KR101148569B1 - Method for manufacturing carbon fiber - Google Patents
Method for manufacturing carbon fiber Download PDFInfo
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- KR101148569B1 KR101148569B1 KR1020090136247A KR20090136247A KR101148569B1 KR 101148569 B1 KR101148569 B1 KR 101148569B1 KR 1020090136247 A KR1020090136247 A KR 1020090136247A KR 20090136247 A KR20090136247 A KR 20090136247A KR 101148569 B1 KR101148569 B1 KR 101148569B1
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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
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
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- 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
- D01D5/04—Dry spinning methods
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- 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
- D01D5/06—Wet spinning methods
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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
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
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- D—TEXTILES; PAPER
- D02—YARNS; MECHANICAL FINISHING OF YARNS OR ROPES; WARPING OR BEAMING
- D02J—FINISHING OR DRESSING OF FILAMENTS, YARNS, THREADS, CORDS, ROPES OR THE LIKE
- D02J1/00—Modifying the structure or properties resulting from a particular structure; Modifying, retaining, or restoring the physical form or cross-sectional shape, e.g. by use of dies or squeeze rollers
- D02J1/22—Stretching or tensioning, shrinking or relaxing, e.g. by use of overfeed and underfeed apparatus, or preventing stretch
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- General Chemical & Material Sciences (AREA)
- Inorganic Fibers (AREA)
Abstract
본 발명은 탄소섬유 제조방법에 관한 것으로, 폴리아크릴로니트릴(PAN)계 탄소섬유의 전구체인 PAN계 중합체를 포함하는 방사용액을 습식 방사, 건식 방사 또는 건습식 방사하여 프리커서를 얻은 후, 이것을 200~400℃의 산화로에서 가열하여 내염화 섬유로 전환시키고, 적어도 1000℃의 온도의 불활성 분위기하에서 탄소화하여 제조되는 탄소섬유 제조방법에 있어서; 상기 프리커서는, 방사시 30~50m/min의 낮은 토출 선속도로 토출되어 낮은 연신배율을 갖도록 제조되고; 이렇게 제조된 프리커서를 산화로에서 내염화처리할 때 내염화 초기단계에서 열연신하는 것을 특징으로 하는 탄소섬유 제조방법을 제공한다.The present invention relates to a method for producing carbon fibers, wherein a spinning solution containing a PAN polymer, which is a precursor of polyacrylonitrile (PAN) carbon fiber, is wet-spun, dry-spun or dry-wet-spun to obtain a precursor. A carbon fiber production method produced by heating in an oxidation furnace at 200-400 ° C. to convert it into flame resistant fiber and carbonizing in an inert atmosphere at a temperature of at least 1000 ° C .; The precursor is manufactured to have a low draw ratio by being discharged at a low discharge linear velocity of 30-50 m / min during spinning; The precursor prepared in this way provides a carbon fiber manufacturing method characterized in that the thermal stretching in the initial stage of the flame resistance when subjected to the flame resistance treatment in the oxidation furnace.
본 발명에 따르면, 프리커서의 생산성과 연신배율의 향상을 통한 고물성 탄소섬유 제조가 가능하여 탄소섬유의 제조원가를 낮출 수 있고, 나아가 방사에 따른 조업성을 향상시키는 효과를 얻을 수 있다.According to the present invention, it is possible to manufacture a high-performance carbon fiber through the improvement of the productivity and the draw ratio of the precursor to reduce the manufacturing cost of the carbon fiber, it is possible to obtain the effect of improving the operability according to the spinning.
탄소섬유, 전구체 섬유, 프리커서, 연신배율, 고물성 Carbon fiber, precursor fiber, precursor, draw ratio, high physical properties
Description
본 발명은 탄소섬유 제조방법에 관한 것으로, 보다 상세하게는 프리커서의 생산성과 연신배율 향상을 통한 고물성의 탄소섬유를 생산할 수 있도록 한 탄소섬유 제조방법에 관한 것이다.The present invention relates to a carbon fiber manufacturing method, and more particularly to a carbon fiber manufacturing method that can produce a high-quality carbon fiber by improving the productivity and stretch ratio of the precursor.
