KR20210124568A - Method of producing water-soluble chitosan non-woven and fiber for manufacturing a mask filter by using the same - Google Patents
Method of producing water-soluble chitosan non-woven and fiber for manufacturing a mask filter by using the same Download PDFInfo
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/30—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with oxides of halogens, oxyacids of halogens or their salts, e.g. with perchlorates
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- A—HUMAN NECESSITIES
- A41—WEARING APPAREL
- A41D—OUTERWEAR; PROTECTIVE GARMENTS; ACCESSORIES
- A41D13/00—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches
- A41D13/05—Professional, industrial or sporting protective garments, e.g. surgeons' gowns or garments protecting against blows or punches protecting only a particular body part
- A41D13/11—Protective face masks, e.g. for surgical use, or for use in foul atmospheres
- A41D13/1192—Protective face masks, e.g. for surgical use, or for use in foul atmospheres with antimicrobial agent
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62B—DEVICES, APPARATUS OR METHODS FOR LIFE-SAVING
- A62B18/00—Breathing masks or helmets, e.g. affording protection against chemical agents or for use at high altitudes or incorporating a pump or compressor for reducing the inhalation effort
- A62B18/02—Masks
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- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62B—DEVICES, APPARATUS OR METHODS FOR LIFE-SAVING
- A62B23/00—Filters for breathing-protection purposes
- A62B23/02—Filters for breathing-protection purposes for respirators
- A62B23/025—Filters for breathing-protection purposes for respirators the filter having substantially the shape of a mask
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D39/00—Filtering material for liquid or gaseous fluids
- B01D39/14—Other self-supporting filtering material ; Other filtering material
- B01D39/16—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres
- B01D39/1607—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous
- B01D39/1615—Other self-supporting filtering material ; Other filtering material of organic material, e.g. synthetic fibres the material being fibrous of natural origin
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- D—TEXTILES; PAPER
- D04—BRAIDING; LACE-MAKING; KNITTING; TRIMMINGS; NON-WOVEN FABRICS
- D04H—MAKING TEXTILE FABRICS, e.g. FROM FIBRES OR FILAMENTARY MATERIAL; FABRICS MADE BY SUCH PROCESSES OR APPARATUS, e.g. FELTS, NON-WOVEN FABRICS; COTTON-WOOL; WADDING ; NON-WOVEN FABRICS FROM STAPLE FIBRES, FILAMENTS OR YARNS, BONDED WITH AT LEAST ONE WEB-LIKE MATERIAL DURING THEIR CONSOLIDATION
- D04H1/00—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres
- D04H1/40—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties
- D04H1/42—Non-woven fabrics formed wholly or mainly of staple fibres or like relatively short fibres from fleeces or layers composed of fibres without existing or potential cohesive properties characterised by the use of certain kinds of fibres insofar as this use has no preponderant influence on the consolidation of the fleece
- D04H1/4282—Addition polymers
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/04—Additives and treatments of the filtering material
- B01D2239/0442—Antimicrobial, antibacterial, antifungal additives
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2239/00—Aspects relating to filtering material for liquid or gaseous fluids
- B01D2239/06—Filter cloth, e.g. knitted, woven non-woven; self-supported material
- B01D2239/0604—Arrangement of the fibres in the filtering material
- B01D2239/0618—Non-woven
Abstract
Description
본 발명은 수용성 키토산 섬유 및 부직포에 관한 것으로서, 더욱 상세하게는 적정 분자량의 키토산섬유 부직포를 묽은 염산용액에 침지후 가수분해한 다음 중화시키고 원하는 분자량으로 10분∼30 동안 별도 반응후 24시간 중화하여 염을 제거하고 열풍건조후 평균분자량 150,000∼300,000의 탈화세틸화도 80%인 수용성 키토산 섬유 및 부직포의 제조방법에 관한 것이다.The present invention relates to water-soluble chitosan fibers and nonwoven fabrics, and more specifically, immersed chitosan fiber nonwoven fabric of an appropriate molecular weight in dilute hydrochloric acid solution, hydrolyzed, and then neutralized, followed by a separate reaction for 10 minutes to 30 minutes at a desired molecular weight, followed by neutralization for 24 hours. It relates to a method for producing a water-soluble chitosan fiber and a nonwoven fabric having an average molecular weight of 150,000 to 300,000 and a degree of cetylation of 80% after removing salt and drying with hot air.
