KR100205908B1 - Manufacture of aramid - Google Patents

Manufacture of aramid Download PDF

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Publication number
KR100205908B1
KR100205908B1 KR1019940014453A KR19940014453A KR100205908B1 KR 100205908 B1 KR100205908 B1 KR 100205908B1 KR 1019940014453 A KR1019940014453 A KR 1019940014453A KR 19940014453 A KR19940014453 A KR 19940014453A KR 100205908 B1 KR100205908 B1 KR 100205908B1
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heat treatment
aramid
resin
present
fibers
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KR1019940014453A
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Korean (ko)
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KR960001321A (en
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최상렬
허철
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구광시
주식회사코오롱
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/11Compounds containing epoxy groups or precursors thereof

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)

Abstract

본 발명은 폴리-파라-페닐렌테레프탈아미드 섬유를 이용하여, 전처리, 열처리, 수지함침, 열처리의 과정을 거침으로써, 아라미드 섬유의 강도 및 탄성율을 더욱 증가시키고 고무나 수지 등으로 피복 또는 성형시 강한 접착력을 가질 수 있어 코드사 또는 각종 벨트와 보강재로 사용할 수 있는 아라미드 섬유의, 제조방법에 관한 것이다.The present invention, by using the poly-para-phenylene terephthalamide fibers, the process of pre-treatment, heat treatment, resin impregnation, heat treatment further increases the strength and elastic modulus of the aramid fibers, and strong when coated or molded with rubber or resin The present invention relates to a method for producing aramid fibers that can have adhesive strength and can be used as cord yarns or various belts and reinforcements.

Description

[발명의 명칭][Name of invention]

아라미드 섬유의 제조방법Method of Making Aramid Fiber

[발명의 상세한 설명]Detailed description of the invention

본 발명은 아라미드 섬유의 제조방법에 관한 것으로서, 더욱 상세하게는 폴리-파라-페닐렌테레프탈아미드 섬유를 이용하여 전처리, 열처리, 수지함침, 열처리의 과정을 거침으로써, 아라미드 섬유의 강도 및 탄성율을 더욱 증가시키고 고무나 수지 등으로 피복 또는 성형시 강한 접착력을 가질 수 있어 코드사 또는 각종 벨트의 보강재로 사용할 수 있는 아라미드 섬유의 제조방법에 관한 것이다.The present invention relates to a method for producing aramid fibers, and more specifically, by using a poly-para-phenylene terephthalamide fiber through a process of pretreatment, heat treatment, resin impregnation, heat treatment, the strength and elastic modulus of the aramid fiber further The present invention relates to a method for producing aramid fibers that can be used as a reinforcing material of cord yarns or various belts by increasing strength and having strong adhesive strength when coating or molding with rubber or resin.

종래에 나일론 또는 폴리에스테르 섬유를 코드(Cord)사 또는 각종 벨트류의 보강재로 사용하기 위해서는 고중합도 폴리머를 사용하거나 고배율 연신을 하는 등의 방법을 이용하였으나, 코드 또는 각종 벨트류의 보강재로 사용될 수 있을 정도의 충분한 물성을 갖는 섬유를 제조하기에는 상당한 어려움이 있었다.Conventionally, in order to use nylon or polyester fiber as a reinforcement material for cord yarn or various belts, a method such as using a high degree of polymerization polymer or high magnification stretching is used, but it can be used as a reinforcing material for cords or various belts. There has been considerable difficulty in producing fibers having sufficient physical properties.

또한, 아라미드 섬유를 코드사나 각종 벨트류의 보강재로 이용하면 나일론 또는 폴리에스테르 섬유에 비해 그 향상된 물성으로 인해 코드 등의 각종 보강재로 유리한 점이 있으나 코드 또는 각종 벨트류의, 보강재로서의 아라미드 섬유는 보다 더 높은 수준의 물성(특히 탄성률)이 요구되고 있으며, 아울러 이러한 문제를 해결하여 각종 보강재로 사용하기 위해서는 분자량을 조절한다든지 하는 공정 조절에 큰 문제가 있었다.In addition, when aramid fibers are used as reinforcements for cord yarns and various belts, they have advantages over various reinforcements such as cords due to their improved physical properties compared to nylon or polyester fibers. Physical properties (especially modulus of elasticity) are required, and in order to solve these problems and use them as various reinforcing materials, there was a big problem in controlling the process such as adjusting the molecular weight.

따라서, 본 발명은 상기와 같은 종래 기술의, 문제점을 해결한 것으로서, 아라미드 섬유를 연속적인 단일 공정내에서 물 또는 각종 용제로 전처리하고 열처리한 후 수지에 함침하고, 다시 열처리하여 보강재로 적합한 아라미드 섬유를 제조하는데 그 목적이 있다.Accordingly, the present invention solves the problems of the prior art as described above, the aramid fibers are pretreated with water or various solvents in a single continuous process, heat treated, impregnated with resin, and then heat treated to be suitable as a reinforcing material. Its purpose is to manufacture.

