KR102534123B1 - Polyester yarn containing graphene oxide - Google Patents

Polyester yarn containing graphene oxide Download PDF

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KR102534123B1
KR102534123B1 KR1020220104883A KR20220104883A KR102534123B1 KR 102534123 B1 KR102534123 B1 KR 102534123B1 KR 1020220104883 A KR1020220104883 A KR 1020220104883A KR 20220104883 A KR20220104883 A KR 20220104883A KR 102534123 B1 KR102534123 B1 KR 102534123B1
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graphene oxide
polyester
weight
polyester yarn
containing graphene
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KR1020220104883A
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Korean (ko)
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김헌상
이기주
이대원
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주식회사 네오엔프라
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    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/08—Melt spinning methods
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D01F1/103—Agents inhibiting growth of microorganisms
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F1/00—General methods for the manufacture of artificial filaments or the like
    • D01F1/02—Addition of substances to the spinning solution or to the melt
    • D01F1/10—Other agents for modifying properties
    • D01F1/106—Radiation shielding agents, e.g. absorbing, reflecting agents
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
    • D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2331/00—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products
    • D10B2331/04—Fibres made from polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds, e.g. polycondensation products polyesters, e.g. polyethylene terephthalate [PET]
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00—Physical properties
    • D10B2401/06—Load-responsive characteristics
    • D10B2401/061—Load-responsive characteristics elastic
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00—Physical properties
    • D10B2401/06—Load-responsive characteristics
    • D10B2401/063—Load-responsive characteristics high strength
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00—Physical properties
    • D10B2401/13—Physical properties anti-allergenic or anti-bacterial
    • D—TEXTILES; PAPER
    • D10—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B—INDEXING SCHEME ASSOCIATED WITH SUBLASSES OF SECTION D, RELATING TO TEXTILES
    • D10B2401/00—Physical properties
    • D10B2401/16—Physical properties antistatic; conductive

Abstract

본 발명은 산화그래핀이 함유된 폴리에스터 원사에 관한 것으로, 더욱 상세하게는 폴리에스터 및 폴리에스터용 산화그래핀 마스터 배치 조성물로 이루어진다.
상기와 같이 산화그래핀이 함유된 폴리에스터 원사는 원적외선 방출 및 항균성능이 부가될 뿐만 아니라, 윤활성, UV 차단성, 전기전도성 및 방열특성을 나타내며, 내스크래치성, 내마모성, 인장강도, 굴곡강도 및 굴곡탄성율 등과 같은 기계적 물성이 향상된 폴리에스터 원사를 제공한다.The present invention relates to a polyester fiber containing graphene oxide, and more particularly, consists of polyester and a graphene oxide master batch composition for polyester.
As described above, the polyester yarn containing graphene oxide not only emits far-infrared rays and has antibacterial performance, but also exhibits lubricity, UV blocking, electrical conductivity and heat dissipation, and exhibits scratch resistance, abrasion resistance, tensile strength, flexural strength and It provides a polyester yarn with improved mechanical properties such as flexural modulus.

Description

산화그래핀이 함유된 폴리에스터 원사 {POLYESTER YARN CONTAINING GRAPHENE OXIDE}Polyester yarn containing graphene oxide {POLYESTER YARN CONTAINING GRAPHENE OXIDE}

본 발명은 산화그래핀이 함유된 폴리에스터 원사에 관한 것으로, 더욱 상세하게는 산화그래핀이 함유되어 원적외선 방출 및 항균성능이 부가될 뿐만 아니라, 윤활성, UV 차단성, 전기전도성 및 방열특성을 나타내며, 내스크래치성, 내마모성, 인장강도, 굴곡강도 및 굴곡탄성율 등과 같은 기계적 물성이 향상된 폴리에스터 원사에 관한 것이다.The present invention relates to a polyester fiber containing graphene oxide, and more particularly, contains graphene oxide, which not only emits far-infrared rays and has antibacterial performance, but also exhibits lubricity, UV blocking, electrical conductivity and heat dissipation characteristics. , It relates to a polyester yarn with improved mechanical properties such as scratch resistance, abrasion resistance, tensile strength, flexural strength and flexural modulus.

