and elvan rock powder (Example 2) as a natural dye according to the present invention compared to the untreated fabric (Comparative Example) as a control to be.
도 3은 본 발명에 따라 천연염료로서 황토(실시예 1)와 10%-맥반석분말(실시예 2), 15%-맥반석분말(실시예 3)을 사용하여 염색한 염색직물의 소취율을 대조군으로서 무처리한 직물(비교예)과 비교하여 나타낸 그래프이다.Figure 3 is a natural dye according to the present invention, the control of the deodorization rate of the dyed fabric dyed using ocher (Example 1) and 10%-bedrock stone powder (Example 2), 15%-bedrock stone powder (Example 3) As a graph compared to untreated fabric (Comparative Example).
도 4 내지 도 6은 항균성효과시험결과로서 도 4(비교예), 도 5(실시예 1), 도 6(실시예 2)에 나타낸 균배양사진이다.4 to 6 are microbial culture photographs shown in FIG. 4 (Comparative Example), FIG. 5 (Example 1), and FIG. 6 (Example 2) as results of the antimicrobial effect test.
도 7 내지 도 10은 염색에 사용된 광물성염료가 직물에 부착된 상태를 전자현미경으로 촬영하여 관찰한 결과로서 도 7(비교예), 도 8(실시예 1), 도 9(실시예 2) 및 도 10(실시예 3)에 나타낸 전자현미경사진이다.7 to 10 is a result of observing the state of the mineral dye used for dyeing attached to the fabric by electron microscopy as a result of Figure 7 (Comparative Example), Figure 8 (Example 1), Figure 9 (Example 2) And electron micrograph shown in FIG. 10 (Example 3).
본 발명에 따른 천연염료의 염색방법은, 염색하고자 하는 직물이 들어있는 제1염욕조내에 양이온화제를 투입하고, 가열한 후 수세하는 양이온화단계; 양이온화제로 처리된 상기 직물이 들어있는 제2염욕조내의 물에 음이온화제로 음이온화시킨 천연염료 또는 천연염료와 음이온화제 각각을 개별적으로 가하고, 계속해서 제2염욕조내의 물을 가열, 승온시킨 후, 바인더를 가하고 일정시간 유지한 후, 수세하여 염색하는 염색단계; 및 천연염료가 염색된 섬유를 제2염욕조로부터 인출하여 수세, 탈수 및 건조시키는 후처리단계;로 이루어진다.The dyeing method of the natural dyes according to the present invention, the cationic agent is added to the first salt bath containing the fabric to be dyed, the cationization step of heating and washing with water; To the water in the second salt bath containing the fabric treated with the cationic agent, natural dyes or natural dyes anionized with an anionizing agent and each of the anionizing agents are added separately, followed by heating and heating the water in the second salt bath. Then, after adding a binder and maintaining for a certain time, the dyeing step of dyeing by washing with water; And a post-treatment step of withdrawing the natural dye-dyed fiber from the second salt bath to wash, dehydrate and dry.
이하, 본 발명의 구체적인 실시예를 첨부한 도면을 참조하여 상세히 설명한다.Hereinafter, exemplary embodiments of the present invention will be described in detail with reference to the accompanying drawings.
본 발명에 따른 천연염료의 염색방법은, 염색될 직물을 양이온화제로 처리하여 양이온화시키고, 염색하고자 하는 천연염료는 음이온화제로 처리하여 음이온화시켜 천연염료에 의한 직물의 염색에서 이들 간의 정전기적 이온결합에 의하여 천연염료에 의한 염색의 단점이었던 염색견뢰도를 크게 향상시키면서 또한 천연염료 특유의 자연적인 색상의 발현 및 기능성의 부여 등을 그대로 살릴 수 있도록 한 천연염료의 염색방법을 제공함을 특징으로 한다.In the dyeing method of natural dyes according to the present invention, the fabric to be dyed is cationicized by treating with a cationic agent, and the natural dye to be dyed is anionicized by treating with a negative ionizing agent and thus electrostatically between them in dyeing of the fabric with natural dyes. It provides a method of dyeing natural dyes that greatly improves the color fastness, which is a disadvantage of dyeing with natural dyes by ion bonding, and makes it possible to preserve the natural color expression and functionality of natural dyes. .