주지된 바와 같이, 탄소섬유를 제조하는 방법으로 원료 섬유에 폴리 아크릴로니트릴(poly acrylonitrile)(PAN) 등의 전구체 섬유(프리커서)을 사용하고, 내염화 처리 및 탄소화 처리를 거쳐 탄소섬유를 얻는 방법이 보편화되어 있다.As is well known, a precursor fiber (precursor) such as poly acrylonitrile (PAN) is used as a raw material fiber as a method for producing carbon fiber, and carbon fiber is subjected to a flameproofing treatment and a carbonization treatment. The method of obtaining is common.
이렇게 제조된 소섬유는 보통 강도와 비탄성률 등 여러가지 양호한 특성을 가진다.The small fibers thus prepared usually have various good properties such as strength and inelasticity.
근래, 탄소섬유를 이용한 복합 재료 예컨대, 카본화이버(CFRP) 등의 공업적인 용도가 넓어지면서 스포츠(sports)/레저(leisure) 분야, 항공 우주 분야, 자동차 분야 등에서 고성능화(고강도화,고탄성화), 경량화(섬유 경량화 및 섬유 함유량 감소), 합성물의 물성 향상(탄소섬유 표면/계면 특성의 향상)에 대한 요구가 강해지고 있다.Recently, as the industrial use of carbon fiber composite materials such as carbon fiber (CFRP) has become wider, high performance (high strength, high elasticity) and light weight in sports / leisure, aerospace, and automobile fields (Fiber weight reduction and fiber content reduction) There is a strong demand for improving the physical properties of composites (improving carbon fiber surface / interface properties).
또한, 탄소섬유와 수지 등의 매트릭스(matrix) 재료와의 복합화에 있어서 고성능화를 추구하기 위해 매트릭스 재료가 가지는 특성도 중요하지만, 탄소섬유 그 자체의 표면 특성, 강도 및 탄성률을 향상시킬 필요가 있다.In addition, although the characteristics of the matrix material are important in order to achieve high performance in the composite of carbon fibers and matrix materials such as resins, it is necessary to improve the surface properties, strength and elastic modulus of the carbon fibers themselves.
뿐만 아니라, 생산성 측면에서도 상당한 연구가 요구되는 바, 특히 아크릴로 니트릴을 주성분으로 하는 PAN 계 중합물을 이용한 탄소섬유를 제조하는 공정에 있어 생산성을 향상은 전구체 섬유의 방사, 내염화, 탄화 등 모든 공정에서 진행되고 있다.In addition, in terms of productivity, considerable research is required. In particular, in the process of producing carbon fibers using PAN-based polymers containing acrylonitrile as the main component, all processes such as spinning, flameproofing, and carbonization of precursor fibers are improved. In progress.
이 경우, 방사에 있어 생산성 향상은 PAN계 중합물의 특성상 방사 드레프트율과 그의 응고 구조에 따른 한계 연신배율로 인하여 생산성이 제한되어 있고, 생산성을 향상하기 위해 방사속도를 높이면 연신성 저하가 발생하여 탄소섬유 물성이 저하하고, 방사속도를 내리면 생산성은 안정되고 고 연신배율의 프리커서 및 탄소섬유 제조가 가능하나 생산성은 저하된다.In this case, productivity improvement in spinning is limited due to the characteristics of the PAN-based polymer due to the radial draft ratio and the limiting draw ratio due to its solidification structure. When the carbon fiber properties are lowered and the spinning speed is lowered, the productivity is stabilized, and the precursor and the carbon fiber can be manufactured with high draw ratio, but the productivity is lowered.
따라서, 전구체 섬유(프리커서)의 생산성과 연신배율의 향상을 통한 고물성의 탄소섬유 생산은 양립이 어렵다는 한계를 가지며, 궁극적으로 이 문제가 해결되어야 향후 기술진보를 기대할 수 있는 실정이다.Therefore, the production of high-performance carbon fiber through the improvement of the productivity and the draw ratio of the precursor fiber (precursor) has a limit that is difficult to be compatible, ultimately, the situation can be expected to progress in the future if this problem is solved.