합성섬유의 경우 천연섬유에 비해 기계적 물성은 우수하지만, 흡수 능력이 적기 때문에, 인체에서 분비되는 땀 및 각종 유기물이 부착되어 세균 및 곰팡이류 등의 미생물 서식에 적합한 환경을 제공하게 되고 이러한 미생물의 번식으로 악취, 섬유제품의 변색 및 오염, 심지어는 인체의 감염으로 인한 질병을 일으키기도 한다. 이러한 이유로 예전부터 섬유재료에 인체에 유해한 균의 증식을 억제하는 기능을 부여하고자 하는 많은 시도가 이루어지고 있다.In the case of synthetic fibers, they have excellent mechanical properties compared to natural fibers, but have low absorption capacity, so sweat and various organic substances secreted from the human body are attached to provide an environment suitable for the habitat of microorganisms such as bacteria and fungi. It can cause odor, discoloration and contamination of textile products, and even diseases caused by human infection. For this reason, many attempts have been made to impart a function of suppressing the proliferation of bacteria harmful to the human body to fiber materials from the past.

또한, 마스터 배치(Master batch)란, 화학섬유를 비롯한 석유화학 관련 공산품의 제조 시에 이들에 각종 필요한 기능성을 부여하기 위하여 첨가제 등의 기능성 배합제를 고농도로 혼합하고, 배합제의 쏠림 현상을 방지하기 위하여 분산제를 사용한 고농축 기능성 수지를 말한다.In addition, a master batch is a mixture of functional compounding agents such as additives at high concentration in order to give various necessary functionalities to them during the manufacture of petrochemical-related industrial products, including chemical fibers, and preventing the blending agent from leaning It refers to a highly concentrated functional resin using a dispersant to do so.

한편, 그래핀은 탄소원자들이 벌집모양의 육각형을 형성하며 공유결합으로 연결된 단원자층 2차원 소재로 기존의 소재들의 근본적인 한계를 극복할 수 있는 열적, 기계적, 전기적, 광학적 특성을 지녀 배리어 코팅소재, 초경량 고강도 복합재 등 다양한 산업 분야들에 무한한 응용 가능성을 가지고 있다.On the other hand, graphene is a monoatomic two-dimensional material in which carbon atoms form a honeycomb-shaped hexagon and are covalently connected. It has thermal, mechanical, electrical, and optical properties that can overcome the fundamental limitations of existing materials. It has infinite application possibilities in various industrial fields such as ultra-light and high-strength composite materials.

하지만, 무결점 그래핀은 그래핀 간의 반데르발스힘에 의해 고분자 수지 및 유기용매 안에서 균일한 분산이 어렵기 때문에 코팅소재 및 고성능 기능성 복합재를 제조하기 어렵고 실제 적용 가능한 기술에 대한 연구가 매우 제한적인 실정이다. 이러한 그래핀의 분산 문제점을 해결하고자 그래핀 산화물의 다양한 기능기을 활용한 표면개질 연구가 활발히 진행되고 있다. 그런데 이러한 연구들은 고온의 반응열, 낮은 재현성, 대량생산의 부적합등과 같은 문제점이 발생되어 이에 대한 개선이 요구되고 있다.However, since it is difficult to uniformly disperse defect-free graphene in polymer resins and organic solvents due to the van der Waals force between graphenes, it is difficult to manufacture coating materials and high-performance functional composites, and research on practically applicable technologies is very limited. am. In order to solve the dispersion problem of graphene, research on surface modification using various functional groups of graphene oxide is being actively conducted. However, these studies have problems such as high temperature reaction heat, low reproducibility, and unsuitability for mass production, and improvement is required.

한국특허등록 제10-1975955호(2019.04.30)Korean Patent Registration No. 10-1975955 (2019.04.30) 한국특허등록 제10-2163232호(2020.09.29)Korean Patent Registration No. 10-2163232 (2020.09.29)

본 발명의 목적은 산화그래핀이 함유되어 원적외선 방출 및 항균성능이 부가될 뿐만 아니라, 윤활성, UV 차단성, 전기전도성 및 방열특성을 나타내며, 내스크래치성, 내마모성, 인장강도, 굴곡강도 및 굴곡탄성율 등과 같은 기계적 물성이 향상된 폴리에스터 원사를 제공하는 것이다.The purpose of the present invention is to contain graphene oxide to provide far-infrared emission and antibacterial performance, as well as to exhibit lubricity, UV blocking, electrical conductivity and heat dissipation, scratch resistance, abrasion resistance, tensile strength, flexural strength and flexural modulus. It is to provide a polyester yarn with improved mechanical properties, such as the like.

