KR0151987B1 - Method of manufacturing carbon fiber - Google Patents
Method of manufacturing carbon fiber Download PDFInfo
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- KR0151987B1 KR0151987B1 KR1019950023891A KR19950023891A KR0151987B1 KR 0151987 B1 KR0151987 B1 KR 0151987B1 KR 1019950023891 A KR1019950023891 A KR 1019950023891A KR 19950023891 A KR19950023891 A KR 19950023891A KR 0151987 B1 KR0151987 B1 KR 0151987B1
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- carbon fibers
- activated carbon
- fiber
- polyacrylonitrile
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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
- D01F9/225—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 from stabilised polyacrylonitriles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28023—Fibres or filaments
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- 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
- D10B2101/00—Inorganic fibres
- D10B2101/10—Inorganic fibres based on non-oxides other than metals
- D10B2101/12—Carbon; Pitch
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- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- General Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Inorganic Fibers (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
본 발명은 활성탄과 같이 흡착제로 사용되는 활성탄소섬유의 제조방법에 관한 것으로, 활성탄소 섬유의 제조조건을 적절히 조절하므로써 산화성 기체를 사용할 때보다 저온 및 단시간에 향상된 비료면적을 갖는 플리아크로 니트릴계 활성탄소섬유를 제조하는 방법을 제공하고자 하는데, 그 목적이 있다.The present invention relates to a method for producing activated carbon fibers used as an adsorbent such as activated carbon, and by controlling the conditions for the production of activated carbon fibers appropriately, a plyclonitrile-based activity having improved fertilizer area at lower temperatures and shorter time than using an oxidizing gas. It is an object of the present invention to provide a method for producing carbon fibers.
상기한 목적달성을 위한 본 발명은 폴리아크로니트릴계 탄소섬유를 원료로 하여 활성탄소섬유를 제조하는 방법에 있어서, 상기 폴리아크로니트릴계 탄소섬유를 공기중에서 안정화시킨후, 안정화된 섬유를 1-4M 농도범위의 KOH 용액에 4시간 이상 침적시키고, 이를 실온 ~ 100℃의 온도범위에서 건조시킨 다음, 불활성 분위기에서 600-800℃ 의 온도범위로 15분 이상 열처리하여 냉각시키고, 물로 세척 및 건조하여 활성탄소 섬유를 제조하는 방법을 그 요지로 한다.The present invention for achieving the above object is a method for producing activated carbon fibers using polyacrylonitrile-based carbon fibers as a raw material, after stabilizing the polyacrylonitrile-based carbon fibers in air, stabilized fibers 1-4M It is immersed in a KOH solution of concentration range for 4 hours or more, dried at a temperature range of room temperature to 100 ° C., then cooled by heat treatment for at least 15 minutes in a temperature range of 600-800 ° C. in an inert atmosphere, washed with water and dried The method to produce a carbon fiber is made into the summary.
Description
본 발명은 활성탄과 같이 흡착제로 사용되는 활성탄소섬유의 제조방법에 관한 것으로, 보다 상세하게는, 폴리아크릴로니트릴 섬유를 원료로 하여 수율 및 비표면적이 우수한 폴리아크릴로니트릴계 활성탄소섬유를 제조하는 방법에 관한 것이다.The present invention relates to a method for producing activated carbon fibers used as an adsorbent such as activated carbon, and more particularly, to produce polyacrylonitrile-based activated carbon fibers having excellent yield and specific surface area using polyacrylonitrile fibers as raw materials. It is about how to.
일반적으로 활성탄소섬유는 핏치계 범용탄소섬유, 페놀계 탄소섬유, 폴리 아크릴로 니트릴계 탄소섬유 등을 출발원료로 하여 제조되며, 이와같이 제조되는 활성탄소 섬유의 가장 중요한 특성은 비표면적이다.In general, activated carbon fibers are prepared using a pitch-based general purpose carbon fiber, phenolic carbon fiber, polyacrylonitrile-based carbon fiber, etc. as a starting material, the most important characteristic of the activated carbon fiber is a specific surface area.