본 발명은 상술한 바와 같은 종래 기술상의 제반 문제점들을 감안하여 이를 해결하고자 창출된 것으로, 전구체 섬유(프리커서)를 생산함에 있어 토출 선속도를 일정한 수준으로 유지한 채 연신배율을 낮추고, 이를 내염화 초기단계에서 특정조건으로 열연신하여 프리커서의 생산성 향상과 연신배율 향상을 통한 고물성 탄소섬유를 생산할 수 있도록 한 탄소섬유 제조방법을 제공함에 그 주된 해결 과제가 있다.The present invention was created in view of the above-mentioned problems in the prior art as described above. In producing the precursor fiber (precursor), the draw ratio is lowered while maintaining the discharge linear velocity at a constant level, which is flameproofed. The main problem is to provide a method for producing a carbon fiber that can be hot-drawn to a specific condition in the initial stage to produce a high-performance carbon fiber by improving the productivity and draw ratio of the precursor.
본 발명은 상기한 해결 과제를 달성하기 위한 수단으로, 폴리아크릴로니트릴(PAN)계 탄소섬유의 전구체인 PAN계 중합체를 포함하는 방사용액을 습식 방사, 건식 방사 또는 건습식 방사하여 프리커서를 얻은 후, 이것을 200~400℃의 산화로에서 가열하여 내염화 섬유로 전환시키고, 적어도 1000℃의 온도의 불활성 분위기하에서 탄소화하여 제조되는 탄소섬유 제조방법에 있어서; 상기 프리커서는, 방사시 30~50m/min의 낮은 토출 선속도로 토출되어 낮은 연신배율을 갖도록 제조되고; 이렇게 제조된 프리커서를 산화로에서 내염화처리할 때 내염화 초기단계에서 열연신하는 것을 특징으로 하는 탄소섬유 제조방법을 제공한다.The present invention provides a precursor by wet spinning, dry spinning or dry wet spinning a spinning solution containing a PAN polymer which is a precursor of polyacrylonitrile (PAN) carbon fiber as a means for achieving the above-described problems. After that, it is heated in an oxidation furnace at 200-400 ° C. to convert it into flame resistant fiber, and the carbon fiber production method produced by carbonization in an inert atmosphere at a temperature of at least 1000 ° C .; The precursor is manufactured to have a low draw ratio by being discharged at a low discharge linear velocity of 30-50 m / min during spinning; The precursor prepared in this way provides a carbon fiber manufacturing method characterized in that the thermal stretching in the initial stage of the flame resistance when subjected to the flame resistance treatment in the oxidation furnace.
이때, 상기 프리커서의 낮은 연신배율은 배향도 80~85, 단섬도 1.8tex이고; 상기 내염화 초기 단계에서의 열연신은 배향도 90~95, 단섬도 1.5tex인 것에도 그 특징이 있다.At this time, the low draw ratio of the precursor is the orientation degree 80 ~ 85, the single fineness 1.8tex; The hot drawing in the initial stage of flameproofing is also characterized by having an orientation of 90 to 95 and a single fineness of 1.5 tex.
또한, 상기 내염화 초기단계는, 산화로의 첫번째 패스 또는 첫번째와 두번째 패스인 것에도 그 특징이 있다.In addition, the initial stage of flameproofing is characterized in that the first pass or the first and second pass of the oxidation furnace.
본 발명에 따르면, 프리커서의 생산성과 연신배율의 향상을 통한 고물성 탄소섬유 제조가 가능하여 탄소섬유의 제조원가를 낮출 수 있고, 나아가 방사에 따른 조업성을 향상시키는 효과를 얻을 수 있다.According to the present invention, it is possible to manufacture a high-performance carbon fiber through the improvement of the productivity and the draw ratio of the precursor to reduce the manufacturing cost of the carbon fiber, it is possible to obtain the effect of improving the operability according to the spinning.
이하에서는, 첨부도면을 참고하여 본 발명에 따른 바람직한 실시예를 더욱 상세하게 설명하기로 한다.Hereinafter, with reference to the accompanying drawings will be described in detail a preferred embodiment according to the present invention.
도 1은 본 발명에 따른 탄소섬유 제조방법을 설명하기 위한 탄소섬유 주행방향과 연신위치를 보여 주는 개략적인 공정도이다.1 is a schematic process chart showing a carbon fiber running direction and a stretching position for explaining the carbon fiber manufacturing method according to the present invention.