본 발명의 목적은 폴리에스터 및 폴리에스터용 산화그래핀 마스터 배치 조성물로 이루어지는 것을 특징으로 하는 산화그래핀이 함유된 폴리에스터 원사를 제공함에 의해 달성된다.An object of the present invention is achieved by providing a polyester yarn containing graphene oxide, characterized in that it consists of polyester and a graphene oxide master batch composition for polyester.

본 발명의 바람직한 특징에 따르면, 상기 산화그래핀이 함유된 폴리에스터 원사는 폴리에스터 100 중량부에 폴리에스터용 산화그래핀 마스터배치 조성물 0.05 내지 0.2 중량부로 이루어지는 것으로 한다.According to a preferred feature of the present invention, the polyester fiber containing graphene oxide is composed of 0.05 to 0.2 parts by weight of a graphene oxide master batch composition for polyester based on 100 parts by weight of polyester.

본 발명의 더 바람직한 특징에 따르면, 상기 폴리에스터용 산화그래핀 마스터 배치 조성물은 폴리에스터 99 내지 99.9 중량% 및 산화그래핀 분산액 0.1 내지 1 중량%로 이루어지는 것으로 한다.According to a more preferred feature of the present invention, the graphene oxide master batch composition for polyester is composed of 99 to 99.9% by weight of polyester and 0.1 to 1% by weight of a graphene oxide dispersion.

본 발명의 더욱 바람직한 특징에 따르면, 상기 산화그래핀 분산액은 이온수 100 중량부, 그래핀 0.1 내지 1 중량부, 중화제 0.07 내지 0.7 중량부 및 분산제 0.05 내지 0.5 중량부로 이루어지는 것으로 한다.According to a more preferred feature of the present invention, the graphene oxide dispersion is composed of 100 parts by weight of ionized water, 0.1 to 1 part by weight of graphene, 0.07 to 0.7 parts by weight of a neutralizer, and 0.05 to 0.5 parts by weight of a dispersing agent.

본 발명의 더욱 더 바람직한 특징에 따르면, 상기 중화제는 스테아린계 및 아민계로 이루어진 그룹에서 선택된 하나 이상으로 이루어지는 것으로 한다.According to a more preferred feature of the present invention, the neutralizing agent is made of at least one selected from the group consisting of stearin-based and amine-based.

본 발명의 더욱 더 바람직한 특징에 따르면, 상기 분산제는 아민계 및 스테아르산계로 이루어진 그룹에서 선택된 하나 이상으로 이루어지는 것으로 한다.According to a more preferred feature of the present invention, the dispersant is made of at least one selected from the group consisting of amines and stearic acids.

본 발명에 따른 산화그래핀이 함유된 폴리에스터 원사는 산화그래핀이 함유되어 원적외선 방출 및 항균성능이 부가될 뿐만 아니라, 윤활성, UV 차단성, 전기전도성 및 방열특성을 나타내며, 내스크래치성, 내마모성, 인장강도, 굴곡강도 및 굴곡탄성율 등과 같은 기계적 물성이 향상되는 탁월한 효과를 나타낸다.The polyester fiber containing graphene oxide according to the present invention not only emits far-infrared rays and has antibacterial performance because graphene oxide is contained, but also exhibits lubricity, UV blocking, electrical conductivity and heat dissipation, and exhibits scratch resistance and abrasion resistance. , shows excellent effects of improving mechanical properties such as tensile strength, flexural strength and flexural modulus.