그 이유는 흡착제로 사용되는 활성탄소섬유의 흡착능이 비표면적에 의해 좌우되기 때문이다.This is because the adsorption capacity of the activated carbon fibers used as the adsorbent depends on the specific surface area.
상기한 출발원료들중 핏치계 범용 탄소섬유와 페놀계 탄소섬유를 원료로 하는 활성탄소섬유의 제조는 종전의 석탄이나 야자 껍질을 원료로 하여 입상 활성탄을 제조하는 것과 같이, 수증기나 이산화탄소등과 같은 산화성 분위기에서 800-1000℃의 온도범위로 열처리하여 탄소섬유의 표면이 산화가스에 의해 부분 산화되도록 하므로써 산화반응이 발생한 곳은 기공이 형성된 활성탄소 섬유를 제조하였다.Among the above starting materials, the production of activated carbon fibers using pitch-type general purpose carbon fibers and phenolic carbon fibers as raw materials, such as water vapor or carbon dioxide, is carried out, as in the case of producing granular activated carbon from raw coal or palm husks as raw materials. The surface of the carbon fiber was partially oxidized by the oxidizing gas by heat treatment at a temperature range of 800-1000 ° C. in an oxidizing atmosphere to prepare activated carbon fibers having pores where oxidation reaction occurred.
그러나 폴리아크릴로니트릴계 탄소섬유를 이용하여 활성탄소섬유를 제조하는 것은 탄소섬유자체만으로 섬유의 결정화가 진행되어 있어 단순히 산화성 기체로 활성화시키는 것은 매우 어렵다. 이것은 산화성 기체가 탄소결정이 결함에 반응하여 산화반응이 개시되기는 하나 탄소섬유의 결정화가 진행되어 있어 산화반응이 진행되기 어렵기 때문이다.However, the production of activated carbon fibers using polyacrylonitrile-based carbon fibers is very difficult to simply activate the oxidizing gas because the crystallization of the fiber is only progressed to the carbon fiber itself. This is because the oxidizing gas initiates the oxidation reaction due to the carbon crystal reacting to the defect, but the crystallization of the carbon fiber proceeds and the oxidation reaction is difficult to proceed.
따라서, 종래에는 폴리아크릴로니트릴계 탄소섬유를 원료로 한 활성탄소섬유의 제조는 안정화 과정에서 연신력을 충분히 주어서 결정화가 가능한한 많이 진행되도록 하는 일반적인 탄소섬유의 제조방법을 따르지 않고, 안정화과정에서 연신력을 주지않고 안정화한 다음 탄화처리를 하고 이후에 이 섬유를 수증기 또는 이산화탄소로 반응시켜 활성탄소섬유를 제조하는 일본공개특허공보 소 49-11632 호의 방법을 주로 사용하였다. 그러나, 상기 일본공개 특허공보 소 49-116332호의 방법은 안정화섬유를 기준으로 할대 최종활성 탄소섬유의 수율이 매우 낮고 또한 활성탄소섬유의 장점인 미세기공의 형성의 한계 및 비표면적을 일정한 값 이상으로 가지는 것이 어려운 단점이 있다.Therefore, conventionally, the production of activated carbon fibers made of polyacrylonitrile-based carbon fibers as a raw material does not follow a general method of manufacturing carbon fibers, which gives sufficient stretching force in the stabilization process so that crystallization proceeds as much as possible, The method of Japanese Patent Application Laid-Open No. 49-11632, which stabilizes without drawing force and then carbonizes and reacts the fibers with water vapor or carbon dioxide, to produce activated carbon fibers, was mainly used. However, the method disclosed in Japanese Patent Laid-Open Publication No. 49-116332 has a very low yield of final activated carbon fibers based on stabilizing fibers and a limit of specific pore formation and specific surface area which is an advantage of activated carbon fibers. It is difficult to have.