상기 양이온화단계에서 사용되는 양이온화제로는 미합중국 소재 센티그레이드 케미칼 인터내셔널(Centigrade Chemical International)사의 상표명 '인덱스(Index)'와 같은 상용적으로 공급되는 양이온화제가 사용될 수 있으며, 이러한 양이온화제는 당해 기술분야에서 통상의 지식을 갖는 자에게는 구입하여 사용할 수 있을 정도로 공지된 것으로 이해될 수 있는 것이다.As the cationic agent used in the cationization step, a commercially supplied cationic agent, such as the trademark 'Index' of Centigrade Chemical International of the United States, may be used. It is to be understood that it is known to those skilled in the art that it can be purchased and used.
상기 양이온화단계는 염색하고자 하는 직물의 종류에 따라 40 내지 60℃의 비교적 저온에서 알칼리를 사용하여 양이온화시키는 저온처리법과, 60℃ 이상의 비교적 고온에서 알칼리의 사용없이 양이온화시키는 고온처리법으로 수행될 수 있다. 상기 저온처리법에서 사용되는 알칼리로는 무수탄산나트륨과 같은 염이 사용될 수 있다. 상기에서 일례로서 언급된 상기 무수탄산나트륨은 당해 기술분야에서는 '소다회(Soda Ash)'로 칭하여지는 것으로서, 당해 기술분야에서 통상의 지식을 갖는 자에게는 극히 용이하게 이해될 수 있는 것임은 자명한 것이다. 상기 저온처리법은 니트류와 같이 성긴 조직을 갖기 때문에 염료의 침투가 쉬운 직물에 주로 적용될 수 있고, 고온처리법은 데님류와 같이 조밀한 조직을 갖기 때문에 염료의 침투가 어려운 직물에 주로 적용될 수 있다.The cationization step may be carried out by a low temperature treatment method for cationization using an alkali at a relatively low temperature of 40 to 60 ° C. and a high temperature treatment method for cationization without using an alkali at a relatively high temperature of 60 ° C. or higher depending on the type of fabric to be dyed. . As the alkali used in the low temperature treatment method, a salt such as anhydrous sodium carbonate may be used. The anhydrous sodium carbonate mentioned as an example in the above is referred to as 'soda ash' in the art, and it is obvious that it can be easily understood by those skilled in the art. The low temperature treatment method may be mainly applied to fabrics that are easy to penetrate dyes because they have a coarse structure, such as knits, and the high temperature treatment method may be mainly applied to fabrics that are difficult to penetrate dyes, since they have a dense structure such as denim.
상기 염색단계에서 사용되는 천연염료로는 염색 전에 음이온화제로 음이온화시킨 것이 사용될 수 있으며, 상기 음이온화제 역시 상기 양이온화제와 마찬가지로 미합중국 소재 센티그레이드 케미칼 인터내셔널(Centigrade Chemical International)사의 상표명 '프리덱스(Predex)나 파인텍스(Finetex)'와 같은 상용적으로 공급되는 음이온화제가 사용될 수 있다. 또한, 염색단계에서 천연염료를 미리 음이온화시키지 아니하고, 천연염료와 음이온화제각각을 개별적으로 염욕조에 투입할 수도 있다.The natural dye used in the dyeing step may be an anionized anionizing agent prior to dyeing, the anionizing agent is also the same as the cationizing agent, the trademark name 'Predex (Centgrade Chemical International) of the United States of America Or commercially available anionizing agents such as " Finetex " may be used. In addition, in the dyeing step, the natural dyes may not be anionized in advance, and each of the natural dyes and the anionizing agent may be separately added to the salt bath.
상기 염색단계에서의 가열에 의한 승온은 염색하고자 하는 천연염료의 종류에 따라 달라질 수 있으며, 50 내지 100℃의 온도범위내에서 가열될 수 있다. 가열의 정도는 주로 천연염료의 열안정성에 의존하여 결정될 수 있다.The temperature increase by heating in the dyeing step may vary depending on the type of natural dye to be dyed, it may be heated within a temperature range of 50 to 100 ℃. The degree of heating can be determined mainly depending on the thermal stability of the natural dyes.