도 1은 본 발명의 실시예 1을 통해 제조된 산화그래핀이 함유된 폴리에스터 원사를 촬영하여 나타낸 사진이다.
도 2는 본 발명의 실시예 1을 통해 제조된 산화그래핀이 함유된 폴리에스터 원사의 중금속 함유여부를 측정하여 나타낸 시험성적서이다.
도 3 내지 4는 본 발명의 실시예 1을 통해 제조된 산화그래핀이 함유된 폴리에스터 원사와 상기 비교예 1을 통해 제조된 폴리에스터 원사로 티셔츠와 양말을 제조한 후에 열감효과를 측정하여 나타낸 사진이다.
도 5는 본 발명의 실시예 1을 통해 제조된 산화그래핀이 함유된 폴리에스터 원사의 자외선 차단효과를 측정하여 나타낸 시험성적서이다.
도 6 내지 7은 본 발명의 실시예 1을 통해 제조된 산화그래핀이 함유된 폴리에스터 원사의 마찰대전성과 항균성을 측정하여 나타낸 시험성적서이다.
도 8은 본 발명의 실시예 1을 통해 제조된 산화그래핀이 함유된 폴리에스터 원사의 항바이러스성능을 측정하여 나타낸 시험성적서이다.
도 9는 본 발명의 실시예 1을 통해 제조된 산화그래핀이 함유된 폴리에스터 원사의 세탁견뢰도를 측정하여 나타낸 시험성적서이다.1 is a photograph showing a polyester yarn containing graphene oxide prepared in Example 1 of the present invention.
2 is a test report showing the presence or absence of heavy metals in the polyester yarn containing graphene oxide prepared in Example 1 of the present invention.
3 to 4 are graphene oxide-containing polyester yarns prepared in Example 1 of the present invention and polyester yarns prepared in Comparative Example 1, after manufacturing T-shirts and socks, and showing the thermal effect measured. It is a picture.
5 is a test report showing the measurement of the UV blocking effect of the polyester yarn containing graphene oxide prepared in Example 1 of the present invention.
6 to 7 are test reports showing the triboelectricity and antibacterial properties of polyester yarn containing graphene oxide prepared in Example 1 of the present invention.
8 is a test report showing the antiviral performance of polyester yarn containing graphene oxide prepared in Example 1 of the present invention.
9 is a test report showing the measurement of wash fastness of polyester yarn containing graphene oxide prepared in Example 1 of the present invention.

이하에는, 본 발명의 바람직한 실시예와 각 성분의 물성을 상세하게 설명하되, 이는 본 발명이 속하는 기술분야에서 통상의 지식을 가진 자가 발명을 용이하게 실시할 수 있을 정도로 상세하게 설명하기 위한 것이지, 이로 인해 본 발명의 기술적인 사상 및 범주가 한정되는 것을 의미하지는 않는다.Hereinafter, a preferred embodiment of the present invention and the physical properties of each component will be described in detail, but this is to be explained in detail so that a person having ordinary knowledge in the art to which the present invention belongs can easily practice the invention, This is not meant to limit the technical spirit and scope of the present invention.

본 발명에 따른 산화그래핀이 함유된 폴리에스터 원사는 폴리에스터 및 폴리에스터용 산화그래핀 마스터 배치 조성물로 이루어지며, 폴리에스터 100 중량부에 폴리에스터용 산화그래핀 마스터배치 조성물 0.05 내지 0.2 중량부를 혼합하여 이루어지는 것이 바람직하다.The polyester fiber containing graphene oxide according to the present invention is made of polyester and a graphene oxide master batch composition for polyester, and 0.05 to 0.2 parts by weight of the graphene oxide master batch composition for polyester is added to 100 parts by weight of polyester. It is preferable to mix them.

상기 폴리에스터용 산화그래핀 마스터 배치 조성물은 0.05 내지 0.2 중량부가 함유되며, 폴리에스터 99 내지 99.9 중량% 및 산화그래핀 분산액 0.1 내지 1 중량%로 이루어진다.The graphene oxide master batch composition for polyester contains 0.05 to 0.2 parts by weight, and is composed of 99 to 99.9% by weight of polyester and 0.1 to 1% by weight of a graphene oxide dispersion.

상기의 성분으로 이루어지는 폴리에스터용 산화그래핀 마스터 배치 조성물은 폴리에스터에 혼합되어 윤활성, UV 차단성, 전기전도성 및 방열특성등의 기능성을 부여할 뿐만 아니라. 내스크래치성, 내마모성, 인장강도, 굴곡강도 및 굴곡탄성율 등과 같은 기계적 물성이 향상된 폴리에스터 원사가 제공될 수 있도록 하는 역할을 한다.The graphene oxide master batch composition for polyester comprising the above components is mixed with polyester to impart functionality such as lubricity, UV blocking, electrical conductivity and heat dissipation. It serves to provide a polyester yarn with improved mechanical properties such as scratch resistance, abrasion resistance, tensile strength, flexural strength and flexural modulus.

상기 산화그래핀 마스터 배치 조성물의 함량이 0.05 중량부 미만이면 상기의 효과가 미미하며, 상기 산화그래핀 마스터 배치 조성물의 함량이 0.2 중량부를 초과하게 되면 상기의 효과는 크게 향상되지 않으면서 제조비용을 지나치게 증가시킬 뿐만 아니라, 폴리에스터의 기계적 물성 등이 오히려 저하될 수 있다.If the content of the graphene oxide master batch composition is less than 0.05 parts by weight, the above effects are insignificant, and if the content of the graphene oxide master batch composition exceeds 0.2 parts by weight, the above effects are not greatly improved and the manufacturing cost is reduced. In addition to excessive increase, the mechanical properties of polyester may rather deteriorate.