이것은 폴리아크릴로니트릴 섬유의 직경이 7㎛ 정도로 매우 가늘어 산화반응시 미세기공의 형성 뿐만 아니라 섬유자체의 산화가 일어나서 섬유가 소모되기 때문이며 또한 800℃ 이상의 고온에서 반응이 진행되기 때문이다.This is because the diameter of the polyacrylonitrile fiber is very thin, such as 7 μm, and not only the formation of micropores during the oxidation reaction but also the oxidation of the fiber itself causes the fiber to be consumed, and the reaction proceeds at a high temperature of 800 ° C. or higher.
이와같은 폴리아크릴로니트릴계 탄소섬유를 이용한 활성탄소 섬유 제조시의 단점을 해결하고자 종래 많은 제안이 행해졌으며, 그중 대표적인 것으로는 일본공개특허공보 소 55-71613, 71614 및 미국특허 US 4285831 을 들수 있다.Many proposals have been made in order to solve the disadvantages of the production of activated carbon fibers using polyacrylonitrile-based carbon fibers, and examples thereof include Japanese Patent Application Laid-Open No. 55-71613, 71614 and US Pat. No. 42,831,831. .
일본공개특허공보 소 55-71613 호는 섬유의 원료에 할로겐화합물을 첨가하여 섬유를 제조한 후, 안정화, 탄화 활성화 과정을 거쳐서 활성탄소섬유를 제조하는 방법에 관한 것으로, 활성화 시간을 단축하는 것을 특징으로 하는 활성탄소섬유제조법에 대해 제안하였다. 그러나 상기와 같이 활성화시간을 단축하기 위새허 원료의 조성이 변하되어 기대하는 활성탄소섬유의 특성이 기대되기 어렵고, 또한 원료에 유해한 할로겐 화합물이 함유되어 있어 취급에 매우 주위를 하여야 하는 단점이 있다.Japanese Laid-Open Patent Publication No. 55-71613 relates to a method for producing activated carbon fibers by adding a halogen compound to the raw material of the fiber, and then stabilizing and carbonizing the activated carbon, and shortening the activation time. An activated carbon fiber manufacturing method was proposed. However, in order to shorten the activation time, the composition of the raw material is changed to shorten the activation time, so it is difficult to expect the characteristics of the activated carbon fiber, and also contains a halogen compound harmful to the raw material has a disadvantage that must be very close to handling.
일본공개 특허공보 소 55-71614 호는 폴리아크릴로니트릴 섬유를 제조할 때 이산화티타늄이나 알루미나 미분말을 0.06 - 10 중량% 범위로 첨가하여 섬유로 방사한 후 이 섬유를 안정화시켜서 활성화하는 과정을 거치는 방법에 관한 것이다. 그러나 이 방법은 폴리아크릴로니트릴 섬유에 첨가되는 첨가물에 의해서 섬유를 방사할 때 섬유의 절단 등의 문제점이 예견되는 단점이 있다.Japanese Patent Application Laid-Open No. 55-71614 discloses a method for producing polyacrylonitrile fiber by adding fine titanium dioxide or alumina powder in the range of 0.06-10 wt%, spinning it into a fiber, and then stabilizing and activating the fiber. It is about. However, this method has a disadvantage in that problems such as cutting of the fiber are expected when spinning the fiber by the additive added to the polyacrylonitrile fiber.
미국특허 US 4,285,831 호는 탄소섬유의 결정화를 만들어주는 연신력을 어느 한계까지 주어서 이것은 기계적 강도가 향상된 폴리아크릴로니트릴계 활성탄소섬유를 제조하는 방법에 관한 것이다. 그러나 이 방법은 섬유내의 산소함량의 변화를 기준으로 하는 연신력의 한계를 주어서 보편성이 제한되어 있고, 또한 비표면적도 크지 않은 단점이 있다.U. S. Patent No. 4,285, 831 gives stretching to the extent that makes the crystallization of carbon fibers to a certain extent, and relates to a process for producing polyacrylonitrile-based activated carbon fibers with improved mechanical strength. However, this method has a drawback in that the universality is limited and the specific surface area is not large due to the limitation of the stretching force based on the change of oxygen content in the fiber.
