KR101558215B1 - Method of manufacturing high molecular polyethylene monofilament by using wasted high molecular polyethylene film containing oil and high molecular polyethylene monofilament manufactured thereby - Google Patents

Method of manufacturing high molecular polyethylene monofilament by using wasted high molecular polyethylene film containing oil and high molecular polyethylene monofilament manufactured thereby Download PDF

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KR101558215B1
KR101558215B1 KR1020140061579A KR20140061579A KR101558215B1 KR 101558215 B1 KR101558215 B1 KR 101558215B1 KR 1020140061579 A KR1020140061579 A KR 1020140061579A KR 20140061579 A KR20140061579 A KR 20140061579A KR 101558215 B1 KR101558215 B1 KR 101558215B1
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high molecular
molecular weight
weight polyethylene
polyethylene film
oil
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전용완
권희재
송재동
전초현
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주식회사 모아
한국섬유개발연구원
권희재
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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
    • D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
    • D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
    • D01F8/06—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyolefin as constituent
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J11/00—Recovery or working-up of waste materials
    • C08J11/04—Recovery or working-up of waste materials of polymers
    • C08J11/06—Recovery or working-up of waste materials of polymers without chemical reactions
    • C08J11/08—Recovery or working-up of waste materials of polymers without chemical reactions using selective solvents for polymer components
    • 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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00—Technologies for solid waste management
    • Y02W30/50—Reuse, recycling or recovery technologies
    • Y02W30/62—Plastics recycling; Rubber recycling

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Cell Separators (AREA)

Abstract

According to the present invention, a high molecular polyethylene monofilament is manufactured by: grinding a waste high molecular polyethylene film containing oil; firstly removing the oil by thermally treating the waste high molecular polyethylene film in a heater; secondly removing oil by continuously treating the waste high molecular polyethylene film with methylene chloride; producing reused high molecular polyethylene pellets by melting and extruding the waste high molecular polyethylene film; making the reused high molecular polyethylene pellets pass through a heat tube by melting and spinning the high molecular polyethylene pellets into monofilaments; and quenching, elongating, thermally setting the monofilaments. According to the present invention, the waste high molecular polyethylene film containing oil which is generated when a separation membrane of a lithium secondary battery is manufactured is used. Therefore, waste of resource, emission of carbon dioxide, consumption of petroleum, and environmental waste can be reduced. Consequently, high molecular polyethylene monofilaments with high performance can be manufactured at low costs and in an eco-friendly manner.

Description

오일함유 폐 고분자량 폴리에틸렌 필름을 이용한 고분자 폴리에틸렌 모노필라멘트의 제조방법 및 이로 제조된 고분자량 폴리에틸렌 모노필라멘트{Method of manufacturing high molecular polyethylene monofilament by using wasted high molecular polyethylene film containing oil and high molecular polyethylene monofilament manufactured thereby}TECHNICAL FIELD The present invention relates to a method for producing a high molecular weight polyethylene monofilament using an oil-containing high molecular weight polyethylene film and a high molecular weight polyethylene monofilament produced by the method and a high molecular weight polyethylene monofilament manufactured thereby,

본 발명은 오일함유 폐 고분자량 폴리에틸렌 필름을 이용한 고분자 폴리에틸렌 모노필라멘트의 제조방법 및 이로 제조된 고분자량 폴리에틸렌 모노필라멘트에 관한 것으로서, 보다 구체적으로는 리튬2차전지의 분리막 제조시 발생되는 오일함유 폐 고분자량 폴리에틸렌 필름(Wasted high molecular polyethylene film)을 재생처리하여 이를 원료로 고분자량 폴리에틸렌 모노필라멘트를 제조하는 방법에 관한 것이다.
The present invention relates to a process for producing a high molecular weight polyethylene monofilament using an oil-containing high molecular weight polyethylene film and a high molecular weight polyethylene monofilament produced by the process, and more particularly to a process for producing a high molecular weight polyethylene monofilament, And a method for producing a high molecular weight polyethylene monofilament from a raw material by regenerating a wasted high molecular polyethylene film.