이하, 본 발명을 상세하게 설명하면 다음과 같다.Hereinafter, the present invention will be described in detail.

본 발명은 폴리-파라-페닐렌테레프탈아미드 섬유를 물 또는 각종 용제로 처리한 후 300∼500℃에서 1∼10초간 제1열처리하고 드라이 픽업(Dry-pick up)이 3∼10중량%가 되도록 수지함침 및 제2열처리 함을 특징으로하는 아라미드 섬유의, 제조방법에 관한 것이다.In the present invention, the poly-para-phenylene terephthalamide fiber is treated with water or various solvents, followed by the first heat treatment at 300 to 500 ° C. for 1 to 10 seconds, so that the dry pick-up becomes 3 to 10% by weight. The present invention relates to a method for producing aramid fibers characterized by resin impregnation and second heat treatment.

이하, 본 발명을 더욱 상세하게 설명하면 다음과 같다.Hereinafter, the present invention will be described in more detail.

본 발명은 아라미드 섬유를 물이나 각종 용제로 전처리하여 섬유의 내부구조를 팽윤 또는 활성화시킨 뒤 고온에서 순간적인 열처리를 함으로써, 아라미드 섬유의 강도 및 탄성율을 보다 증가시킨다.The present invention swells or activates the internal structure of the fiber by pretreatment of the aramid fiber with water or various solvents and then instant heat treatment at high temperature, thereby further increasing the strength and elastic modulus of the aramid fiber.

전처리 용제로서는 물이나 디메틸포름알데히드(DMF), N_메틸피롤리돈(NMP), 디메틸아세트아미드(DMAc)등을 사용했으며, 이들 물이나 용제가 담겨 있는 용기(bath)내로 원사를 통과시키므로써, 섬유 내부의 결정구조가 어느 정도 흐트러져서 후에 열처리시 결정구조가 재배열되고 배향성이 더욱 증가될 수있는 상태로 내부구조를 활성화시킬 수있다.As a pretreatment solvent, water, dimethylformaldehyde (DMF), N_methylpyrrolidone (NMP), dimethylacetamide (DMAc), etc. were used, and the yarn was passed through a bath containing water or a solvent. In addition, it is possible to activate the internal structure in such a state that the crystal structure inside the fiber is disturbed to some extent so that the crystal structure can be rearranged and the orientation can be further increased during the heat treatment.

열처리는 300∼500℃에서 1∼10초간 처리하였는데, 처리온도가 300℃미만이거나,처리시간이 1초 미만일 경우에는 열처리 효과가 나타나지 않으며, 처리온도가 500℃보다 높거나 처리시간이 10초를 초과할 경우에는 아라미드 섬유에 탄화가 일어난다.The heat treatment was performed at 300 to 500 ° C. for 1 to 10 seconds. If the treatment temperature is less than 300 ° C. or the treatment time is less than 1 second, the heat treatment is not effective. The treatment temperature is higher than 500 ° C. or the treatment time is 10 seconds. If exceeded, carbonization occurs in the aramid fibers.

이러한 방법에 의해 전처리,열처리를 하면, 아라미드 섬유의 내부 구조 재배열 및 고배향성이 일어나, 섬유의 강도 및 탄성율이 더욱 증가된다.Pretreatment and heat treatment by this method result in internal structure rearrangement and high orientation of the aramid fibers, further increasing the strength and elastic modulus of the fibers.

연속되는 공정으로, 고무나 수지와의 접착력을 부여하기 위하여 수지 함침 후 열처리를 하게 되는데, 함침에 사용되는 수지로는 에폭사이드 폴리에틸렌이민, 트리메틸올, 비스(베타-아지도-포밀옥시에틸)-이소프탈레이트(Bis(β-azido-fomyloxyethy1)-isophthalate), 레조시놀-포름알데히드-라텍스(RFL)등이며 수지 함침된 섬유가 오존, 자외선, 산화질소, 이산화황등에 노출시 접착력의 감소를 방지하기 위해 메틸메타크릴레이트, 아크릴산, N-메틸올아크릴아미드 등의 첨가제를 혼합하여 사용한다. 이러한 수지 및 첨가제를 포함하는 수용액에 1차 열처리된 섬유를 함침하여 200∼280℃에서 1∼10분간 2차 열처리를 하며, 수지함침은 드라이 픽업이 3∼10중량%가 되게 한다.In a continuous process, heat treatment is performed after resin impregnation to give adhesion to rubber or resin. Resin used for impregnation includes epoxide polyethyleneimine, trimethylol, bis (beta-azido-formyloxyethyl)- Isophthalate (Bis (β-azido-fomyloxyethy1) -isophthalate), resorcinol-formaldehyde-latex (RFL), etc., and resin-impregnated fibers to prevent loss of adhesion when exposed to ozone, ultraviolet light, nitrogen oxides, sulfur dioxide, etc. To this end, additives such as methyl methacrylate, acrylic acid, and N-methylol acrylamide are mixed and used. The aqueous solution containing the resin and the additive is impregnated with the first heat-treated fiber and subjected to the second heat treatment at 200 to 280 ° C. for 1 to 10 minutes, and the resin impregnation causes the dry pickup to be 3 to 10% by weight.