이에, 본 발명자는 상기한 종래 방법들의 단점을 해결하기 위하여 연구와 실험을 행하고, 그 결과에 근거하여 본 발명을 제안하게 된 것으로, 본 발명은 활성탄소섬유의 제조조건을 적절히 조절함으로써 산화성 기체를 사용할 때 보다 저온 및 단시간에 향상된 비표면적을 가지는 폴리아크릴로니트릴계 활성탄소섬유를 제조하는 방법을 제공하고자 하는데, 그 목적이 있다.Accordingly, the present inventors conducted research and experiments to solve the disadvantages of the conventional methods described above, and proposed the present invention based on the results, and the present invention provides an oxidizing gas by appropriately adjusting the production conditions of activated carbon fibers. It is an object of the present invention to provide a method for producing a polyacrylonitrile-based activated carbon fiber having an improved specific surface area at a lower temperature and shorter time of use.
이하, 본 발명을 설명한다.Hereinafter, the present invention will be described.
본 발명은 폴리아크릴로니트릴계 탄소섬유를 원료로 하여 활성탄소 섬유를 제조하는 방법에 있어서, 상기 폴리아크릴로니트릴계 탄소섬유를 공기중에서 안정화 시킨 후, 안정화된 섬유를 1-4M 농도범위의 KOH 용액에 4 - 24 시간 침적시키고, 이를 실온 - 100℃의 온도범위에서 건조시킨 다음, 불활성 분위기에서 600 - 800℃ 의 온도범위로 15 - 60분 동안 열처리하여 냉각시키고, 물로 세척 및 건조하여 활성탄소섬유를 제조하는 방법에 관한 것이다.The present invention is a method for producing activated carbon fibers using polyacrylonitrile-based carbon fibers as a raw material, after stabilizing the polyacrylonitrile-based carbon fibers in the air, the stabilized fibers KOH of 1-4M concentration range The solution was immersed in a solution for 4 to 24 hours, dried at a temperature range of room temperature to 100 ° C., then cooled by heat treatment for 15 to 60 minutes in an inert atmosphere at a temperature range of 600 to 800 ° C., washed with water and dried to form activated carbon. A method for producing a fiber
이하 본 발명을 보다 상세히 설명한다.Hereinafter, the present invention will be described in more detail.
상기한 목적을 달성하기 위하여 본 발명에서는 먼저 폴리아크릴로니트릴계 탄소 섬유를 공기중에 안정화시킴이 바람직하며, 그 이유는 다음과 같다.In order to achieve the above object, in the present invention, it is preferable to first stabilize the polyacrylonitrile-based carbon fiber in air, and the reason is as follows.
폴리아크릴로니트릴계 탄소섬유를 공기중에서 안정화시키는 것이 가장 단순하고 경제적이기 때문이며, 이때 조건은 230℃에서 2시간 내지 2시간 30분 정도면 충분하다.This is because stabilizing polyacrylonitrile-based carbon fibers in the air is the simplest and most economical, and the conditions are sufficient for 2 hours to 2 hours 30 minutes at 230 ° C.
이러한 안정화 처리는 오존 분위기에서도 가능하나 오존이 인체에 유해한 단점이 있다.This stabilization process is possible in an ozone atmosphere, but ozone is harmful to humans.
상기와 같이 안정화처리된 탄소섬유는 1-4M 농도범위 KOH 용액에 4 - 24시간 침적하는 것이 바람직하며 그 이유는 다음과 같다.As described above, the stabilized carbon fiber is preferably deposited for 4 to 24 hours in a 1-4M concentration range KOH solution for the following reasons.