리튬2차전지의 분리막으로 사용되는 고분자량 폴리에틸렌 필름(High molecular weight polyethylene film)은 고분자량 폴리에틸렌 수지를 파라핀 또는 데카하이드로 나프탈렌(decahydro naphthalene) 등과 같은 유기용매에 용해시킨 용액을 압출, 초연신하여 제조되며, 그로 인해 제조된 상기 고분자량 폴리에틸렌 필름 내에는 액체 파라핀오일(Liquid paraffin oil) 등과 같은 오일(Oil)이 적어도 3중량% 이상 함유되어 있다.A high molecular weight polyethylene film used as a separator of a lithium secondary battery is produced by extruding a solution prepared by dissolving a high molecular weight polyethylene resin in an organic solvent such as paraffin or decahydro naphthalene, , And the high molecular weight polyethylene film produced thereby contains at least 3% by weight of oil such as liquid paraffin oil.

한편, 상기 고분자량 폴리에틸렌 필름으로 리튬2차전지의 분리막을 제조시 고분자량 폴리에틸렌 필름의 가장자리(Edge) 절단공정을 거치면서 액체 파라핀 오일이 함유된 폐 고분자량 폴리에틸렌 필름(Wasted high molecular weight polyethylene film)이 1차로 발생되고, 액체 파라핀 오일이 제거되어 함유안된 폐 고분자량 폴리에틸렌 필름이 2차로 발생 된다.Meanwhile, a high molecular weight polyethylene film containing liquid paraffin oil is produced through the edge cutting process of a high molecular weight polyethylene film when the separation membrane of a lithium secondary battery is produced using the high molecular weight polyethylene film. And the liquid paraffin oil is removed, so that a pulverized high molecular weight polyethylene film not containing is generated secondarily.

종래에는 상기와 같이 고분자량 폴리에틸렌 필름으로 리튬2차전지의 분리막을 제조할때 발생되는 액체 파라민 오일 함유 폐 고분자량 폴리에틸렌 필름은 재활용 방법이 없어서 소각 및/또는 매립 등의 방법으로 폐기처리하였고, 그로 인해 자원이 낭비되고, 이산화탄소의 배출이 증가하고, 환경폐기물이 증가하는 등의 많은 문제점이 발생되었다.
Conventionally, a liquid paraffin oil-containing high molecular weight polyethylene film produced when a separator of a lithium secondary battery is produced using a high molecular weight polyethylene film has no recycling method and is disposed of by incineration and / or landfill. Thereby causing wasted resources, increasing carbon dioxide emissions, and increasing environmental wastes.

본 발명의 과제는 리튬2차전지의 분리막 제조시 발생되는 오일 함유 폐 고분자량 폴리에틸렌 필름으로부터 오일을 제거하여 재생 고분자량 폴리에틸렌 펠렛을 제조한 다음, 이를 용융방사하여 고분자량 폴리에틸렌 모노필라멘트를 제조하는 방법을 제공하는 것이다.
The object of the present invention is to provide a method for producing high molecular weight polyethylene monofilament by producing oil of high molecular weight polyethylene pellets by removing oil from oil-containing high molecular weight polyethylene film produced in the production of a separator of lithium secondary battery, .

본 발명은 오일 함유 폐 고분자량 폴리에틸렌 필름을 분쇄한 후, 이를 히터내에서 열처리하여 오일을 1차로 제거하고, 계속해서 메틸렌클로라이드로 처리하여 오일을 2차로 제거한 후, 이를 용융, 압출하여 재생 고분자량 폴리에틸렌 펠렛으로 제조하고, 이를 모노필라멘트 상태로 용융방사하여 열튜브를 통과시킨 다음 차례로 퀀칭, 연신 및 열고정시켜 고분자량 폴리에틸렌 모노필라멘트를 제조한다.
The present invention relates to a process for producing an oil-containing waste high molecular weight polyethylene film by pulverizing an oil-containing high molecular weight polyethylene film, heat treating the oil-containing waste high molecular weight polyethylene film in a heater to remove oil therefrom first, then treating the oil with methylene chloride to remove oil secondarily, Polyethylene pellets, melt-spun in a monofilament state, passed through a heat tube, and then quenched, stretched and heat-set in order to produce a high molecular weight polyethylene monofilament.