또한, 본 발명은 이렇게 제조된 수용성 키토산 섬유 및 부직포를 70g/㎡∼150g/㎡의 중량으로 0.4g∼0.8g 절단하여 정제수에 넣어 용해시켜서 제조함으로써, 기존 나노필터나 현재 MB 필터의 피부자극 문제나 통기성 문제를 보완할 수 있는 마스크 필터에 관한 것이다.In addition, the present invention is prepared by cutting 0.4 g to 0.8 g of the water-soluble chitosan fiber and nonwoven fabric prepared in this way at a weight of 70 g/m 2 to 150 g/m 2 and dissolving it in purified water. It is about a mask filter that can compensate for the breathability problem.
최근 전세계에 걸쳐 수십만명의 확진자와 사망자 발생을 초래하고 있는 코로나바이러스(SARS-CoV-2)는 호흡기 감염질환의 일종으로서 현재 치료제가 개발되지 않은 상태여서 그 피해규모가 어느정도에 이를지 쉽게 판단이 서지 않을 정도로 인류의 삶과 건강을 심각하게 위협하고 있다. 코로나바이러스는 2019년 12월 중국 우한에서 처음 발생한 이후 중국 전역과 우리나라는 물론 전세계로 확산된 질병으로서, 감염자의 비말이 호흡기나 눈·코·입의 점막으로 침투될 때 전염되고, 감염되면 잠복기를 거친 뒤 발열, 기침, 호흡곤란 등 호흡기 증상이나 폐렴이 주요증상으로 나타나는 것으로 알려져 있다.Coronavirus (SARS-CoV-2), which has recently caused hundreds of thousands of confirmed cases and deaths around the world, is a type of respiratory infection that has not yet been developed, so it is difficult to determine the extent of the damage. It seriously threatens human life and health. Coronavirus is a disease that has spread throughout China and Korea, as well as around the world since it first emerged in Wuhan, China in December 2019. It is known that respiratory symptoms such as fever, cough, and shortness of breath or pneumonia appear as the main symptoms after roughing.
코로나바이러스에 대응하기 위한 방책으로서 중국이나 한국, 일본 등의 아시아 국가들에서는 손씻기와 마스크 착용이 권고되고 있으나, 마스크 착용에 대해 정서적으로 거부감을 갖고 있는 유럽 등의 선진국에서는 마스크 착용이 제대로 이루어지지 않아서인지 코로나바이러스 환자들이 급증하고 있다. 따라서. 최근 유럽국가들에서도 코로나바이러스를 예방하기 위한 방책으로서 마스크착용을 다시 권장하는 추세이다. As a measure to counter the coronavirus, hand washing and wearing a mask are recommended in Asian countries such as China, Korea, and Japan. Cognitive coronavirus cases are on the rise. thus. In recent years, European countries are also re-recommending the use of masks as a measure to prevent coronavirus.
한때 아시아지역은 물론 현재 전세계적으로 제품품귀현상을 겪고 있는 마스크는 코로나바이러스를 예방하기 위한 아주 기초적인 수단으로서 각광받고 있다. 마스크는 미세먼지는 물론 코로나바이러스와 같은 전염성 질병까지 차단이 가능한 것으로서, 제품 포장에 '의약외품'이라는 문자와 함께 KF80, KF94, KF99 등이 표시되어 있다. KF80, KF94, KF99는 입자차단 성능을 나타내는데, KF80은 평균 0.6μm 크기의 미세입자를 80퍼센트 이상 걸러낼 수 있으며, KF94, KF99는 평균 0.4μm 크기의 미세먼지 입자를 94% 및 99%이상 차단한다.Masks, which once experienced a product shortage not only in Asia but also around the world, are in the spotlight as a very basic means to prevent coronavirus. The mask is capable of blocking not only fine dust but also infectious diseases such as coronavirus, and KF80, KF94, KF99, etc. are marked on the product packaging along with the word 'quasi-drug'. KF80, KF94, and KF99 show particle blocking performance. KF80 can filter out more than 80% of fine particles with an average size of 0.6μm, and KF94 and KF99 block 94% and more than 99% of fine dust particles with an average size of 0.4μm. do.
마스크는 핵심 소재인 MB(Melt Blown) 필터는 미세먼지나 바이러스 차단 필터로, 식품의약품안전처의 KF(Korea Filter) 인증 마스크를 만드는 주요 소재 중 하나다. MB필터는 정전기 방식으로 먼지를 잡아내는 방식인데, 장시간 착용하면 입김이 나오면서 정전기 발생 효과가 현저히 떨어지게 된다. 이러한 문제를 개선하기 위해서 개발된 나노필터는 100나노미터급 섬유를 정밀하고 균일하게 짠 나노섬유 구조망인 나노 멤브레인(Nano Membrane)이다. The MB (melt blown) filter, which is a key material for the mask, is a filter that blocks fine dust or viruses, and is one of the main materials for making KF (Korea Filter) certified masks by the Ministry of Food and Drug Safety. The MB filter is an electrostatic method to catch dust, and if worn for a long time, the effect of generating static electricity is significantly reduced as the breath comes out. The nano-filter developed to improve this problem is a nano-membrane, which is a nano-fiber structure in which 100-nanometer-class fibers are woven precisely and uniformly.