처리용액으로 KOH를 선택한 것은 탄소섬유에 가장 효과적으로 삽입되는 것이 K원소이고 KOH가 수용액에 가장 잘녹기 때문이며, 용액의 농도가 1M 이하일 경우에는 활성탄소섬유를 제조한 후 비표면적이 크지 않거나 침적시간을 장시간 유지시켜야 하는 단점이 있으며, 4M 이상일 경우에는 섬유가 끊어지기 쉬어 취급이 어렵기 때문이다. 그리고 탄소섬유를 KOH용액에 4시간 이상 침적시키는 것은 KOH가 안정화 처리된 섬유에 충분히 부착되어 내부로 확산될수 있도록 하기 위해서이며, 침적시간을 24시간 이하로 하는 것은 KOH가 섬유에 과다하게 부착되어 섬유가 부러지기 쉽고, 또한, 비표면적이 떨어질 수 있기 때문이다.KOH was selected as the treatment solution because it is the most effective insertion of carbon into the carbon fiber and KOH is most soluble in the aqueous solution.When the concentration of the solution is less than 1M, the specific surface area is not large or the deposition time is reduced after the production of activated carbon fiber. There is a disadvantage that it must be maintained for a long time, because when the fiber is more than 4M is difficult to handle broken. The carbon fiber is deposited in the KOH solution for 4 hours or more so that the KOH can be sufficiently attached to the stabilized fiber and diffused therein. The deposition time is 24 hours or less, and the KOH is excessively attached to the fiber. This is because it is easy to break, and the specific surface area may fall.
KOH용액에 침전된 탄소섬유의 건조시에는 특별한 조건은 없으나 100℃ 이상의 온도에서는 섬유가 발화되기 쉽기 때문에 가능한한 100℃ 이하에서 건조시키는 것이 바람직하다.There is no particular condition when drying the carbon fibers precipitated in the KOH solution, but it is preferable to dry them at 100 ° C. or lower as much as possible since the fibers are easily ignited at a temperature of 100 ° C. or higher.
상기와 같이 건조된 탄소섬유는 불활성 분위기에서 600-800℃ 의 온도범위로 15-60분 동안 열처리한후 냉각함이 바람직하며, 그 이유는 다음과 같다.Carbon fiber dried as described above is preferably cooled after heat treatment for 15-60 minutes in a temperature range of 600-800 ℃ in an inert atmosphere, the reason is as follows.
이때 불활성 분위기를 선택한 것은 고온에서 탄소가 산화되는 것을 방지하기 위함이며, 열처리 온도가 600℃이하일 경우에는 열처리에 장시간이 소요되고 비표면적이 적어 효율적인 활성탄소 섬유의 제조방법이 되지 못하며, 800℃ 이상일 경우에는 큰 문제는 없으나 고온이 되면 에너지 소모가 많아지기 때문에 특별한 장점이 없는 상태에서는 이 온도 범위에서 처리함이 바람직하기 때문이다. 그리고 처리시간은 반응을 위한 최소한의 시간을 고려하여 15분 이상으로 제한한다. 그런데, 처리시간이 60분을 넘으면 비표면적이 넓어져 유리한 점은 있으나 섬유에 부착된 KOH중 K이 너무 많이 섬유에 삽입되고 또한, KOH중의 O가 탄소와 너무 많이 반응하여 섬유의 강도확보가 어려우므로 15-60분으로 한정한다.At this time, the inert atmosphere was selected to prevent the carbon from being oxidized at a high temperature. When the heat treatment temperature is lower than 600 ° C., the heat treatment takes a long time and the specific surface area is small, so that it is not an efficient method of producing activated carbon fibers, and is higher than 800 ° C. In this case, there is no big problem, but when it is high temperature, energy consumption increases, so it is preferable to treat in this temperature range without any special advantage. And the treatment time is limited to 15 minutes or more considering the minimum time for the reaction. However, if the treatment time exceeds 60 minutes, the specific surface area is advantageous, but there is an advantage, but too much K in the KOH attached to the fiber is inserted into the fiber, and O in the KOH reacts too much with the carbon, making it difficult to secure the strength of the fiber. Therefore, it is limited to 15-60 minutes.
열처리후에는 물로 세척하여 섬유에 부착된 KOH를 완전히 제거하여야 하며 이는 KOH가 섬유에 남아 있을 때 향후 활용면에서 제약이 따를 수 있기 때문이다. 이때, 물을 선택한 것은 단순 세척용이므로 물이 가장 적합하고 K와 반응하지 않기 때문이다.After the heat treatment, the KOH attached to the fiber should be completely removed by washing with water, because it may be restricted in terms of future utilization when KOH remains in the fiber. At this time, since the water is selected for simple washing, water is most suitable and does not react with K.