상기 염색단계에서 사용되는 바인더로는 대한민국 소재 정암교역상사에서 상용적으로 공급하고 있는 픽서(Fixer)와 같은 상용적으로 제공되는 것으로서, 특히 염료나 안료의 고착용으로 사용되어 염색견뢰도를 증대시키기 위하여 사용되는 것으로서, 당해 기술분야에서 숙련된 자에게는 용이하게 이해될 수 있는 것이다.The binder used in the dyeing step is commercially provided, such as a fixture (Fixer) commercially supplied by Jeongam Trading Co., Ltd., South Korea in order to increase the color fastness, especially for fixing dyes or pigments As used herein, one of ordinary skill in the art will readily understand.
또한 염색단계에 의하여 염색된 직물은 역시 당해 기술분야에서 통상의 지식을 가진 자에게는 용이하게 이해될 수 있는 매염제처리 등에 의하여 색상조절을 할 수 있다. 매염제는 동일한 염료에 의하여 염색된 경우에서도 발색을 촉진하고, 색소를 섬유에 염착시키는 역할을 하는 것으로서, 천연염료에 의한 염색방법을 제공하는 본 발명에서 사용될 수 있는 매염제로서는 통상의 금속염들이 사용될 수 있으며, 특히 명반(황산알루미늄칼륨), 초산알루미늄, 염화알루미늄 등의 알루미늄매염제나 초산구리나 황산구리와 같은 구리매염제가 주로 사용될 수 있으며, 그외 천연염료의 종류에 따라서는 크롬매염제, 철매염제 또는 주석매염제 등도 사용될 수 있으며, 이들은 모두 당해 기술분야에서 통상의 지식을 가진 자에게는 상용적으로 제공되는 매염제를 구입하여 사용할 수 있을 정도로 공지된 것으로 이해될 수 있다.In addition, the fabric dyed by the dyeing step can also be adjusted by the mordant treatment, etc. can be easily understood by those skilled in the art. The mordant promotes color development even when dyed with the same dye and serves to dye the dye on the fiber. As the mordant that can be used in the present invention which provides a dyeing method using natural dyes, conventional metal salts may be used. In particular, aluminum mordant such as alum (potassium aluminum sulfate), aluminum acetate, aluminum chloride, or copper mordant such as copper acetate or copper sulfate may be mainly used. Other chromium mordant, iron mordant or tin mordant may be used depending on the type of natural dye. It can be understood that they are all known enough to purchase and use mordant commercially available to those of ordinary skill in the art.
상기 후처리단계는 염색업계에서 종사하는 자들에게는 극히 용이하게 이해되는 염색후의 처리들로서 통상의 수세, 탈수 및 건조들로 이루어진다.The post-treatment step is a post-dyeing treatment that is very readily understood by those working in the dyeing industry and consists of conventional washing, dehydration and drying.
상기한 바와 같은 양이온화 및 음이온화에 의하여 천연염료의 사용에 의한 염색에서 단 1회의 함침만으로도 100 내지 500%의 염색농도를 얻을 수 있으며, 직물과 염료간의 결합에 이온결합이 동시에 이루어지기 때문에 제반 견뢰도가 상승되며 직물과의 결합력이 극히 약한 천연염료의 경우에는 보조제로서 가교화제(Cross-linking agent)가 더 사용될 수 있다. 상기 가교화제로서는 아크릴공중합체 또는 폴리우레탄과 같이 당해 기술분야에서 상용화된 가교화제들이 사용될 수 있다.By the above-mentioned cationization and anionization, dyeing concentration of 100 to 500% can be obtained by only one impregnation in dyeing by using natural dyes, and since ionic bonding is simultaneously performed for bonding between fabric and dye, In the case of natural dyes having a high fastness and having a very weak bonding force with a fabric, a cross-linking agent may be further used as an adjuvant. As the crosslinking agent, crosslinking agents commercially available in the art such as acrylic copolymer or polyurethane may be used.
이하에서 본 발명의 바람직한 실시예 및 비교예들이 기술되어질 것이다.Hereinafter, preferred embodiments and comparative examples of the present invention will be described.
이하의 실시예들은 본 발명을 예증하기 위한 것으로서 본 발명의 범위를 국한시키는 것으로 이해되어져서는 안될 것이다.The following examples are intended to illustrate the invention and should not be understood as limiting the scope of the invention.