MB필터나 나노필터는 모두 부직포를 이용하여 제조되는데, 이는 일정한 굵기와 길이를 가진 섬유를 카딩(carding) 공정을 이용하여 얇고 넓게 펼친 후, 여러 겹으로 겹쳐서 니들펀칭 또는 수류결합 등의 물리적 수단으로 결합시키거나 케미칼 본딩에 의한 화학적 수단으로 결합시켜 제조하게 된다. 부직포는 천연섬유에서부터 화학섬유까지 다양한 섬유들이 이용되고 있지만, 일반적으로 사용하고 있는 것은 면, 레이온, 폴리프로필렌, 폴리프로필렌, 나일론 등이며, 그 외 아크릴, 비닐론, 유리섬유, 펄프, 탄소섬유 등도 사용되고 있다. MB filter and nano filter are all manufactured using non-woven fabric, which is made by stretching a fiber having a certain thickness and length thinly and widely using a carding process, then overlapping it in several layers and using physical means such as needle punching or water flow bonding. It is prepared by bonding or bonding by chemical means by chemical bonding. A variety of fibers are used for non-woven fabrics, from natural fibers to chemical fibers, but those commonly used are cotton, rayon, polypropylene, polypropylene, nylon, etc., and acrylic, vinylon, glass fiber, pulp, carbon fiber, etc. are also used. have.
그런데, 기존의 부직포를 이용하여 제조되는 MB필터나 나노필터는 시간이 경과함에 따라서 에센스가 증발하게 되어 보습 유지력이 떨어지게 되고, 이로 인하여 피부를 자극하여 피부 트러블을 일으키는 문제점이 있었다. 게다가, 통기성이 저하되어 마스크 착용자들이 사용시 불편함을 느끼는 문제점이 있었다. However, the MB filter or nano filter manufactured using the existing nonwoven fabric has a problem in that the essence evaporates over time and the moisture retention power is lowered, thereby stimulating the skin and causing skin troubles. In addition, there is a problem that the breathability is lowered, the mask wearers feel uncomfortable when using.
따라서，본 발명이 해결하고자 하는 기술적 과제는, 적정 분자량의 키토산섬유 부직포를 묽은 염산용액에 침지후 가수분해한 다음 중화시키고 원하는 분자량으로 10분∼30 동안 별도 반응후 24시간 중화하여 염을 제거하고 열풍건조후 평균분자량 150,000∼300,000의 탈화세틸화도 80%인 수용성 키토산 섬유 및 부직포의 제조방법을 제공하려는 것이다.Therefore, the technical problem to be solved by the present invention is to immerse the chitosan fiber nonwoven fabric of an appropriate molecular weight in a dilute hydrochloric acid solution, hydrolyze it, then neutralize it, and then neutralize it for 10 minutes to 30 minutes at the desired molecular weight and then neutralize it for 24 hours to remove the salt An object of the present invention is to provide a method for producing a water-soluble chitosan fiber and a nonwoven fabric having an average molecular weight of 150,000 to 300,000 and a degree of cetylation of 80% after hot air drying.
또한, 본 발명은 이렇게 제조된 수용성 키토산 섬유 및 부직포를 70g/㎡∼150g/㎡의 중량으로 0.4g∼0.8g 절단하여 정제수에 넣어 용해시켜서 제조함으로써, 기존 나노필터나 현재 MB 필터의 피부자극 문제나 통기성 문제를 보완할 수 있는 마스크 필터를 제공하려는 것이다.In addition, the present invention is prepared by cutting 0.4 g to 0.8 g of the water-soluble chitosan fiber and nonwoven fabric prepared in this way at a weight of 70 g/m 2 to 150 g/m 2 and dissolving it in purified water. I am trying to provide a mask filter that can compensate for the air permeability problem.
