KR100206488B1 - The manufacture method of the active carbon fiber - Google Patents
The manufacture method of the active carbon fiber Download PDFInfo
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- KR100206488B1 KR100206488B1 KR1019950040518A KR19950040518A KR100206488B1 KR 100206488 B1 KR100206488 B1 KR 100206488B1 KR 1019950040518 A KR1019950040518 A KR 1019950040518A KR 19950040518 A KR19950040518 A KR 19950040518A KR 100206488 B1 KR100206488 B1 KR 100206488B1
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- activated carbon
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- fibers
- sodium hydroxide
- carbon fiber
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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
Abstract
본 발명은 폴리아크릴로니트릴 섬유를 원료로 하여 활성탄소섬유를 제조하는 방법에 관한 것으로, 활성탄소 섬유의 제조시 수산화나트륨을 수용액 상태를 전처리하여 활성화 하므로서, 비표면적이 우수한 활성탄소섬유를 제공하고자 하는데, 그 목적이 있다.The present invention relates to a method for producing activated carbon fibers using polyacrylonitrile fibers as a raw material, and to provide activated carbon fibers having a specific surface area by activating sodium hydroxide by pre-treatment of aqueous solutions during the production of activated carbon fibers. There is a purpose.
상기한 목적을 달성하기 위한 본 발명은 폴리아크릴로니트릴 섬유를 공기중에서 안정화시킨 후, 안정화된 섬유를 1-5M의 농도범위를 가지는 수산화나트륨 용액에 1시간 이상 침적시키고 이를 실온에서 100℃의 사이에서 건조시킨 다음, 이를 불활성분위기에서 600℃-1000℃의 온도범위에서 15분 이상 열처리하고, 물로 세척 및 건조하는 것을 포함하여 이루어짐을 특징으로 하는 활성탄소섬유의 제조방법에 관한 것을 그 요지로 한다.In order to achieve the above object, the present invention stabilizes polyacrylonitrile fibers in air, and then, the stabilized fibers are immersed in a sodium hydroxide solution having a concentration range of 1-5 M for at least 1 hour and at room temperature between 100 ° C. After drying at, the heat treatment is carried out in an inert atmosphere at a temperature range of 600 ℃-1000 ℃ for more than 15 minutes, washed with water and dried, the method for producing an activated carbon fiber characterized in that it comprises. .
Description
본 발명은 폴리아크릴로니트릴 섬유를 원료로 하여 활성탄소섬유를 제조하는 방법에 관한 것으로, 보다 상세하게는, 폴리아크릴로니트릴 섬유를 공기중에서 안정화시킨 후, 안정화된 섬유를 수산화나트륨 용액에 침적시키고 건조시킨 후, 이것을 불활성 분위기에서 열처리에 의해 활성화한 것을 물로 세척, 건조함에 의해 기존의 수증기 부활에 의한 방법이나 수산화칼륨등에 의한 활성화 방법으로 제조한 것에 비해 비표면적이 향상된 활성탄소섬유를 제조하는 방법에 관한 것이다.The present invention relates to a method for producing activated carbon fibers using polyacrylonitrile fibers as a raw material, and more particularly, after stabilizing polyacrylonitrile fibers in air, the stabilized fibers are immersed in a sodium hydroxide solution. After drying, the activated carbon fiber having an improved specific surface area is prepared by washing and drying the activated product by heat treatment in an inert atmosphere, and by using the method of revitalizing steam or activating by potassium hydroxide. It is about.
활성탄소섬유의 원료는 크게 핏치계 범용탄소섬유 및 폴리아크릴로니트릴계 탄소섬유의 두가지가 가장 일반적이라고 할 수 있는데, 특히 핏치계 탄소섬유 중 이방성 핏치계 탄소섬유의 경우 종전의 석탄이나 야자껍질을 원료로 하는 입상활성탄과 같이 수증기나 이산환탄소 등과 같은 산화성 분위기에서 800-1000℃의 온도로 열처리함에 의해 활성화함으로써 활성탄소섬유의 제조가 가능하여 현재 널리 이용되고 있다.There are two types of activated carbon fibers, pitch-type general purpose carbon fibers and polyacrylonitrile-based carbon fibers. In particular, the anisotropic pitch-based carbon fibers among the pitch-based carbon fibers can be used for coal or palm skin. Like granular activated carbon as a raw material, activated carbon fibers are activated by heat treatment at an temperature of 800-1000 ° C. in an oxidizing atmosphere such as water vapor or dicyclic ring carbon, and are currently widely used.