실시예 1Example 1
광물성염료로서 황토염색을 실시하였다. 우선, 염색될 직물을 상온 내지 40℃의 온도에서 양이온화제와 혼합하여 5 내지 12분 방치한 후, 70℃로 승온시키고, 10분 경과 후, 인출하여 수세하였다. 다음으로, 천연염료로서 사용될 황토염료를 준비하였다. 황토염료는 국내에 널리 존재하는 황토를 채취하여 잡물들을 제거하고, 정선한 황토를 온수에 희석한 것을 사용하였다. 황토염료는 고형분으로서 황토가 15% 포함된 황토염액에 음이온화제를 첨가하여 음이온화시킨 염액에 상기 양이온화된 직물을 담그고 5 내지 10분 경과한 후, 60℃로 승온시켰다. 계속해서, 승온된 온도에서 빙초산 등의 산을 가하여 pH를 4 내지 5로 조절하고, 5 내지 10분 경과 후, 다시 90℃까지 승온시키고, 10분 경과 후, 60 내지 70℃로 냉각시킨 후, 바인더를 가하고, 15분 방치하였다. 염색이 완료된 직물은 인출하여 수세, 탈수 및 건조시켰다.Ocher dyeing was carried out as a mineral dye. First, the fabric to be dyed was mixed with a cationic agent at a temperature of room temperature to 40 ° C, left for 5 to 12 minutes, then heated to 70 ° C, and after 10 minutes, taken out and washed with water. Next, an ocher dye to be used as a natural dye was prepared. The ocher dye was used to remove the miscellaneous by removing the loess widely existing in Korea, and dilute the selected ocher in hot water. The ocher dye was heated to 60 ° C. after 5 to 10 minutes of dipping the cationized fabric in an anionized salt solution by adding an anionizing agent to the ocher salt containing 15% of the ocher as a solid. Subsequently, an acid such as glacial acetic acid was added at an elevated temperature to adjust the pH to 4 to 5, after 5 to 10 minutes elapsed, the temperature was further raised to 90 ° C., after 10 minutes, cooled to 60 to 70 ° C., A binder was added and left to stand for 15 minutes. The dyed fabric was taken out, washed with water, dehydrated and dried.
실시예 2Example 2
고형분으로서 맥반석분말이 10% 포함된 맥반석염액에 음이온화제를 첨가하여 음이온화시킨 염액을 사용하는 것을 제외하고는 상기 실시예 1과 동일하게 수행하여 맥반석염색을 실시하였다.Elvan was stained in the same manner as in Example 1, except that the salt solution was anionized by adding an anionizing agent to the elvan rock salt containing 10% of the elvan rock powder as a solid.
실시예 3Example 3
고형분으로서 맥반석분말이 15% 포함된 맥반석염액에 음이온화제를 첨가하여 음이온화시킨 염액을 사용하는 것을 제외하고는 상기 실시예 1과 동일하게 수행하여 맥반석염색을 실시하였다.Elvan was stained in the same manner as in Example 1, except that the salt solution was anionized by adding an anionic agent to the elvan rock salt containing 15% of the elvan rock powder as a solid.
실시예 4Example 4
식물성염료로서 치자염색을 실시하였다. 우선, 염색될 직물을 상온 내지 40℃의 온도에서 양이온화제와 혼합하여 5 내지 12분 방치한 후, 70℃로 승온시키고, 10분 경과 후, 인출하여 수세하였다. 다음으로, 천연염료로서 사용될 치자염료를 준비하였다. 치자는 꼭두서니과에 속하는 상록활엽관목으로서, 열매로부터 염료를 채취하여 사용한다. 우선, 잘게 부순 치자열매를 물에 완전히 잠길 정도로 붓고 약한 불로 끓여서 염료를 추출한 것을 사용하였다. 추출된 염료로 된 염액에 상기 양이온화된 직물을 담그고 5분 경과한 후, 음이온화제를 투입하고, 다시 5분 경과 후, 60℃로 승온시켰다. 계속해서, 10분 경과 후, 무수탄산나트륨을 가하고, 30분 경과 후, 다시 바인더를 가하고, 15분 방치하였다. 염색이 완료된 직물은 인출하여 수세, 탈수 및 건조시켰다.Gardenia staining was performed as a vegetable dye. First, the fabric to be dyed was mixed with a cationic agent at a temperature of room temperature to 40 ° C, left for 5 to 12 minutes, then heated to 70 ° C, and after 10 minutes, taken out and washed with water. Next, a gardenia dye to be used as a natural dye was prepared. Gardenia japonica is an evergreen broad-leaved shrub belonging to the genus Maldiaceae. First, a finely crushed gardenia fruit was poured into water and boiled over low heat to extract dye. After dipping the cationized fabric in the salt solution of the extracted dye for 5 minutes, the anionizing agent was added, and after 5 minutes, the temperature was raised to 60 ° C. Then, after 10 minutes, anhydrous sodium carbonate was added, after 30 minutes, a binder was added again, and it was left to stand for 15 minutes. The dyed fabric was taken out, washed with water, dehydrated and dried.