이때, 상기 산화그래핀 마스터 배치 조성물에 함유되는 산화그래핀 분산액은 이온수 100 중량부, 그래핀 0.1 내지 1 중량부, 중화제 0.07 내지 0.7 중량부 및 분산제 0.05 내지 0.5 중량부로 이루어지는데, 상기의 성분으로 이루어지는 산화그래핀 분산액의 함량이 0.1 중량% 미만이면 상기의 효과가 미미하며, 상기 산화그래핀 분산액의 함량이 1 중량%를 초과하게 되면 상기의 효과는 크게 향상되지 않으면서 폴리에스터 원사의 기계적 물성이 저하되며, 제조비용을 지나치게 증가시키게 된다.At this time, the graphene oxide dispersion contained in the graphene oxide master batch composition is composed of 100 parts by weight of ionized water, 0.1 to 1 part by weight of graphene, 0.07 to 0.7 parts by weight of a neutralizer, and 0.05 to 0.5 parts by weight of a dispersant. If the content of the graphene oxide dispersion is less than 0.1% by weight, the above effect is insignificant, and if the content of the graphene oxide dispersion exceeds 1% by weight, the above effect is not greatly improved and the mechanical properties of the polyester yarn This decreases, and the manufacturing cost is excessively increased.

상기 이온수는 흑연에서 박리된 나노수준의 얇은 판상형인 그래핀을 중화하는 역할을 하며, 상기 그래핀은 50 내지 500 나노미터 수준의 얇은 판상형을 사용하는 것이 바람직하다.The ionized water serves to neutralize graphene, which is a nano-level thin plate-like graphene exfoliated from graphite, and it is preferable to use a thin plate-like graphene of 50 to 500 nanometers.

또한, 상기 중화제는 0.07 내지 0.7 중량부가 함유되며, 스테아린계 및 아민계로 이루어진 그룹에서 선택된 하나 이상으로 이루어지는데, 상기의 산화그래핀 분산액의 pH를 3 내지 4로 조절하는 역할을 한다.In addition, the neutralizing agent is contained in an amount of 0.07 to 0.7 parts by weight and is composed of at least one selected from the group consisting of stearin and amine, and serves to adjust the pH of the graphene oxide dispersion to 3 to 4.

또한, 상기 분산제는 0.05 내지 0.5 중량부가 함유되며, 아민계 및 스테아르산계로 이루어진 그룹에서 선택된 하나 이상으로 이루어지는데, 상기 판상형의 그래핀이 상기 이온수에 고르게 분산될 수 있도록 하는 역할을 한다.In addition, the dispersing agent is contained in an amount of 0.05 to 0.5 parts by weight and is composed of at least one selected from the group consisting of amine-based and stearic acid-based, and serves to ensure that the plate-like graphene is evenly dispersed in the ionized water.

또한, 상기의 성분으로 이루어지는 산화그래핀이 함유된 폴리에스터 원사는 폴리에스터 펠릿에 폴리에스터용 산화그래핀 마스터 배치 조성물을 물리적으로 혼합된 후에 폴리에스터 원사를 제조하는데 사용되는 통상의 조건으로 용융방사하여 산화그래핀이 함유된 폴리에스터 원사로 제조되는데, 상기와 같이 폴리에스터용 산화그래핀 마스터 배치 조성물을 이용하여 제조된 산화그래핀이 함유된 폴리에스터 원사는 산화그래핀 성분이 폴리에스터 원사에 전체적으로 균일하여 분포하여 균질한 물성을 나타낼 수 있다.In addition, the polyester yarn containing graphene oxide composed of the above components is melt-spun under normal conditions used to manufacture polyester yarn after physically mixing the graphene oxide master batch composition for polyester with polyester pellets. As described above, the graphene oxide-containing polyester yarn prepared using the graphene oxide master batch composition for polyester has a graphene oxide component in the polyester yarn. It can be uniformly distributed throughout and exhibits homogeneous physical properties.

상기의 과정을 통해 제조되는 산화그래핀이 함유된 폴리에스터 원사는 다양한 데니어(D, Denier)와 필라멘트(F, Filament)를 나타내도록 형성될 수 있는데, 아래 도 1에는 40D와 36F를 나타내는 산화그래핀이 함유된 폴리에스터 원사를 촬영하여 나타내었다.The polyester yarn containing graphene oxide produced through the above process may be formed to exhibit various denier (D, Denier) and filament (F, Filament). In FIG. 1 below, graphene oxide showing 40D and 36F A polyester yarn containing pins was photographed and shown.