전술한 바와 같은 기술적 과제를 해결하기 위해서, 본 발명은, In order to solve the technical problem as described above, the present invention,
마스크 제조용 수용성 키토산 섬유 및 부직포의 제조방법으로서,A method for producing water-soluble chitosan fibers and nonwoven fabrics for mask production, the method comprising:
일정 분자량의 키토산 섬유 부직포를 묽은 염산용액에 침지후 가수분해한 다음 중화시켜서 원하는 분자량으로 10분∼30분 동안 별도 반응시키고 24시간 중화하여 염을 제거하고, 열풍건조후 평균분자량 150,000∼300,000의 탈화세틸화도 80%이상인 수용성 부직포로 제조하는 것을 특징으로 하는 마스크 제조용 수용성 키토산 섬유 및 부직포의 제조방법을 제공한다. After immersing a chitosan fiber nonwoven fabric of a certain molecular weight in a dilute hydrochloric acid solution, it is hydrolyzed and then neutralized to react separately for 10 to 30 minutes to the desired molecular weight, neutralized for 24 hours to remove salt, and deoxidized with an average molecular weight of 150,000 to 300,000 after hot air drying It provides a method for producing a water-soluble chitosan fiber and a nonwoven fabric for manufacturing a mask, characterized in that it is prepared with a water-soluble nonwoven fabric having a cetylation degree of 80% or more.
또한, 전술한 바와 같은 기술적 과제를 해결하기 위해서, 본 발명은, 위에서 언급한 제조방법에 의해서 제조된 상기 키토산 섬유 부직포를 70g/㎡∼150g/㎡의 중량으로 0.4g∼0.8g 절단하여 정제수에 넣어 용해시켜서 제조하는 것을 특징으로 하는 마스크 필터를 제공한다. In addition, in order to solve the technical problem as described above, the present invention, the chitosan fiber nonwoven fabric prepared by the above-mentioned manufacturing method is cut by 0.4 g to 0.8 g at a weight of 70 g/m 2 to 150 g/m 2 and added to purified water. It provides a mask filter, characterized in that it is prepared by dissolving it.
이상에서 언급한 바와 같이, 본 발명에 따르면, 인장강도，섬도，신도 등 물리적 특성이 우수한 키토산섬유를 이용하여 키토산섬유 부직포를 제조하고, 이렇게 제조된 키토산섬유 부직포를 이용하여 마스크 필터를 제조함으로써, 기존 나노필터나 현재 MB 필터의 피부자극 문제나 통기성 문제를 완벽하게 보완할 수 있게 된다. As mentioned above, according to the present invention, a chitosan fiber nonwoven fabric is prepared using chitosan fiber having excellent physical properties such as tensile strength, fineness, and elongation, and a mask filter is manufactured using the chitosan fiber nonwoven fabric thus prepared. It will be able to perfectly complement the skin irritation problem and breathability problem of the existing nano filter or MB filter.
도 1은 본 발명의 바람직한 실시 예에 따른 수용성 키토산 섬유 및 부직포의 제조공정도.1 is a manufacturing process diagram of a water-soluble chitosan fiber and a nonwoven fabric according to a preferred embodiment of the present invention.
키토산 섬유는 고순도 천연키토산을 그대로 섬유화하였기 때문에 인체에 무해하고 부작용이 없으며, 항염，항균, 방취 및 면역력 향상 등 키토산의 고유한 기능 때문에 마스크 필터로서 적용해도 아주 좋은 제품이 될 수 있다. 키토산 섬유는 일반적으로 고순도 천연키토산을 용해한 키토산 용액을 방사노즐을 통하여 압출하여 방사한 후 이를 수산화나트륨，황산나트륨，아세트산나트륨 중에서 선택되는 알칼리금속염을 함유하는 알칼리 수용액으로 구성된 응고액 속에서 중화반응에 의해 응고시켜 제조한다.Since chitosan fiber is made of high-purity natural chitosan as it is, it is harmless to the human body and has no side effects. Chitosan fibers are generally produced by extruding and spinning a chitosan solution in which high-purity natural chitosan is dissolved through a spinning nozzle, and then by neutralizing it in a coagulating solution comprising an alkali metal salt selected from sodium hydroxide, sodium sulfate, and sodium acetate. It is prepared by coagulation.
이하, 첨부도면 도 1을 참조하여 본 발명의 바람직한 실시 예에 따른 수용성 키토산 섬유 및 부직포의 제조방법에 대해 상세히 설명한다.Hereinafter, a method for producing a water-soluble chitosan fiber and a nonwoven fabric according to a preferred embodiment of the present invention will be described in detail with reference to the accompanying drawings.
Ι. 키토산 섬유의 제조과정Ι. Manufacturing process of chitosan fiber
수용성 키토산 섬유 및 부직포를 제조하기 위한 전단계로서 다음과 같은 과정을 거쳐서 키토산 섬유를 제조한다.As a pre-step for producing water-soluble chitosan fibers and nonwoven fabrics, chitosan fibers are prepared through the following process.