실시예 5Example 5
식물성염료로서 소목염색을 실시하였다. 우선, 염색될 직물을 상온 내지 40℃의 온도에서 양이온화제와 혼합하여 5 내지 12분 방치한 후, 70℃로 승온시키고, 10분 경과 후, 인출하여 수세하였다. 다음으로, 천연염료로서 사용될 소목염료를 준비하였다. 소목은 콩과에 속하는 상록교목으로 염색에는 심재를 사용한다. 우선, 잘게 부순 소목심재에 물을 가하고 소량의 식초를 가하여, 끓인 후 걸르기를 2 내지 3회 반복하여 염료를 추출한 것을 사용하였다. 추출된 염료로 된 염액에 상기 양이온화된 직물을 담그고 5분 경과한 후, 음이온화제를 투입하고, 다시 5분 경과 후, 90℃로 승온시켰다. 계속해서, 12분 경과 후, 바인더를 가하고, 15분 방치하였다. 염색이 완료된 직물은 인출하여 수세, 탈수 및 건조시켰다.Joiner staining was performed as a vegetable dye. First, the fabric to be dyed was mixed with a cationic agent at a temperature of room temperature to 40 ° C, left for 5 to 12 minutes, then heated to 70 ° C, and after 10 minutes, taken out and washed with water. Next, a joiner dye to be used as a natural dye was prepared. Joiner is an evergreen tree belonging to the legumes. Heartwood is used for dyeing. First, water was added to a finely crushed timber core, a small amount of vinegar was added, and the mixture was boiled and then filtered twice to three times to extract dye. After dipping the cationized fabric in the salt solution of the extracted dye for 5 minutes, the anionizing agent was added, and after 5 minutes, the temperature was raised to 90 ° C. Subsequently, after 12 minutes, a binder was added and left to stand for 15 minutes. The dyed fabric was taken out, washed with water, dehydrated and dried.
비교예Comparative example
비교예로서는 염색되지 않은 직물원단을 대조군으로 사용하여 각종의 효과를 측정하였다.As a comparative example, various effects were measured using undyed fabric as a control.
우선, 광물성염료에 의한 원적외선방출효과를 측정하였다.First, the far-infrared emission effect by mineral dyes was measured.
원적외선방출효과시험은 실시예 1, 실시예 2 및 비교예에서 각각 취한 샘플을 사용하여 40℃에서, 퓨리에변환-적외선분광분석기(FT-IR Spectrometer ; Fourier Transfer - InfraRed Spectrometer)를 사용하여 흑체(Black body) 대비 측정하여 그 결과를 그래프로 도 1(방사율) 및 도 2(방사에너지)에 나타내었다.Far-infrared emission effect test was carried out using a sample taken in Examples 1, 2 and Comparative Examples, respectively, at 40 ° C., using a Fourier Transfer-InfraRed Spectrometer (FT-IR Spectrometer). body) and the results are shown graphically in Figure 1 (emissivity) and Figure 2 (radiation energy).
또한, 광물성염료에 의한 소취성효과를 측정하였다.In addition, the deodorizing effect of the mineral dye was measured.