이와같은 핏치계 탄소섬유를 원료로 하는 활성탄소 섬유의 제조방법에 관한 것으로는, 일본 공개특허공보(평)5-247781호의 방법이 대표적인데, 이 방법은 50％이상의 메조페이스 함량을 갖는 이방성 핏치섬유를 원료로 할 때 수산화칼륨, 수산화나트륨등을 첨가하여 활성화 하는 방법이다. 그러나 이 방법에서는 원료섬유의 4-7배의 대단히 많은 양의 수산화칼륨을 그대로 사용하므로서 후저리등에 있어서 심각한 문제를 일으킬 수 있으며 경제적인 면에서도 불리한 단점이 있으며 이방성 핏치계 탄소섬유의 제조에 한정되는 단점이 있다.As a method for producing activated carbon fibers using such pitch-based carbon fibers as a raw material, the method of JP-A-5-247781 is typical, which is an anisotropic pitch having a mesoface content of 50% or more. When fiber is used as a raw material, it is activated by adding potassium hydroxide and sodium hydroxide. In this method, however, 4-7 times as much potassium hydroxide as raw material is used, which can cause serious problems in post-treatment, etc., which is disadvantageous in terms of economics, and is limited to the production of anisotropic pitch-based carbon fibers. There are disadvantages.
폴리아크릴로나트릴계 탄소섬유를 이용하여 활성탄소섬유를 제조하는 것은 탄소섬유자체만으로는 섬유가 결정화가 진행되어 있어 단순히 산화성기체로 활성화시키는 것은 매우 어렵다. 이것은 산화성 기체가 탄소 결정의 결함에 반응하여 활성화 반응이 개시되나 결정화가 진행되어 있어 활성화반응이 진행되기 어렵기 때문이다.The production of activated carbon fibers using polyacrylonitrile-based carbon fibers is very difficult to activate simply by oxidizing gas because the fibers are crystallized only by the carbon fibers themselves. This is because the oxidizing gas reacts with the defect of the carbon crystal to initiate the activation reaction, but the crystallization is in progress and the activation reaction is difficult to proceed.
폴리아크릴로니트릴계 탄소섬유를 원료로 이용하여 활성 탄소를 제조하는 방법에 관한 종래기술로는 일본 공개특허 공보(소)49-116332호, (소)55-71613호, (소)55-71614호 및 미국특허 us 4,285,831호가 대표적이다.Prior arts relating to a method for producing activated carbon using polyacrylonitrile-based carbon fibers as a raw material include Japanese Patent Application Laid-Open Nos. 49-116332, 55-71613 and 55-71614. And U.S. Patent 4,285,831.
일반적인 탄소섬유를 제조할때에는 안정화 과정에서 연신력을 충분히 주어서 결정화가 가능한 한 많이 진행되도록 하는 것에 반해, 일본 공개특허공보(소)49-116332호의 방법에서는 활성탄소섬유를 제조할 때는 안정화 과정에서 연신력을 주지않고 안전화한 다음 탄화처리를 하고, 이후에 이 섬유를 수증기 또는 이산화탄소로 반응시켜 활성탄소섬유를 제조하는 방법을 사용하였다.In the manufacture of general carbon fibers, the stretching process is sufficiently given to allow the crystallization to proceed as much as possible, whereas in the method of JP 49-116332, the stretching in the stabilization process when manufacturing the activated carbon fibers is performed. Safety was applied without force, and then carbonized, and then the fiber was reacted with water vapor or carbon dioxide to produce activated carbon fibers.