[고분자원료의 전처리][Pre-treatment of polymer materials]
고분자 원료의 전처리 공정은 원료의 용해력을 향상시키고 또한 고분자의 개질을 위한 것이다. 새우나 게 등의 키틴을 함유한 물질을 5중량%의 염산수용액으로 처리하여 탄산칼슘을 주성분으로 하는 무기 염을 제거한다. 상기 무기염을 제거한 키틴을 5중량%의 수산화나트륨 수용액으로 처리하여 단백질을 제거한다. 상기 단백질을 제거한 키틴을 50중량%의 수산화나트륨 수용액으로 처리하여 키틴 분자내의 아세테이트기(-COCH3)를 제거하여 고순도 키토산을 제조한다(= 단계 S11).The pretreatment process of the polymer raw material is to improve the solubility of the raw material and also to modify the polymer. A substance containing chitin, such as shrimp or crab, is treated with a 5% by weight aqueous hydrochloric acid solution to remove inorganic salts containing calcium carbonate as a main component. The chitin from which the inorganic salt has been removed is treated with a 5% by weight aqueous sodium hydroxide solution to remove the protein. The chitin from which the protein has been removed is treated with a 50% by weight aqueous sodium hydroxide solution to remove the acetate group (-COCH3) in the chitin molecule to prepare high-purity chitosan (= step S11).
[키토산 방사원액의 제조][Preparation of chitosan radiation stock solution]
상기 단계(S11)를 거친 키토산을 용매에 용해시켜 키토산 방사원액을 제조한다(= 단계 S12). 키토산의 용액에서의 함량은 3 내지 30중량%가 바람직하다. 상기 키토산 함량이 3중량% 미만이면 방사원액이 너무 묽고，30중량% 이상이면 점성도가 상승해서 방사가 이루어지지 않는다. The chitosan that has undergone the step (S11) is dissolved in a solvent to prepare a chitosan spinning stock solution (= step S12). The content of chitosan in the solution is preferably 3 to 30% by weight. If the chitosan content is less than 3% by weight, the spinning dope is too thin, and if it is more than 30% by weight, the viscosity increases and spinning is not performed.
용매는 각종 유무기산을 사용할 수 있으나 무기산의 경우 분자량의 저하를 초래할 수 있어，유기산 사용하는 것이 좋으나 가장 좋기로는 젖산을 쓰는 것이 바람직하다. Various organic/inorganic acids may be used as the solvent, but inorganic acids may cause a decrease in molecular weight, so it is preferable to use an organic acid, but it is preferable to use lactic acid.
또한，키토산 용액과 천연약재추출물，폴리감마글루탐산 용액을 3:1:1의 부피비로 공중합시킨 용액을 키토산 방사원액으로 사용할 수도 있다. 폴리감마글루탐산과천연약재추출물의 용액에서의 함량은 3 내지 30중량%가 바람직하다. 폴리감마글루탐산 함량이 3중량% 미만이면 용액이 너무 묽고，30중량% 이상이면 점성도가 상승해서 방사가 이루어지지 않는다.In addition, a solution obtained by copolymerizing a chitosan solution, a natural medicinal extract, and a polygamma-glutamic acid solution in a volume ratio of 3:1:1 may be used as a chitosan radiation stock solution. The content in the solution of polygamma-glutamic acid and natural medicinal herb extract is preferably 3 to 30% by weight. If the polygamma-glutamic acid content is less than 3% by weight, the solution is too dilute, and if it is more than 30% by weight, the viscosity increases and spinning is not performed.
[방사원액의 여과][Filtration of spinning dope]
상기 키토산 방사원액에 글리세롤(glycerol, Sigma) 또는 솔비톨(sorbitol, Sigma)을 가소제로 첨가하여 잘 교반한 후 여과하여 기포를 제거한다(= 단계 S13). 이 여과액은 고점도의 액체로서 방사용 원액(방사 도프(DOPE))로서 적당한 점도(150,000~400,000cps)를 나타낸다.Glycerol (Sigma) or sorbitol (Sigma) is added to the chitosan spinning stock solution as a plasticizer, stirred well, and then filtered to remove air bubbles (= step S13). This filtrate is a high-viscosity liquid and exhibits a suitable viscosity (150,000 to 400,000 cps) as a spinning dope (DOPE).
[방사원액의 방사][Radiation of undiluted solution]
균일한 방사원액(dope)을 방사원액탱크(dope tank)에 이송한다. 이 방사원액을 응고시키기 위하여 정량펌프(gear pump)에 의하여 토출량을 조절하여 노즐을 통하여 방사한다(= 단계 S14). 방사방법은 방사원액을 섬유형성능이 우수함은 물론 섬유끼리의 접사, 용제 제거의 용이，생산성 향상 등의 방사 안정성이 우수한 습식 방사하는 것이 좋다. A uniform dope is transferred to the dope tank. In order to coagulate this spinning dope, the amount of discharge is controlled by a gear pump, and the spinning solution is spun through the nozzle (= step S14). As for the spinning method, it is preferable to wet spinning the spinning undiluted solution with excellent fiber-forming performance, as well as excellent spinning stability, such as attaching fibers to each other, easy solvent removal, and improved productivity.