먼저, 탄소섬유 중에서 가장 널리 이용되어 있는 폴리아크릴로니트릴(PAN)계 탄소섬유는 그의 전구체가 되는 PAN계 중합체를 포함하는 방사 용액을 습식 방사, 건식 방사 또는 건습식 방사하여 탄소섬유 전구체 섬유를 얻은 후, 이것을 200 내지 400℃의 온도의 산화성 분위기하에서 가열하여 내염화 섬유로 전환시키고, 적어도 1000℃의 온도의 불활성 분위기하에서 가열하여 탄소화함으로써 공업적으로 제조된다.First, polyacrylonitrile (PAN) -based carbon fiber, which is most widely used among carbon fibers, is obtained by wet spinning, dry spinning or wet-wetting spinning a spinning solution containing a PAN polymer which is a precursor thereof. Thereafter, this is industrially produced by heating in an oxidizing atmosphere at a temperature of 200 to 400 ° C. to convert it into a flame resistant fiber, and carbonizing by heating in an inert atmosphere at a temperature of at least 1000 ° C.
이러한 PAN계 탄소섬유의 생산성 향상은 탄소섬유 전구체 섬유의 방사, 내염화 또는 탄소화의 어느 측면에서든 행해지고 있다.The productivity improvement of such PAN system carbon fiber is performed in any aspect of spinning, flameproofing, or carbonization of a carbon fiber precursor fiber.
하지만, 앞서 설명하였듯이, PAN계 탄소섬유 전구체 섬유를 얻을 때의 방사에 있어 PAN계 중합체 용액의 특성에 수반되는 한계 방사 드래프트율과 그의 응고 구조에 따른 한계 연신 배율에 의해 생산성이 제한되어 있고, 생산성을 향상시키기 위해 방사 속도를 높이면 연신성 저하가 발생하여 생산이 불안정화되기 쉽고, 방사 속도를 내리면 생산은 안정화되지만 생산성은 저하되기 때문에 생산성 향상과 안정화의 양립이 곤란하다는 것이 현실이었다.However, as described above, the productivity is limited by the limiting spin rate in accordance with the properties of the PAN polymer solution and the limit draw ratio according to its solidification structure in spinning when obtaining a PAN-based carbon fiber precursor fiber, Increasing the spinning speed to reduce the elongation occurs to reduce the elongation, which makes the production unstable, and lowering the spinning speed, the production is stabilized, but the productivity is lowered, so it is difficult to achieve both productivity and stabilization.
이에, 본 발명에서는 연신율이 낮은 프리커서를 제조하고, 이를 내염화 초기단계에서 일정 배향도를 갖도록 열연신함으로써 프리커서의 생산성 향상과 함께 고물성 특성도 갖는 탄소섬유를 생산할 수 있도록 구현하였다.Thus, in the present invention, a precursor having a low elongation is manufactured and heat-stretched to have a certain degree of orientation at the initial stage of flameproofing, thereby improving carbon productivity having high physical properties as well as productivity of the precursor.
보다 구체적으로, 도 1에서와 같이, 본 발명은 탄소섬유가 산화로(100)로 진입된 후 다수의 패스(Path)를 거쳐 탄소섬유 주행방향(100)으로 진행할 때 상기 탄소섬유 주행방향(100)의 특정 지점, 즉 상기 산화로(100)의 첫번째 또는 첫번째와 두번째 패스에서 연신하도록 연신 위치(200)가 설정된다.More specifically, as shown in FIG. 1, the present invention provides the carbon
그리고, 상기 연신 위치(200)에서 배향도가 90~95 수준에 이르도록 이 수준까지만 연신하게 되는데, 그 이유는 이 이상 과도하게 연신하게 되면 단사절, 모우 발생 등 내염화사의 품위를 저하시키고, 이로 인해 탄소섬유 전체의 품위를 떨어뜨리므로 상기 범위로 연신하여야 한다.And, the stretching position (200) is stretched only up to this level so that the degree of orientation reaches 90 ~ 95 level, the reason is that if excessively stretched more than this lowers the dignity of flame-resistant yarn, such as single thread, moor occurrence, Due to the deterioration of the overall quality of the carbon fiber should be drawn in the above range.