이하에서는, 본 발명에 따른 산화그래핀이 함유된 폴리에스터 원사의 제조방법 및 그 제조방법으로 제조된 산화그래핀이 함유된 폴리에스터 원사의 물성을 실시예를 들어 설명하기로 한다.Hereinafter, the manufacturing method of the polyester yarn containing graphene oxide according to the present invention and the physical properties of the polyester yarn containing graphene oxide produced by the manufacturing method will be described with examples.

<제조예 1> 산화그래핀 분산액의 제조<Preparation Example 1> Preparation of graphene oxide dispersion

이온수 100 중량부, 그래핀(50 내지 500 나노미터 두께의 판상형) 0.5 중량부, 중화제(스테아린계) 0.35 중량부 및 분산제(아민계) 0.25 중량부를 혼합하여 산화그래핀 분산액을 제조하였다.A graphene oxide dispersion was prepared by mixing 100 parts by weight of ionized water, 0.5 parts by weight of graphene (plate-shaped with a thickness of 50 to 500 nanometers), 0.35 parts by weight of a neutralizer (stearin-based), and 0.25 parts by weight of a dispersing agent (amine-based).

<제조예 2> 폴리에스터용 산화그래핀 마스터 배치 조성물의 제조<Preparation Example 2> Preparation of graphene oxide master batch composition for polyester

폴리에스터(폴리에틸렌테레프탈레이트) 99.5 중량% 및 상기 제조예 1을 통해 제조된 산화그래핀 분산액 0.5 중량%를 혼합하고 용융압출한 후에 절단 및 냉각하여 펠릿형태의 폴리에스터용 산화그래핀 마스터 배치 조성물을 제조하였다.99.5% by weight of polyester (polyethylene terephthalate) and 0.5% by weight of the graphene oxide dispersion prepared in Preparation Example 1 were mixed and melt-extruded, then cut and cooled to obtain a graphene oxide master batch composition for polyester in pellet form. manufactured.

<실시예 1><Example 1>

폴리에스터(폴리에틸렌테레프탈레이트) 100 중량부에 상기 제조예 2를 통해 제조된 폴리에스터용 산화그래핀 마스터 배치 조성물 0.1 중량부를 혼합하고 용융방사하여 산화그래핀이 함유된 폴리에스터 원사(125D, 36F)를 제조하였다.Polyester yarn (125D, 36F) containing graphene oxide by mixing 0.1 part by weight of the graphene oxide master batch composition for polyester prepared in Preparation Example 2 with 100 parts by weight of polyester (polyethylene terephthalate) and melt-spun was manufactured.

<비교예 1><Comparative Example 1>

폴리에스터 원사(40D, 36F).Polyester yarn (40D, 36F).

상기 실시예 1을 통해 제조된 산화그래핀이 함유된 폴리에스터 원사의 중금속 함유여부를 측정하여 아래 도 2에 나타내었다.Heavy metal content of the polyester yarn containing graphene oxide prepared in Example 1 was measured and shown in FIG. 2 below.

{단, 중금속 함유여부는 한국화학융합시험연구원에 의뢰하여 측정하였다.} {However, the content of heavy metals was measured by requesting the Korea Testing & Research Institute for Chemical Convergence.}

아래 도 2에 나타낸 것처럼, 본 발명의 실시예 1을 통해 제조된 폴리에스터 원사에는 중금속이 함유되지 않은 것을 알 수 있다.As shown in Figure 2 below, it can be seen that the polyester yarn prepared through Example 1 of the present invention does not contain heavy metals.

또한, 상기 실시예 1을 통해 제조된 산화그래핀이 함유된 폴리에스터 원사와 상기 비교예 1을 통해 제조된 폴리에스터 원사로 티셔츠와 양말을 제조한 후에 열감효과를 측정하여 아래 도 3 내지 4에 나타내었다.In addition, after manufacturing T-shirts and socks with the polyester yarn containing graphene oxide prepared in Example 1 and the polyester yarn prepared in Comparative Example 1, the thermal effect was measured and shown in FIGS. 3 to 4 below. showed up

아래 도 3 내지 4에 나타낸 것처럼, 본 발명의 실시예 1을 통해 제조된 산화그래핀이 함유된 폴리에스터 원사는 비교예 1의 폴리에스터 원사에 비해 우수한 열감효과를 나타내는 것을 알 수 있다.As shown in Figures 3 to 4 below, it can be seen that the polyester yarn containing graphene oxide prepared through Example 1 of the present invention exhibits an excellent thermal effect compared to the polyester yarn of Comparative Example 1.