사용한 노즐은 응고욕이 강알칼리인 관계로 중금속이온을 용출할 수 있는 스테인레스 재질은 피하고 백금/금의 합금재질이 요구된다.Since the used nozzle has a strong alkali coagulation bath, stainless materials that can elute heavy metal ions are avoided, and platinum/gold alloy materials are required.
[응고][coagulation]
상기 방사된 키토산을 응고시키는 공정으로서, 방사된 필라멘트를 응고 고화조인 알칼리수용액 저조，즉 응고욕조(nozzle spinning bath)에서 응고반응(중화반응)을 시켜 키토산 섬유를 제조한다(= 단계 S15).As a process for coagulating the spun chitosan, the spun filaments are subjected to a coagulation reaction (neutralization reaction) in a coagulation and solidification tank, that is, an alkaline aqueous solution bath, that is, a nozzle spinning bath to prepare chitosan fibers (= step S15).
본 발명에서는 규산염과 천연약재추출물 및 허브추출물이 포함된 응고액에서 응고시킨다. 바람직하게는, 1 내지 10중량%의 수산화나트륨 수용액에 10 내지 80중량%의 규산염과 천연약초추출 수용액을 혼합한 완충용액으로 구성된 응고액에서 응고시키는 것이 좋다. In the present invention, it is coagulated in a coagulation solution containing silicate and natural medicinal extracts and herbal extracts. Preferably, it is good to coagulate in a coagulation solution composed of a buffer solution of 1 to 10% by weight of sodium hydroxide aqueous solution mixed with 10 to 80% by weight of silicate and an aqueous solution of natural herbal extracts.
상기 허브추출물은 밀폐된 용기내에서 허브에 물을 붓고 끓이면서 감압법을 이용하여 수증기를 포집하고 이렇게 포집되는 수증기로부터 얻어지는 증류수를 다른 밀폐 용기에 투입된 규산염과 천연약재추출물을 교반할 때 함께 넣어주게 된다. 즉, 종래의 방식에서는 규산염과 천연약재추출물을 교반할 때 보통의 물을 넣어주게 되는데, 본 발명에서는 물 대신에 허브추출물 증류수를 규산염과 천연약재추출물을 교반할 때 넣어줌으로써, 변성이 일어나지 않고 곰팡이 등이 발생하지 않기 때문에 썩지 않는다. 결과적으로, 물성이 원상태 그대로 유지되어 항염효과를 얻을 수 있게 되는 것이다. The herbal extract collects water vapor using a reduced pressure method while pouring water into the herb in a closed container and boiling, and distilled water obtained from the collected water vapor in another sealed container is put together when stirring the silicate and natural medicinal extract. . That is, in the conventional method, ordinary water is added when stirring the silicate and the natural medicinal extract, but in the present invention, distilled water of the herbal extract is added when stirring the silicate and the natural medicinal extract instead of water. It does not rot because the back does not occur. As a result, the physical properties are maintained as they are, so that the anti-inflammatory effect can be obtained.
따라서, 상기 완충용액은 응고시 용액 중의 수소이온농도를 거의 일정하게 유지시키고，pH도 거의 변화시키지 않는다. 이와 같이 완충용액은 산이나 염기를 가해도 용액의 pH를 그다지 변화시키지 않는 능력이 있는데 이런 능력을 완충능이라고 한다. 우수한 완충용액은 또한 조성(組成)을 변화시켜 넓은 pH 영역을 커버할 수도 있다.Therefore, the buffer solution maintains the hydrogen ion concentration in the solution almost constant during coagulation and hardly changes the pH. In this way, the buffer solution has the ability to not change the pH of the solution much even when acid or base is added, and this ability is called buffering capacity. A good buffer can also cover a wide pH range by changing its composition.
규산염과 천연약재추출물이 함유된 완충용액은 가소제 역할도 하여 연신 배 율을 높일 수 있어，섬도 강도 신도를 더욱 좋게 한다.The buffer solution containing silicate and natural medicinal extracts can also increase the draw ratio by acting as a plasticizer, improving fineness, strength and elongation.
응고중 규산염과 천연약재추출물은 키토산섬유를 응고시키는 동시에 규산(Si02)이 부착되어 섬유끼리 달라 붙지(fibrilation) 않고 인장강도가 크게 증가되고 항염 및 항균력 원적외선 방사능도 일반 키토산 섬유에 비해 크게 증가된다.During coagulation, silicate and natural medicinal extracts coagulate chitosan fibers and at the same time, silicic acid (SiO 2 ) is attached, so the fibers do not stick together (fibrilation) and tensile strength is greatly increased. .