상술한 바는 내염화 초기 단계에서 이루어지는 열연신(배향도 90~95, 단섬도 1.5tex)이다.What has been described above is the thermal stretching (orientation degree 90 to 95, single fineness 1.5 tex) made in the initial stage of flameproofing.
그전에, 프리커서, 즉 전구체 섬유를 토출할 때 토출 선속도를 30~50m/min으로 유지하여야 한다.Before that, the discharge linear velocity should be maintained at 30-50 m / min when discharging the precursor, that is, the precursor fiber.
이는 연신배율이 낮은 프리커서를 제조하기 위함이며, 이때 프리커서의 배향도는 80~85, 단섬도는 1.8tex를 만족해야 한다.This is to prepare a precursor having a low draw ratio, wherein the orientation of the precursor should be 80 to 85, and the single fineness should satisfy 1.8 tex.
이또한 후속공정인 산화로(100)에서의 연신시 모두에서 설명한 범주까지 열연신을 용이하고 정확하며 균일하게 하기 위한 것으로, 이를 벗어나게 되면 산화로(100)의 연신 위치(200)에서 열연신할 때 단사절, 모우 등의 주된 발생요인이 되기 때문이다.This is also for easy, accurate and uniform thermal stretching up to the range described in the stretching process in the
이와 같이, 본 발명은 프리커서 생산시 토출 선속도를 30~50m/min으로 낮게 유지하여 연신배율이 낮은 프리커서를 만들고, 이 프리커서를 산화로(100)에서 내염화처리할 때 그 초기 단계인 첫번째 혹은 첫번째와 두번째 패스에서 열연신시킴으로써 프리커서의 생산성을 향상시킴과 동시에 내염화 처리시 연신배율을 높여 고물성을 갖는 탄소섬유를 제조할 수 있게 된다.As described above, the present invention maintains the discharge linear velocity at the time of precursor production at 30 to 50 m / min to make a precursor having a low draw ratio, and when the precursor is flameproofed in the
도 1은 본 발명에 따른 탄소섬유 제조방법을 설명하기 위한 탄소섬유 주행방향과 연신위치를 보여 주는 개략적인 공정도이다.1 is a schematic process chart showing a carbon fiber running direction and a stretching position for explaining the carbon fiber manufacturing method according to the present invention.
* 도면의 주요 부분에 대한 부호의 설명 *Explanation of symbols on the main parts of the drawings
100 : 산화로 200 : 탄소섬유 주행방향100: oxidation furnace 200: carbon fiber traveling direction
300 : 연신 위치300: stretching position
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2001192937A (en) | 2000-01-06 | 2001-07-17 | Toray Ind Inc | Method of producing carbon fiber |
| JP2003138435A (en) | 2001-11-01 | 2003-05-14 | Toho Tenax Co Ltd | Method for producing flameproofed fiber |
| KR20080076937A (en) * | 2005-12-13 | 2008-08-20 | 도레이 가부시끼가이샤 | Carbon fiber, process for production of polyacrylonitrile-base precursor fiber for carbon fiber production, and process for production of carbon fiber |
| KR20090068370A (en) * | 2006-10-18 | 2009-06-26 | 도레이 카부시키가이샤 | Polyacrylonitrile polymer, process for production of the polymer, process for production of precursor fiber for carbon fiber, carbon fiber, and process for production of the carbon fiber |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2001192937A (en) | 2000-01-06 | 2001-07-17 | Toray Ind Inc | Method of producing carbon fiber |
| JP2003138435A (en) | 2001-11-01 | 2003-05-14 | Toho Tenax Co Ltd | Method for producing flameproofed fiber |
| KR20080076937A (en) * | 2005-12-13 | 2008-08-20 | 도레이 가부시끼가이샤 | Carbon fiber, process for production of polyacrylonitrile-base precursor fiber for carbon fiber production, and process for production of carbon fiber |
| KR20090068370A (en) * | 2006-10-18 | 2009-06-26 | 도레이 카부시키가이샤 | Polyacrylonitrile polymer, process for production of the polymer, process for production of precursor fiber for carbon fiber, carbon fiber, and process for production of the carbon fiber |
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