드라이 픽업이 3중량% 미만일 경우는 충분한 접착성을 발휘하지 못하며, 10중량%를 초과하는 경우 수지의 과다 부착으로 경화가 불충분하여 점착성을 가져 해사성 불량의 원인이 된다.If the dry pick-up is less than 3% by weight, sufficient adhesiveness cannot be exhibited. If the dry pickup is more than 10% by weight, excessive adhesion of the resin may result in insufficient curing, resulting in poor adhesion and cause deterioration of nautical properties.

2차 열처리의 온도가 200℃ 미만이거나 열처리 시간이 1분 미만일 경우 수지층이 충분히 경화되지 않아 해사성 불량의 원인이 되며, 온도가 280℃를 초과하거나 시간이 10분을 초과하는 경우 코드사가 뻣뻣해짐으로 인해 내구성이 불량해진다.If the temperature of the secondary heat treatment is less than 200 ° C or the heat treatment time is less than 1 minute, the resin layer is not sufficiently cured, which may cause decomposability. If the temperature exceeds 280 ° C or the time exceeds 10 minutes, the cord yarn is stiff. As a result, the durability is poor.

본 발명에 의하면 단일화된 공정으로 아라미드 코드사를 제조할 수있고, 기존의 아라미드 코드사 보다 강도 및 탄성율이 보다 개선되고 우수한 접착력을 가지는 아라미드 코드사를제조할 수 있다.According to the present invention, the aramid cord yarn can be manufactured by a unified process, and the aramid cord yarn can be manufactured with improved strength and elastic modulus and excellent adhesion than the existing aramid cord yarn.

이하, 본 발명을 실시예를 통하여 더욱 구체적으로 설명하겠는 바, 본 발명이 실시예에 의하여 한정되는 것은 아니다.Hereinafter, the present invention will be described in more detail with reference to Examples, but the present invention is not limited by Examples.

[실시예 및 비교예][Examples and Comparative Examples]

인장강도가 20g/d, 탄성율이 500g/d인 아라미드 섬유 1,500d/2ply를 이용하여표 1과 같은 조건으로 전처리 및 열처리를 하였으며, 수지함침에는 레조시놀-포름알데히드-라텍스와 첨가제로 메틸메타크릴레이트를 포함하는 수용액 상태로 만들어 표 1과 같은 조건으로 함침 후 재 열처리 하였으며, 제조된 섬유의 물성변화를 표 1에 나타내었다.Pretreatment and heat treatment were carried out under the conditions shown in Table 1 using 1,500 d / 2 ply of aramid fiber having a tensile strength of 20 g / d and an elastic modulus of 500 g / d. It was made into an aqueous solution containing acrylate, and then re-annealed under the conditions as shown in Table 1, and the physical properties of the prepared fiber are shown in Table 1.

※ DMF : 디메틸포름알데히드※ DMF: Dimethylformaldehyde

DMA: 디메틸아세트아미드DMA: Dimethylacetamide

Claims (1)

폴리-파라-페닐렌테레프탈아미드 섬유를 디메틸포름알데히드, 디메틸아세트아마이드, N-메틸피롤리돈 또는 물로 전처리한 후 300∼500℃에서 1∼10초간 제1 열처리하고, 드라이 픽업(Dry-pick up)이 3∼10중량%가 되도록 수지함침 및 제2열처리 함을 특징으로 하는 아라미드 섬유의 제조방법.The poly-para-phenylene terephthalamide fibers are pretreated with dimethylformaldehyde, dimethylacetamide, N-methylpyrrolidone or water, followed by first heat treatment at 300 to 500 ° C. for 1 to 10 seconds and dry pick-up. ) Is a 3 to 10% by weight resin impregnation and second heat treatment method for producing aramid fibers. [청구항 2][Claim 2] 제1항에 있어서, 제2열처리는 200∼280℃에서 1∼10분간 열처리함을 특징으로 하는 아라미드 섬유의 제조방법.The method of claim 1, wherein the second heat treatment is a heat treatment for 1 to 10 minutes at 200 ~ 280 ℃.
KR1019940014453A 1994-06-23 1994-06-23 Manufacture of aramid KR100205908B1 (en)

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KR100205908B1 true KR100205908B1 (en) 1999-07-01

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101235676B1 (en) 2010-09-03 2013-02-21 주식회사 삼부포리마 High-strength yarn complex substituting iron rod and method of manufacturing the same

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR101235676B1 (en) 2010-09-03 2013-02-21 주식회사 삼부포리마 High-strength yarn complex substituting iron rod and method of manufacturing the same

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