이러한 효과는 규산염 및 천연약재추출물이 아닌 다른 어떠한 알칼리 금속염 을 함유하는 수용액에서 응고시키는 것으로는 달성될 수 없는 효과이다. This effect cannot be achieved by coagulating in an aqueous solution containing any alkali metal salt other than silicate and natural medicinal extracts.
응고，고화는 응고과정인 응고욕조에서 30초 내지 1분이내의 짧은 시간에 완료된다.Coagulation and solidification are completed in a short time of 30 seconds to 1 minute in the coagulation bath, which is the coagulation process.
[수세 ·연신][Washing / Stretching]
상기 응고된 키토산 섬유를 수세공정을 통하여 수세를 행하며(= 단계 S16), 이렇게 수세한 키토산 섬유를 비등수 및 스팀공정을 통해 연신하여 연신 섬유를 얻는다(= 단계 S17). The coagulated chitosan fiber is washed with water through a water washing process (= step S16), and the washed chitosan fiber is drawn through a boiling water and steam process to obtain a drawn fiber (= step S17).
연신 욕조의 온도는 연신 온도가 높을수록 연신 비율이 증가하기 때문에, 바람직하게는 80 내지 100℃가 좋으며, 95 내지 100℃로한 후 스팀공정인 130℃로 한번 더 연신한다. 연신배율을 1.0에서 3,5까지 변화하였다.As for the temperature of the stretching bath, since the stretching ratio increases as the stretching temperature increases, preferably 80 to 100° C. is good, and after setting the temperature to 95 to 100° C., stretching is performed once again at 130° C. which is a steam process. The draw ratio was changed from 1.0 to 3,5.
[출하][Shipment]
연신섬유를 후처리 및 건조하여 키토산 섬유를 얻는다(= 단계 S18).The drawn fibers are post-treated and dried to obtain chitosan fibers (= step S18).
Ⅱ. 키토산 부직포 제조과정II. Chitosan Nonwoven Fabric Manufacturing Process
건조하여 얻어진 키토산 섬유를 부직포 형성에 적합한 길이로 절단하여 키토산 단섬유를 제조한 다음, 이를 시트형상으로 결합하여 키토산 섬유 부직포를 제조한다(= 단계 S21). The chitosan fibers obtained by drying are cut to a length suitable for forming a nonwoven fabric to prepare short chitosan fibers, and then combined in a sheet shape to prepare a chitosan fiber nonwoven fabric (= step S21).
적정 분자량의 키토산 섬유 부직포를 묽은 염산용액에 침지후 가수분해한다(=단계 S22). The chitosan fiber nonwoven fabric having an appropriate molecular weight is immersed in a dilute hydrochloric acid solution and then hydrolyzed (=step S22).
다음에는, 원하는 분자량으로 10분∼30분 동안 별도 반응시킨다(=단계 S23). Next, it is separately reacted for 10 to 30 minutes at a desired molecular weight (=step S23).
상기 단계(S23)후에는, 24시간 중화하여 염을 제거한다(=단계 S24). After the step (S23), the salt is removed by neutralization for 24 hours (=step S24).
상기 단계(S24)후에는, 열풍건조하여 평균분자량 150,000∼300,000 탈화세틸화도 80%이상인 수용성 부직포를 제조한다(단계 S25). After the step (S24), hot air drying is performed to prepare a water-soluble nonwoven fabric having an average molecular weight of 150,000 to 300,000 and a degree of de-cetylation of 80% or more (step S25).
결과 및 고찰Results and Discussion
전술한 바와 같은 제조과정을 거쳐서 제조한 키토산 섬유의 인장강도 및 신도의 테스트 결과가 아래 표 1과 같았다. The test results of the tensile strength and elongation of the chitosan fibers manufactured through the manufacturing process as described above are shown in Table 1 below.
다음으로, 하기 표 2는 동국대학교 약학대학 생화약연구실에 의뢰하여 측정한 키토산의 항염효능에 대한 테스트 결과이다.Next, Table 2 below is a test result for the anti-inflammatory effect of chitosan measured by the biochemical laboratory of Dongguk University College of Pharmacy.
이와 같은 테스트 결과를 통해서도 알 수 있듯이, 본 발명에 따라 제조된 키토산 섬유는 규산분(Si02)이 부착되어 있어서 다공성 키토산 섬유의 특징인 인장강도와 신도가 크게 향상되었다. 또한, 우수한 항염성을 나타냄을 알 수 있다. As can be seen from these test results, the chitosan fiber prepared according to the present invention has silicic acid powder (SiO 2 ) attached, so that the tensile strength and elongation, which are characteristics of the porous chitosan fiber, are greatly improved. In addition, it can be seen that exhibits excellent anti-inflammatory properties.