또한, 상기 실시예 1을 통해 제조된 산화그래핀이 함유된 폴리에스터 원사의 기계적 물성을 측정하여 아래 표 1에 나타내었다.In addition, the mechanical properties of the polyester yarn containing graphene oxide prepared in Example 1 were measured and shown in Table 1 below.

<표 1><Table 1>

Figure 112022087668890-pat00001
Figure 112022087668890-pat00001

상기 표 1에 나타낸 것처럼, 본 발명의 실시예 1을 통해 제조된 산화그래핀이 함유된 폴리에스터 원사는 기계적 물성이 우수한 것을 알 수 있다.As shown in Table 1, it can be seen that the polyester yarn containing graphene oxide prepared in Example 1 of the present invention has excellent mechanical properties.

또한, 상기 실시예 1을 통해 제조된 산화그래핀이 함유된 폴리에스터 원사의 자외선 차단효과를 측정하여 아래 도 5에 나타내었다.In addition, the UV blocking effect of the polyester yarn containing graphene oxide prepared in Example 1 was measured and shown in FIG. 5 below.

{단, 자외선차단효과는 제조된 산화그래핀이 함유된 폴리에스터 원사를 직조하여 니트로 제조한 상태에서 한국의류시험연구원에 의뢰하여 측정하였다.}{However, the UV blocking effect was measured by requesting the Korea Apparel Testing & Research Institute in a state in which the produced graphene oxide-containing polyester yarn was woven into knitwear.}

아래 도 5에 나타낸 것처럼, 본 발명의 실시예 1을 통해 제조된 산화그래핀이 함유된 폴리에스터 원사는 자외선 차단효과가 우수한 것을 알 수 있다.As shown in FIG. 5 below, it can be seen that the polyester fiber containing graphene oxide prepared in Example 1 of the present invention has excellent UV blocking effect.

또한, 상기 실시예 1을 통해 제조된 산화그래핀이 함유된 폴리에스터 원사의 마찰대전성과 항균성을 측정하여 아래 도 6 내지 7에 나타내었다.In addition, the triboelectricity and antibacterial properties of the polyester yarn containing graphene oxide prepared in Example 1 were measured and shown in FIGS. 6 to 7 below.

{단, 마찰대전성과 항균성은 FITI시험연구원에 의뢰하여 측정하였다.}{However, triboelectricity and antibacterial properties were measured by requesting the FITI Research Institute.}

아래 도 6 내지 7에 나타낸 것처럼, 본 발명의 실시예 1을 통해 제조된 산화그래핀이 함유된 폴리에스터 원사는 면포나 모포에 대해 우수한 대전방지효과를 나타내며, 우수한 항균성능을 나타내는 것을 알 수 있다.As shown in FIGS. 6 and 7 below, it can be seen that the graphene oxide-containing polyester yarn prepared in Example 1 of the present invention exhibits excellent antistatic effect on cotton cloth or blanket and exhibits excellent antibacterial performance. .

또한, 상기 실시예 1을 통해 제조된 산화그래핀이 함유된 폴리에스터 원사의 항바이러스성능을 측정하여 아래 도 8에 나타내었다.In addition, the antiviral performance of the polyester yarn containing graphene oxide prepared in Example 1 was measured and shown in FIG. 8 below.

{단, 항바이러스성능은 한국의과학연구소에 의뢰하여 측정하였다.}{However, the antiviral performance was measured by requesting the Korea Institute of Medical Science.}

아래 도 8에 나타낸 것처럼, 본 발명의 실시예 1을 통해 제조된 산화그래핀이 함유된 폴리에스터 원사는 인플로엔자A 바이러스에 대해 우수한 항바이러스성능을 나타내는 것을 알 수 있다.As shown in FIG. 8 below, it can be seen that the polyester yarn containing graphene oxide prepared in Example 1 of the present invention exhibits excellent antiviral performance against influenza A virus.

또한, 상기 실시예 1을 통해 제조된 산화그래핀이 함유된 폴리에스터 원사의 세탁견뢰도를 측정하여 아래 도 9에 나타내었다.In addition, the washing fastness of the polyester yarn containing graphene oxide prepared in Example 1 was measured and shown in FIG. 9 below.