그러나 이 방법은 안정화섬유를 기준으로 할때 최종활성탄소섬유의 수율이 매우 낮고 또한 활성탄소섬유의 장점인 미세기공의 형성의 한계 및 비표면적이 일정한 값 이상을 가지는 것이 어려운 단점이 있다.However, this method has a disadvantage in that the yield of the final activated carbon fiber is very low and the specific surface area of the fine pores, which is an advantage of the activated carbon fiber, has a specific surface area more than a certain value.
이것은 폴리아크릴로나트릴 섬유의 직경이 매우 가늘어 산화반응시 미세기공의 형성 뿐만아니라 섬유자체의 산화가 일어나서 섬유가 소모되기 때문이며 또한 800℃ 이상의 고온에서 반응이 진행되기 때문이다.This is because the diameter of the polyacrylonitrile fiber is so thin that 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.
일본 공개특허공보(소)55-71613호는 상기 일본 공개특허공보(소)49-116,332호의 방법에 있어서의 문제점을 해결하기 위한 방안중 하나를, 섬유의 원료에 할로겐화합물을 첨가하여 섬유를 제조한 후 안정화, 탄화, 활성화과정을 거쳐서 활성탄소섬유를 제조하는 방법으로 활성화시간을 단축하는 것을 특징으로 하는 활성탄소섬유 제조법에 대해 설명하였으나 이를 위해서는 원료의 조성이 변화됨으로서 기대하는 활성탄소섬유의 특성이 기대되기 어렵고 또한 원료에 유해한 할로겐화합물이 함유되어 있어 취급에 매유 주의를 하여야 하는 단점이 있다.Japanese Unexamined Patent Application Publication No. 55-71613 describes one of the methods for solving the problems in the method of Japanese Unexamined Patent Publication No. 49-116,332 to produce a fiber by adding a halogen compound to the raw material of the fiber. After that, the method for producing activated carbon fiber was characterized by shortening the activation time by stabilizing, carbonizing, and activating the activated carbon fiber. However, for this, the characteristics of the activated carbon fiber are expected as the composition of the raw material is changed. This is difficult to expect, and also contains harmful halogen compounds in the raw material has a disadvantage that must be very careful in handling.
일본 공개특허공보(소) 55-76614호는 상기(소) 55-71614와 같은 방법중의 하나로, 폴리아크릴로니트릴섬유를 제조할 때 이산화티타늄이나 알루미나 미분말을 0.06-10무게％까지 첨가하여 섬유로 방사한 후 이 섬유를 안정화시켜서 활성화하는 과정을 거치는 방법이나 이 방법에서는 첨가물의 첨가에 따른 원활한 방사의 곤란등의 단점이 있다.Japanese Laid-Open Patent Publication (S) 55-76614 is one of the same methods as (S) 55-71614. In the production of polyacrylonitrile fibers, a fine powder of titanium dioxide or alumina is added up to 0.06-10% by weight. After spinning into a method of stabilizing and activating the fiber, this method has a disadvantage, such as the difficulty of smooth spinning by the addition of additives.
또한, 미국특허US4285831호는 결정화를 위한 연신력을 어느 한계까지 주고, 이것으로 기계적 강도가 향상된 폴리아크릴로니트릴계 활성탄소섬유를 제조하는 방법에 관한 것이나, 섬유내의 산소함량의 변화를 기준으로 하는 연신력의 한계에 따른 보편성이 떨어지며 또한 비표면적도 떨어지는 단점이 있다.In addition, US Patent US4285831 relates to a method for producing a polyacrylonitrile-based activated carbon fiber which gives a stretching force for crystallization to a certain limit, thereby improving the mechanical strength, or based on the change of oxygen content in the fiber Due to the limitation of drawing force, the universality is also lowered and the specific surface area is also disadvantageous.
이에, 본 발명자들은 수산화칼륨 용액에 의한 안정황섬유의 전처리에 의하여 상기 여러가지 방법의 문제점을 해소하고 또한 산화성기체를 사용할 때보다 저온 및 단시간에 향상된 비표면적을 가지는 폴리아크릴로니트릴계 활성탄소섬유를 제조할 수 있는 방법을 대한민국특허출원95-23891호에 제안한 바 있다.Accordingly, the present inventors solve the problems of the various methods by pretreatment of stable sulfur fibers with a potassium hydroxide solution, and also the polyacrylonitrile-based activated carbon fibers having an improved specific surface area at a low temperature and a short time than when using an oxidizing gas The method that can be produced has been proposed in the Republic of Korea Patent Application No. 95-23891.