본 발명은 리튬2차전지의 분리막 제조시 발생하는 오일을 함유하는 폐 고분자량 폴리에틸렌 필름을 재활용하기 때문에 자원의 낭비 감소, 이산화탄소의 배출 감소, 석유자원 절감 및 환경폐기물의 감소가 가능하여 친환경적이며 저렴한 제조비용으로 고성능의 고분자량 폴리에틸렌 모노필라멘트를 제조할 수 있다.
The present invention recycles a high molecular weight polyethylene film containing an oil generated in the production of a separator of a lithium secondary battery, thereby reducing waste of resources, reducing carbon dioxide emission, reducing petroleum resources and reducing environmental wastes, High-molecular-weight polyethylene monofilaments can be produced with high production cost.

이하, 본 발명을 상세하게 설명한다.Hereinafter, the present invention will be described in detail.

본 발명에 따른 오일 함유 폐 고분자량 폴리에틸렌 필름을 이용한 고분자량 폴리에틸렌을 제조하는 방법은, (ⅰ) 리튬2차전지의 분리막 제조시 발생되는 폐기물로서 오일(Oil)을 함유하는 고분자량 폴리에틸렌 필름(High molecular weight polyethylene film)을 분쇄하는 공정; (ⅱ) 분쇄된 상기 고분자 폴리에틸렌 필름의 조각들을 히터(Heater) 내에서 열처리하여 상기 고분자량 폴리에틸렌 필름의 조각내에 함유된 오일을 1차로 제거하는 공정; (ⅲ) 히터(Heater) 내에서 열처리되어 1차로 오일이 제거된 고분자량 폴리에틸렌 필름의 조각들을 메틸렌 클로라이드(Methylene chloride)로 처리하여 상기 고분자량 폴리에틸렌 필름의 조각내에 함유된 오일을 2차로 제거하는 공정; (ⅳ) 2차로 오일이 제거된 고분자량 폴리에틸렌 필름의 조각들을 용융, 압출하여 재생 고분자량 폴리에틸렌 펠렛(Pellet)을 제조하는 공정; 및 (ⅴ) 재생 고분자량 폴리에틸렌 펠렛(Pellet)을 용융한 다음 방사구금을 통해 모노필라멘트 상태로 방사하고, 계속해서 열튜브(Hot tube)를 통과시킨 다음, 차례로 퀀칭, 연신 및 열고정시켜 고분자량 폴리에틸렌 모노필라멘트를 제조하는 공정;을 포함한다.The method for producing the high molecular weight polyethylene using the oil-containing high molecular weight polyethylene film according to the present invention is characterized in that (i) a high molecular weight polyethylene film containing oil as a waste generated in the production of a separation membrane of a lithium secondary battery (High molecular weight polyethylene film); (Ii) heat treating the pieces of the pulverized high molecular weight polyethylene film in a heater to primarily remove the oil contained in the high molecular weight polyethylene film piece; (Iii) a step of secondarily removing the oil contained in the piece of the high molecular weight polyethylene film by treating the pieces of the high molecular weight polyethylene film subjected to the heat treatment in the heater and having the oil removed first, with methylene chloride ; (Iv) a step of melting and extruding the pieces of the high molecular weight polyethylene film from which the oil has been removed in the second stage to produce regenerated high molecular weight polyethylene pellets; And (v) spinning the regenerated high molecular weight polyethylene pellets through a spinneret in a monofilament state and then passing them through a hot tube, followed by quenching, stretching and heat setting to obtain high molecular weight And a step of producing a polyethylene monofilament.

구체적으로, 본 발명에서는 먼저 리튬2차전지의 분리막 제조시 발생되는 폐기물로서 오일(Oil)을 함유하는 고분자량 폴리에틸렌 필름(High molecular weight polyethylene film)을 분쇄한다.Specifically, in the present invention, a high molecular weight polyethylene film containing oil is pulverized as a waste generated in the production of a separation membrane of a lithium secondary battery.

분쇄된 고분자량 폴리에틸렌 필름의 크기는 폭 5㎝×길이 5~20㎝ 수준인 것이 바람직하다.The size of the pulverized high molecular weight polyethylene film is preferably 5 cm wide × 5 cm to 20 cm long.