하기 표 3에는 전술한 과정을 거쳐서 제조된 키토산 섬유 및 부직포의 테스트 결과가 나타나 있다. Table 3 below shows the test results of the chitosan fibers and nonwoven fabrics prepared through the above-described process.
하기 표 4에는 본 발명에 따라 제조된 키토산섬유 부직포의 항염효능이 나타나 있다. Table 4 below shows the anti-inflammatory effect of the chitosan fiber nonwoven fabric prepared according to the present invention.
이상에서 설명한 바와 같이, 본 발명에 의해서 제조된 키토산 섬유 부직포는, 마스크 필터로 적용하였을 경우, 기존 마스크 제조에 사용되는 나노필터나 MB 필터의 피부자극이나 통기성의 문제점을 개선할 수 있는 우수한 특성을 나타냄을 알 수 있다.As described above, the chitosan fiber nonwoven fabric manufactured by the present invention has excellent properties that, when applied as a mask filter, can improve skin irritation or air permeability problems of nano filters or MB filters used in conventional mask manufacturing. can be seen to indicate
이상의 설명은 본 발명의 기술적 사상을 예시적으로 설명한 것에 불과한 것으로서, 본 발명이 속하는 기술 분야에서 통상의 지식을 가진 자라면, 본 발명의 본질적 특성을 벗어나지 않는 범위에서 다양한 수정 및 변형이 가능함을 이해할 수 있을 것이다. 따라서, 본 명세서에서 표현된 실시 예는 본 발명의 기술적 사상을 한정하는 것이 아니라, 설명하기 위한 것이고, 이러한 실시 예에 의하여 본 발명의 권리범위가 한정되는 것은 아니다. 본 발명의 보호 범위는 하기 특허청구범위에 의하여 해석되어야 하고, 그와 동등하거나, 균등한 범위 내에 있는 모든 기술적 사상은 본 발명의 권리범위에 포함되는 것으로 해석되어야 할 것이다.The above description is merely illustrative of the technical idea of the present invention, and those of ordinary skill in the art to which the present invention pertains will understand that various modifications and variations are possible without departing from the essential characteristics of the present invention. will be able Therefore, the embodiments expressed in this specification are not intended to limit the technical spirit of the present invention, but to explain, and the scope of the present invention is not limited by these embodiments. The protection scope of the present invention should be construed by the following claims, and all technical ideas equivalent to or within the equivalent range should be construed as being included in the scope of the present invention.
Claims (2)
일정 분자량의 키토산 섬유 부직포를 묽은 염산용액에 침지후 가수분해한 다음 중화시켜서 원하는 분자량으로 10분∼30분 동안 별도 반응시키고 24시간 중화하여 염을 제거하고, 열풍건조후 평균분자량 150,000∼300,000의 탈화세틸화도 80%이상인 수용성 부직포로 제조하는 것을 특징으로 하는 마스크 제조용 수용성 키토산 섬유 및 부직포의 제조방법.A method for producing water-soluble chitosan fibers and nonwoven fabrics for mask production, the method comprising:
After immersing a chitosan fiber nonwoven fabric of a certain molecular weight in a dilute hydrochloric acid solution, it is hydrolyzed and then neutralized to react separately for 10 to 30 minutes to the desired molecular weight, neutralized for 24 hours to remove salt, and deoxidized with an average molecular weight of 150,000 to 300,000 after hot air drying A method for producing a water-soluble chitosan fiber for mask manufacturing and a non-woven fabric, characterized in that it is prepared with a water-soluble nonwoven fabric having a cetylation degree of 80% or more.
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| KR102445210B1 (en) | 2022-02-23 | 2022-09-19 | 김향선 | Method of producing water-soluble chitosan fiber and method of producing chitosan non-woven fabric by using the same |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR101149061B1 (en) | 2010-11-16 | 2012-05-24 | 이수복 | Chitosan non-woven fabric for mask pack material, and method for manufacturing the non-woven fabric |
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| KR101149061B1 (en) | 2010-11-16 | 2012-05-24 | 이수복 | Chitosan non-woven fabric for mask pack material, and method for manufacturing the non-woven fabric |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR102445210B1 (en) | 2022-02-23 | 2022-09-19 | 김향선 | Method of producing water-soluble chitosan fiber and method of producing chitosan non-woven fabric by using the same |
| WO2023163309A1 (en) * | 2022-02-23 | 2023-08-31 | 주식회사 에스유엔생명과학 | Method for preparing water-soluble chitosan fibers and method for manufacturing chitosan nonwoven fabric by using same |
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