항균성효과시험은 균주로서 스타필로코쿠스 아우레우스(Staphylococcus aureus ; ATCC 6538)를 사용하여 KS K 0693의 시험법에 따라 항균도를 측정하였으며, 그 결과를 균감소율 %로 나타내었다. 시험결과의 항균도는 대조군으로서의 비교예가 22.6%를 보이는 반면에, 실시예 1은 41.7%, 실시예 2는 92.7%를 보여주고 있음을 확인할 수 있었다. 이들 항균성효과시험결과로서의 균배양사진을 도 4(비교예), 도 5(실시예 1), 도 6(실시예 2)에 나타내었다.In the antimicrobial effect test, Staphylococcus aureus (Staphylococcus aureus; ATCC 6538) was used to measure the antimicrobial activity according to the test method of KS K 0693, and the result was expressed as percent reduction. The antimicrobial activity of the test results was 22.6% compared to the control as a control, while Example 1 showed 41.7%, Example 2 showed 92.7%. The bacterial culture photographs as the results of these antimicrobial effect tests are shown in Fig. 4 (Comparative Example), Fig. 5 (Example 1), and Fig. 6 (Example 2).
또한, 암모니아가스가 들어있는 용기내에 시험편을 노출시켜, 흡수되고 남은 양을 시간의 경과에 따라 측정하여 냄새흡수율을 측정한 소취성시험에서도 도 3에 그래프로 나타낸 바와 같이, 비교예가 시간 경과에 따라 30 내지 40%에 불과한 반면에, 실시예 1은 83 내지 86%, 실시예 2는 63 내지 69%, 실시예 3은 78 내지 80%에 달하는 높은 소취율을 보임을 확인할 수 있었다.In addition, in the deodorizing test in which the test piece was exposed in a container containing ammonia gas, and the amount absorbed and absorbed was measured over time, and the odor absorption rate was measured, as shown in the graph of FIG. While only 30 to 40%, Example 1 was 83 to 86%, Example 2 was 63 to 69%, Example 3 was found to show a high deodorization rate of 78 to 80%.
염색에 사용된 광물성염료가 직물에 부착된 상태를 전자현미경으로 촬영하여 관찰한 결과를 각각 도 7(비교예), 도 8(실시예 1), 도 9(실시예 2) 및 도 10(실시예 3)에 나타내었으며, 부착성이 양호함을 확인할 수 있었다.7 (comparative example), FIG. 8 (example 1), FIG. 9 (example 2), and FIG. 10 (execution) of the mineral dyes used for dyeing were photographed and observed by electron microscopy. It was shown in Example 3), it was confirmed that the adhesion is good.
또한, 견뢰도시험에서도 KS K 0430에 따른 세탁견뢰도에서 본 발명에 따른 실시예들은 4 내지 5등급의 견뢰도를, KS K 0650에 따른 마찰견뢰도에서는 3 내지 4등급의 견뢰도를 그리고 KS K 0700에 따른 일광견뢰도에서도 3 내지 4등급의 견뢰도를 나타내어 견뢰도가 매우 우수하게 나타남을 확인할 수 있었다.In addition, in the fastness test according to the present invention in the color fastness to washing according to KS K 0430, the fastnesses of 4 to 5 grades, the fastness of 3 to 4 grades of friction fastness according to KS K 0650 and daylight according to KS K 0700 In the fastness also showed a fastness of 3 to 4 ratings was confirmed that the fastness is very excellent.
따라서, 본 발명에 의하면 천연염료를 직물에 염색함에 있어 견뢰도를 높이고, 천연염료 특유의 기능성을 나타낼 수 있는 새로운 염색방법을 제공하며, 그에 따라 우수한 염색효과를 갖는 염색직물을 수득할 수 있는 효과가 있다.Therefore, the present invention provides a new dyeing method that can increase the fastness in dyeing the natural dyes on the fabric, and can exhibit the unique functionality of the natural dyes, accordingly has the effect of obtaining a dyeing fabric having an excellent dyeing effect have.
이상에서 본 발명은 기재된 구체예에 대해서만 상세히 설명되었지만 본 발명의 기술사상 범위 내에서 다양한 변형 및 수정이 가능함은 당업자에게 있어서 명백한 것이며, 이러한 변형 및 수정이 첨부된 특허청구범위에 속함은 당연한 것이다.Although the present invention has been described in detail only with respect to the described embodiments, it will be apparent to those skilled in the art that various modifications and variations are possible within the technical scope of the present invention, and such modifications and modifications are within the scope of the appended claims.
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