다음으로, 분쇄된 상기 고분자 폴리에틸렌 필름의 조각들을 히터(Heater) 내에서 열처리하여 상기 고분자량 폴리에틸렌 필름의 조각 내에 함유된 오일을 1차로 제거한다.Next, the pieces of the pulverized high molecular weight polyethylene film are heat treated in a heater to primarily remove the oil contained in the high molecular weight polyethylene film piece.

상기 공정에 의해 오일함유 폐 고분자량 폴리에틸렌 필름에 함유된 전체 오일 중 약 45% 정도가 제거된다.By this process, about 45% of the total oil contained in the oil-containing waste high molecular weight polyethylene film is removed.

다음으로, 히터(Heater) 내에서 열처리되어 1차로 오일이 제거된 고분자량 폴리에틸렌 필름의 조각들을 메틸렌 클로라이드(Methylene chloride)로 처리하여 상기 고분자량 폴리에틸렌 필름의 조각내에 함유된 오일을 2차로 제거한다.Next, the pieces of the high molecular weight polyethylene film which has been heat-treated in the heater and the oil is firstly removed are treated with methylene chloride to remove the oil contained in the pieces of the high molecular weight polyethylene film secondarily.

상기 공정에 의해 오일 함유 폐 고분자량 폴리에틸렌 필름에 함유된 오일의 함량은 1중량% 미만으로 된다.By this process, the content of the oil contained in the oil-containing high molecular weight polyethylene film is less than 1% by weight.

다음으로는, 2차로 오일이 제거된 고분자량 폴리에틸렌 필름의 조각들을 용융, 압출하여 재생 고분자량 폴리에틸렌 펠렛(Pellet)을 제조한다.Next, the pieces of the secondarily degreased, high molecular weight polyethylene film are melted and extruded to produce regenerated high molecular weight polyethylene pellets.

이때, 2차로 오일이 제거된 고분자량 폴리에틸렌 필름의 조각들을 280~300℃로 용융, 압출하는 것이 바람직하다. 상기와 같이 제조된 재생 고분자량 폴리에틸렌 펠렛은 항복강도가 106 kgf/㎠, 인장강도가 193 kgf/㎠, 충격강도가 48.3 kgf·㎝/㎠로 우수하다.At this time, it is preferable to melt and extrude the pieces of the high molecular weight polyethylene film from which the oil has been removed at a temperature of 280 to 300 占 폚. The regenerated high molecular weight polyethylene pellets prepared as described above had a yield strength of 106 kgf / cm 2, a tensile strength of 193 kgf / cm 2 and an impact strength of 48.3 kgf · cm / cm 2.

다음으로는, 재생 고분자량 폴리에틸렌 펠렛(Pellet)을 용융한 다음 방사구금을 통해 모노필라멘트 상태로 방사하고, 계속해서 열튜브(Hot tube)를 통과시킨 다음, 차례로 퀀칭, 연신 및 열고정시켜 고분자량 폴리에틸렌 모노필라멘트를 제조 한다.Next, the regenerated high molecular weight polyethylene pellets are melted and then spun in a monofilament state through a spinneret, followed by passing through a hot tube, followed by quenching, stretching and heat setting to obtain a high molecular weight Thereby producing a polyethylene monofilament.

이때, 열튜브(Hot tube)를 통과한 모노필라멘트를 40~60℃의 온도에서 퀀칭하고 10~12배의 연신비로 연신한 후 180℃에서 열고정 한다.At this time, the monofilaments passed through a hot tube are quenched at a temperature of 40 to 60 ° C, stretched at a stretching ratio of 10 to 12 times, and then thermally fixed at 180 ° C.

상기와 같은 제조방법으로 제조된 고분자량 폴리에틸렌 모노필라멘트는 강도가 9~15 g/d이고 신도가 10~20%로 우수하다.The high molecular weight polyethylene monofilament prepared by the above-mentioned method has excellent strength of 9 to 15 g / d and elongation of 10 to 20%.