본 발명은 상기 대한민국 특허출원95-23891호의 방법에 의한 경우보다 활성탄소섬유의 흡착성능을 보다 개선시키기 위하여 연구와 실험을 행하고 그 결과에 근거하여 본 발명을 제안하게 된 것으로, 본 발명은 활성탄소 섬유의 제조시 수산화나트륨을 수용액 상태로 전처리하여 활성화 하므로서, 비표면적이 우수한 활성탄소섬유를 제공하고자 하는데, 그 목적이 있다.The present invention is to study and experiment to improve the adsorption performance of activated carbon fiber than in the case of the method of the Republic of Korea Patent Application No. 95-23891 and to propose the present invention based on the results, the present invention is activated carbon The purpose of the present invention is to provide activated carbon fibers having a specific surface area by activating sodium hydroxide by pretreatment in aqueous solution.
이하, 본 발명에 대하여 설명한다.EMBODIMENT OF THE INVENTION Hereinafter, this invention is demonstrated.
본 발명은 폴리아크릴로니트릴 섬유을 원료로 하여 활성탄소섬유를 제조하는 방법에 있어서, 상기 폴리아크릴로니트릴 섬유를 공기중에서 안정화시킨 후, 안정화된 섬유를 1-5M의 농도범위를 가지는 수산화나트륨 용액에 1시간 이상 침적시키고 이를 실온에서 100℃의 사이에서 건조시킨 다음, 이를 불활성 분위기에서 600℃-1000℃의 온도범위에서 15분 이상 열처리하고, 물로 세척 및 건조하는 것을 포함하여 이루어지는 활성탄소섬유의 제조방법에 관한 것이다.The present invention provides a method for producing activated carbon fibers using polyacrylonitrile fibers as a raw material, after stabilizing the polyacrylonitrile fibers in air, the stabilized fibers in a sodium hydroxide solution having a concentration range of 1-5M Preparation of activated carbon fiber comprising immersing for at least 1 hour and drying it at room temperature at 100 ° C., then heat-treating it at 600 ° C.-1000 ° C. for at least 15 minutes in an inert atmosphere, and washing and drying with water. It is about a method.
이하, 본 발명에 대하여 보다 상세히 설명한다.Hereinafter, the present invention will be described in more detail.
상기한 목적을 달성하기 위하여 본 발명에서는 먼저 원료인 폴리아크릴로니트릴 섬유를 공기중에서 안정화시킨 섬유를 1-5M의 농도범위를 가지는 수산화나트륨 용액에 1시간이상 침적시킨후 실온에서 100℃의 온도범위에서 건조시킴이 바람직한데, 그 이유는 다음과 같다.In order to achieve the above object, in the present invention, a fiber obtained by stabilizing a polyacrylonitrile fiber as a raw material in air is first immersed in a sodium hydroxide solution having a concentration range of 1-5 M for at least 1 hour, and then at room temperature to 100 ° C. Drying is preferable because of the following reasons.
전처리에 사용되는 수산화나트륨용액의 농도는 1M-5M의 농도범위인 것이 바람직한데, 이것은 1M이하의 농도에 의한 처리에 있어서는 충분한 반응이 이루어지지 않으므로 충분히 활성화가 이루어지지 않기 때문에 제품의 비표면적이 활성탄소섬유로서 어려울 정도의 작은 비표면적을 갖기 때문이다.The concentration of sodium hydroxide solution used in the pretreatment is preferably in the concentration range of 1M-5M. This is because the specific surface area of the product is not active because sufficient reaction does not occur in the treatment by the concentration below 1M. This is because the carbon fiber has a small specific surface area that is difficult.