이하, 실시예를 통하여 본 발명을 보다 구체적으로 설명한다.Hereinafter, the present invention will be described in more detail with reference to Examples.
[실시예 1]Example 1
안정화 폴리아크릴로니트릴 섬유를 1M KOH 용액에 4시간 침적시킨 것을 100℃ 에서 건조한 다음 700℃에서 15분간 불활성 분위기에서 열처리를 한 결과, 수율이 48%이고 비표면적인 1080㎡/g 인 활성탄소섬유를 제조할 수 있었다.The stabilized polyacrylonitrile fiber was immersed in a 1M KOH solution for 4 hours, dried at 100 ° C., and then heat-treated at 700 ° C. for 15 minutes in an inert atmosphere. The result was an activated carbon fiber having a yield of 48% and a specific surface area of 1080 m 2 / g. Could be prepared.
[실시예 2]Example 2
상기 실시예 1의 안정화섬유를 이용하여 2M KOH 용액에 20시간 침적하고 이것을 상온에서 건조한 후 800℃에서 15분간 불활성 분위기에서 열처리 한 결과, 수율이 45% 이며 비표면적이 1290㎡/g 인 활성탄소 섬유를 제조할 수 있었다.After immersing in 2M KOH solution for 20 hours using the stabilizing fiber of Example 1 and drying it at room temperature, and heat-treated at 800 ℃ for 15 minutes in an inert atmosphere, the yield is 45% and the specific surface area of 1290㎡ / g Fibers could be produced.
[실시예 3]Example 3
상기 실시예 1의 안정화섬유를 이용하여 3M KOH 용액에 20시간 침적한 후 100℃에서 건조한 것을 700℃ 에서 15분간 불활성 분위기에서 열처리 한 결과, 수율이 45%이며 비표면적이 1290㎡/g 인 활성탄소 섬유를 제조할 수 있었다.After immersing in 3M KOH solution for 20 hours using the stabilizing fiber of Example 1 and then dried at 100 ℃ heat treatment at 700 ℃ for 15 minutes in an inert atmosphere, the yield is 45% and the specific surface area of 1290㎡ / g Carbon fibers could be produced.
[실시예4]Example 4
상기 실시예 1의 안정화섬유를 이용하여 4M KOH 용액에 20시간 침적시킨 후 100℃에서 건조한 것은 700℃에서 15분간 불활성 분위기에서 열처리 한 결과, 수율이 34%이며 비표면적이 2236㎡/g 인 활성탄소 섬유를 제조할 수 있었다.After immersing in 4M KOH solution for 20 hours using the stabilizing fiber of Example 1 and dried at 100 ℃ heat treatment in an inert atmosphere at 700 ℃ for 15 minutes, the yield is 34% and the specific surface area of 2236㎡ / g Carbon fibers could be produced.
[비교예 1]Comparative Example 1
상기 실시예 1의 안정화섬유를 이용하여 830℃에서 30분간 수증기로 활성화하여 활성탄소섬유를 제조한 결과, 수율이 12% 이며 비표면적이 760㎡/g이었다.The activated carbon fiber was prepared by activating with water vapor at 830 ° C. for 30 minutes using the stabilizing fiber of Example 1, and the yield was 12% and the specific surface area was 760 m 2 / g.
[실시예 5]Example 5
상기 실시예 1의 안정화섬유를 이용하여 2M KOH 용액에 20시간 침적시킨후 불활성분위기에서 800℃에서 15분간만 열처리 한 결과, 수율이 44% 이며 비표면적이 1500㎡/g 인 활성탄소 섬유를 제조할 수 있었다.After immersing in 2M KOH solution for 20 hours using the stabilizing fiber of Example 1 and heat-treated only at 800 ℃ for 15 minutes in an inert atmosphere, the yield is 44% and the specific surface area of 1500 m 2 / g to produce an activated carbon fiber Could.