Claims (5)

(ⅰ) 리튬2차전지의 분리막 제조시 발생되는 폐기물로서 오일(Oil)을 함유하는 고분자량 폴리에틸렌 필름(High molecular weight polyethylene film)을 분쇄하는 공정;
(ⅱ) 분쇄된 상기 고분자 폴리에틸렌 필름의 조각들을 히터(Heater) 내에서 열처리하여 상기 고분자량 폴리에틸렌 필름의 조각내에 함유된 오일을 1차로 제거하는 공정;
(ⅲ) 히터(Heater) 내에서 열처리되어 1차로 오일이 제거된 고분자량 폴리에틸렌 필름의 조각들을 메틸렌 클로라이드(Methylene chloride)로 처리하여 상기 고분자량 폴리에틸렌 필름의 조각내에 함유된 오일을 2차로 제거하는 공정;
(ⅳ) 2차로 오일이 제거된 고분자량 폴리에틸렌 필름의 조각들을 용융, 압출하여 재생 고분자량 폴리에틸렌 펠렛(Pellet)을 제조하는 공정; 및
(ⅴ) 재생 고분자량 폴리에틸렌 펠렛(Pellet)을 용융한 다음 방사구금을 통해 모노필라멘트 상태로 방사하고, 계속해서 열튜브(Hot tube)를 통과시킨 다음, 차례로 퀀칭, 연신 및 열고정시켜 고분자량 폴리에틸렌 모노필라멘트를 제조하는 공정;을 포함하는 것을 특징으로 하는 오일함유 폐 고분자량 폴리에틸렌 필름을 이용한 고분자량 폴리에틸렌 모노필라멘트의 제조방법.(I) a step of pulverizing a high molecular weight polyethylene film containing oil as a waste generated in the production of a separation membrane of a lithium secondary battery;
(Ii) heat treating the pieces of the pulverized high molecular weight polyethylene film in a heater to primarily remove the oil contained in the high molecular weight polyethylene film piece;
(Iii) a step of secondarily removing the oil contained in the piece of the high molecular weight polyethylene film by treating the pieces of the high molecular weight polyethylene film subjected to the heat treatment in the heater and having the oil removed first, with methylene chloride ;
(Iv) a step of melting and extruding the pieces of the high molecular weight polyethylene film from which the oil has been removed in the second stage to produce regenerated high molecular weight polyethylene pellets; And
(V) Recycled high molecular weight polyethylene pellets are melted and then spun in a monofilament state through a spinneret, followed by passing through a hot tube, followed by quenching, stretching and heat setting to obtain high molecular weight polyethylene Comprising the steps of: preparing a high molecular weight polyethylene monofilament using an oil-containing high molecular weight polyethylene film. 제1항에 있어서, 2차로 오일이 제거된 고분자량 폴리에틸렌 필름의 조각들 내 오일 함량이 1중량% 미만인 것을 특징으로 하는 오일함유 폐 고분자량 폴리에틸렌 필름을 이용한 고분자량 폴리에틸렌 모노필라멘트의 제조방법.A process for the preparation of high molecular weight polyethylene monofilaments according to claim 1, wherein the oil content in the pieces of the secondarily oil-removed high molecular weight polyethylene film is less than 1% by weight. 제1항에 있어서, 2차로 오일이 제거된 고분자량 폴리에틸렌 필름의 조각들을 280~300℃로 용융/압출하는 것을 특징으로 하는 오일함유 폐 고분자량 폴리에틸렌 필름을 이용한 고분자량 폴리에틸렌 모노필라멘트의 제조방법.The method for producing a high molecular weight polyethylene monofilament according to claim 1, wherein the pieces of the high molecular weight polyethylene film from which the oil has been removed are melted / extruded at 280 to 300 占 폚. 제1항에 있어서, 열튜브(Hot tube)를 통과한 모노필라멘트를 40~60℃의 온도에서 퀀칭하고 10~12배의 연신비로 연신한 후 180℃에서 열고정시키는 것을 특징으로 하는 오일함유 폐 고분자량 폴리에틸렌 필름을 이용한 고분자량 폴리에틸렌 모노필라멘트의 제조방법.The method according to claim 1, wherein the monofilament having passed through a hot tube is quenched at a temperature of 40 to 60 캜, stretched at a stretching ratio of 10 to 12 times, and thermally fixed at 180 캜. Method for producing high molecular weight polyethylene monofilament using high molecular weight polyethylene film. 삭제delete
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KR102181876B1 (en) * 2019-05-17 2020-11-24 강창기 Manufacturing method of composite resin composition using waste separator for secondary battery
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