그리고 5M이상인 경우에는 수산화나트륨용액 처리하여 건조한 안정화 섬유를 그대로 불활성 분위기에서 열처리할 경우 활성화 반응은 진행되지만 섬유표면이 지나치게 반응되어 쉽게 부스러지므로 활성탄소섬유로서 사용하기 어렵기 때문이다.In the case of 5M or more, the activation reaction proceeds when the dried stabilizing fiber is heat treated in an inert atmosphere by treating with sodium hydroxide solution, but it is difficult to use as activated carbon fiber because the fiber surface is excessively reacted and brittle.
안정화된 섬유를 수산화나트륨용액에 1시간 이상 침적시키는 것은 수산화나트륨이 안정화섬유에 충분히 부착하고 내부로 확산시키기 위해서이다. 침적시에는 초음파등의 보조수단을 사용하면 그 이하의 시간에서도 가능하다.The stabilized fiber is deposited in the sodium hydroxide solution for at least 1 hour in order for the sodium hydroxide to adhere sufficiently to the stabilized fiber and to diffuse inside. At the time of deposition, it is possible to use the auxiliary means such as the ultrasonic wave in less time.
건조시에는 100℃이상의 온도에서는 섬유가 산화되기 쉬우므로 실온에서 100℃이하의 온도에서 건조시키는 것이 바람직하다.At the time of drying, since a fiber is easy to oxidize at the temperature of 100 degreeC or more, it is preferable to dry at the temperature of 100 degreeC or less at room temperature.
본 발명에서 안정화된 섬유를 침적시키는 용액으로 수산화나트륨을 선택한 것은 기존에 제안된 수산화칼륨에 비하여 안정화 섬유와의 반응성이 크므로 비표면적이 보다 향상된 활성탄소섬유를 제조할 수 있기 때문이다.Sodium hydroxide is selected as a solution for depositing stabilized fibers in the present invention because it is more reactive with stabilized fibers than conventionally proposed potassium hydroxide because it can produce activated carbon fibers with improved specific surface area.
상기와 같은 조건으로 건조된 섬유는 불활성 분위기하에서 600-1000℃의 온도범위에서 열처리한 다음, 세척 및 건조하여 본 발명의 활성탄소섬유를 제조함이 바람직한데, 그 이유는 다음과 같다.The fiber dried under the above conditions is preferably heat-treated at 600-1000 ° C. under an inert atmosphere, and then washed and dried to produce the activated carbon fiber of the present invention. The reason is as follows.
수산화나트륨 침적한 안정화섬유는 불활성분위기에서 600℃-1000℃의 온도범위에서 열처리를 하는 것이 바람직한데, 이것은 600℃이하의 온도에서 활성화 반응의 속도가 작으므로 활성화를 수시간 이상 매우 길게 행해 주어야 하므로 에너지 소모면에서 비경제적인 것이 되므로 불리하며, 1000℃이상의 온도에서는 반응이 매우 빨리 일어나므로 반응의 조절이 곤란해져 제품의 품질이 저하될 우려가 있기 때문이다.Sodium hydroxide deposited stabilizing fibers are preferably heat treated in an inert atmosphere at a temperature range of 600 ° C.-1000 ° C. Since the rate of activation reaction is small at temperatures below 600 ° C., the activation should be carried out for several hours or longer. It is disadvantageous because it is uneconomical in terms of energy consumption, and because the reaction occurs very quickly at a temperature of 1000 ° C. or higher, it is difficult to control the reaction, which may lower the product quality.
활성화처리 후에는 물로 세척하여 섬유에 부착된 수산화나트륨을 완전히 제거하여야 하는데 이것은 수산화나트륨이 섬유에 남아 있을때 향후 활용면에서 제약이 따를 수 있기 때문이나, 산성기체등의 처리등에 이용하는 것처럼 완전히 제거하지 않고 일부만을 제거한 상태로 사용하여도 유리한 경우등 활용목적에 적합하게 세척을 행하는 것이 바람직하다.After the activation treatment, the sodium hydroxide attached to the fiber should be completely removed by washing with water. This is because when sodium hydroxide remains in the fiber, it may be restricted in the future, but it is not completely removed as used for treatment of acid gas. It is preferable to perform the washing suitably for the purpose of use, such as in the case where it is advantageous to use only a part removed.