{단, 세탁견뢰도는 KOTITI시혐연구원에 의뢰하여 측정하였다.}{However, washing fastness was measured by requesting the KOTITI Test Research Institute.}

아래 도 9에 나타낸 것처럼, 본 발명의 실시예 1을 통해 제조된 산화그래핀이 함유된 폴리에스터 원사는 3회 세척 후에도 항균성능이 유지되어 우수한 세탁견뢰도를 나타내는 것을 알 수 있다.As shown in FIG. 9 below, it can be seen that the polyester yarn containing graphene oxide prepared in Example 1 of the present invention maintains antibacterial performance even after washing three times and exhibits excellent washing fastness.

따라서, 본 발명에 따른 산화그래핀이 함유된 폴리에스터 원사는 산화그래핀이 함유되어 원적외선 방출 및 항균성능이 부가될 뿐만 아니라, 윤활성, UV 차단성, 전기전도성 및 방열특성을 나타내며, 내스크래치성, 내마모성, 인장강도, 굴곡강도 및 굴곡탄성율 등과 같은 기계적 물성이 향상된다.Therefore, the polyester fiber containing graphene oxide according to the present invention not only emits far-infrared rays and has antibacterial performance because graphene oxide is contained, but also exhibits lubricity, UV blocking, electrical conductivity and heat dissipation, and scratch resistance. , mechanical properties such as abrasion resistance, tensile strength, flexural strength and flexural modulus are improved.

Claims (6)

폴리에스터 100 중량부 및 폴리에스터용 산화그래핀 마스터 배치 조성물 0.05 내지 0.2 중량부로 이루어지며,
상기 폴리에스터용 산화그래핀 마스터 배치 조성물은 폴리에스터 99 내지 99.9 중량% 및 산화그래핀 분산액 0.1 내지 1 중량%로 이루어지고,
상기 산화그래핀 분산액은 이온수 100 중량부, 그래핀 0.1 내지 1 중량부, 중화제 0.07 내지 0.7 중량부 및 분산제 0.05 내지 0.5 중량부로 이루어지는 것을 특징으로 하는 산화그래핀이 함유된 폴리에스터 원사.
It consists of 100 parts by weight of polyester and 0.05 to 0.2 parts by weight of a graphene oxide master batch composition for polyester,
The graphene oxide master batch composition for polyester is composed of 99 to 99.9% by weight of polyester and 0.1 to 1% by weight of a graphene oxide dispersion,
The graphene oxide dispersion comprises 100 parts by weight of ionized water, 0.1 to 1 part by weight of graphene, 0.07 to 0.7 parts by weight of a neutralizer, and 0.05 to 0.5 parts by weight of a dispersant.
 삭제delete 삭제delete 삭제delete 청구항 1에 있어서,
상기 중화제는 스테아린계 및 아민계로 이루어진 그룹에서 선택된 하나 이상으로 이루어지는 것을 특징으로 하는 산화그래핀이 함유된 폴리에스터 원사.
The method of claim 1,
The neutralizer is polyester yarn containing graphene oxide, characterized in that consisting of at least one selected from the group consisting of stearin-based and amine-based.
 청구항 1에 있어서,
상기 분산제는 아민계 및 스테아르산계로 이루어진 그룹에서 선택된 하나 이상으로 이루어지는 것을 특징으로 하는 산화그래핀이 함유된 폴리에스터 원사.The method of claim 1,
The dispersant is graphene oxide-containing polyester yarn, characterized in that consisting of at least one selected from the group consisting of amine-based and stearic acid-based.
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KR101975955B1 (en) 2018-12-20 2019-05-08 맥섬석 지.엠. 주식회사 Manufacturing method of antimicrobial plastic masterbatch using macsumsuk granule
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KR102163232B1 (en) 2020-08-14 2020-10-08 주식회사 일송글로벌 Masterbatch having antibacterial and anti-fungal properties and its manufacturing method
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR20040012125A (en) * 2002-08-01 2004-02-11 주식회사 효성 Black Dope Dyed Full-Dull Polyester Fiber
JP2020525661A (en) * 2017-06-26 2020-08-27 ハンヂョウ ガオシー テクノロジー カンパニー リミテッドＨａｎｇｚｈｏｕ Ｇａｏｘｉ Ｔｅｃｈｎｏｌｏｇｙ Ｃｏ．， Ｌｔｄ． Graphene composite material and manufacturing method thereof
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