[실시예 6]Example 6
상기 실시예 1의 안정화 섬유를 이용하여 2M KOH용액에 24시간 침적시킨 후 100℃에서 건조한 것을 600℃ 에서 15분간 불활성 분위기에서 열처리 한 결과, 수율이 50%이며 비표면적이 1000㎡/g인 활성탄소 섬유를 제조할 수 있었다.After immersing in 2M KOH solution for 24 hours using the stabilizing fibers of Example 1 and then dried at 100 ℃ heat treatment at 600 ℃ for 15 minutes in an inert atmosphere, the yield is 50% and the specific surface area 1000㎡ / g Carbon fibers could be produced.
[비교예2]Comparative Example 2
상기 실시예 1의 안정화 섬유를 이용하여 600℃에서 4시간 수증기로 활성화시켜 활성탄소섬유를 제조한 결과, 수율은 50% 이며 비표면적이 50㎡/g인 활성탄소섬유를 제조할 수 있었다.As a result of activating the activated carbon fiber by steam at 600 ° C. for 4 hours using the stabilizing fiber of Example 1, the yield was 50% and the specific surface area of 50 m 2 / g was able to produce an activated carbon fiber.
상기 실시예 (1-6) 및 비교예(1-2) 에서 알수 있는 바와 같이, 본 발명의 범위를 만족시키는 실시예 (1-6)의 경우 본 발명의 범위를 만족하지 못하는 종래방법인 비교예(1-2)의 경우에 비하여 수율이 3배이상 높고 낮은 온도에서 비표면적이 향상된 활성탄소섬유를 제조할 수 있음을 알수 있다.As can be seen from the above Example (1-6) and Comparative Example (1-2), in the case of Example (1-6) that satisfies the scope of the present invention, the comparison is a conventional method that does not satisfy the scope of the present invention. Compared with the case of Example (1-2), it can be seen that the activated carbon fiber with improved yield is more than three times higher and the specific surface area is reduced.
상술한 바와 같이, 본 발명은 폴리아크릴로니트릴을 원료로 한 섬유를 공기중에서 안정화 한후 1-4M KOH 용액에 침적시켜서 건조한후 이를 열처리하므로서, 종래에 수증기에 의해 제조된 활성탄소섬유보다 수율이 높고 낮은 온도에서 비표면적이 향상된 활성탄소 섬유의 제조가 가능하여 에너지 절감효과 및 수율 향상으로인한 생산성 증대에 매우 유용한 효과가 있다.As described above, the present invention stabilizes the fiber made of polyacrylonitrile in air, and then, dipped in 1-4M KOH solution, dried, and then heat-treated, thereby yielding higher yield than the conventional activated carbon fiber produced by water vapor. It is possible to manufacture activated carbon fibers with improved specific surface area at low temperature, which is very useful for increasing productivity due to energy saving and yield improvement.
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| KR20060071628A (en) * | 2004-12-22 | 2006-06-27 | 주식회사 포스코 | A method of increasing the nitrogen content in an active carbon fiber |
| KR101360465B1 (en) * | 2006-12-20 | 2014-02-07 | 주식회사 포스코 | Activated fiber for siloxane removal and manufacturing method thereof |
| US20190302849A1 (en) * | 2016-07-12 | 2019-10-03 | Kortek Corporation | Curved display |
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| JP3638778B2 (en) | 1997-03-31 | 2005-04-13 | 株式会社ルネサステクノロジ | Semiconductor integrated circuit device and manufacturing method thereof |
| KR20000072686A (en) * | 2000-09-19 | 2000-12-05 | 이순환 | crank two engine = C.2. engine |
| KR100509965B1 (en) * | 2002-11-29 | 2005-08-25 | (주)대동 에이씨 | Mass manufacturing method of activated carbon fiber from phenol resin fiber |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20060071628A (en) * | 2004-12-22 | 2006-06-27 | 주식회사 포스코 | A method of increasing the nitrogen content in an active carbon fiber |
| KR101360465B1 (en) * | 2006-12-20 | 2014-02-07 | 주식회사 포스코 | Activated fiber for siloxane removal and manufacturing method thereof |
| US20190302849A1 (en) * | 2016-07-12 | 2019-10-03 | Kortek Corporation | Curved display |
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