이하, 실시예를 통하여 본 발명을 보다 구체적으로 설명한다.Hereinafter, the present invention will be described in more detail with reference to Examples.
[실시예1]Example 1
폴리아크릴니트릴 섬유를 공기중에서 230℃에서 25시간 안정화한 안정화 섬유를 1M수산화나트륨용액에 24시간 침적시킨 것을 60℃에서 2시간 건조한 다음 700℃에서 30분간 질소분위기에서 열처리를 하여 초음파중에서 물로 세척하고 건조한 결과, 수율이 63.5％이고 비표면적이 764㎡/g인 활성탄소섬유를 제조할 수 있었다.After stabilizing the polyacrylonitrile fiber in air for 24 hours at 230 ° C., stabilized fibers were immersed in 1M sodium hydroxide solution for 24 hours, dried at 60 ° C. for 2 hours, heat-treated at 700 ° C. for 30 minutes in nitrogen atmosphere, and washed with water in ultrasonic wave. As a result of the drying, an activated carbon fiber having a yield of 63.5% and a specific surface area of 764 m 2 / g could be produced.
[실시예2]Example 2
상기 실시예1의 안정화섬유를 2M수산화나트륨용액에 24시간 침적하고 이것을 상기 실시예1과 동일하게 처리한 결과, 수율이 35％이며 비표면적이 2040㎡/g인 활성탄소섬유를 제조할 수 있었다.The stabilized fiber of Example 1 was immersed in 2M sodium hydroxide solution for 24 hours and treated in the same manner as in Example 1, whereby an activated carbon fiber having a yield of 35% and a specific surface area of 2040 m 2 / g could be prepared. .
[비교예1]Comparative Example 1
상기 실시예1의 안정화섬유를 2M수산화칼륨용액에 24시간 침적하고 이것을 상기 실시예1과 동일하게 처리한 결과, 수율이27％이며 비표면적이 165㎡/g인 활성탄소섬유를 제조할 수 있었다.The stabilizing fiber of Example 1 was immersed in 2M potassium hydroxide solution for 24 hours and treated in the same manner as in Example 1, whereby an activated carbon fiber having a yield of 27% and a specific surface area of 165 m 2 / g could be prepared. .
[비교예2]Comparative Example 2
상시 실시예1의 안정화 섬유르 830℃에서 30분간 수증기로 활성화하여 활성탄소성유를 제조한 결과, 수율이 12％이며 비표면적이 760㎡/g인 활성탄소섬유를 제조할 수 있었다.Activated carbonaceous oil was prepared by activating the stabilizing fibers of Example 1 with steam at 830 ° C. for 30 minutes. As a result, activated carbon fibers having a yield of 12% and a specific surface area of 760 m 2 / g could be prepared.
[실시예3]Example 3
상기 실시예1의 안정화섬유를 3M수산화나트륨용액에 24시간 침적하고 이것을 상기 실시예1과 동일하게 처리한 결과, 수율이 32.8％이며 비표면적이 2295㎡/g인 활성탄소섬유를 제조할 수 있었다.The stabilizing fiber of Example 1 was immersed in 3M sodium hydroxide solution for 24 hours and treated in the same manner as in Example 1, whereby an activated carbon fiber having a yield of 32.8% and a specific surface area of 2295 m 2 / g could be prepared. .
[비교예3]Comparative Example 3
상기 실시예1의 안정화섬유를 3M수산화칼륨용액에 24시간 침적하고 이것을 상기 실시예1과 동일하게 처리한 결과, 수율이 35.2％이며 비표면적이 1908㎡/g인 활성탄소섬유를 제조할 수 있었다.The stabilizing fiber of Example 1 was immersed in 3M potassium hydroxide solution for 24 hours and treated in the same manner as in Example 1, whereby an activated carbon fiber having a yield of 35.2% and a specific surface area of 1908 m 2 / g could be prepared. .
[비교예4]Comparative Example 4
상기 실시예1의 안정화섬유를 0.5M수산화나트륨용액에 24시간 침적하고 이것을 상기 실시예1과 동일하게 처리한 결과, 수율이 63％이며 비표면적이 146㎡/g인 물성을 나타내는 섬유가 제조되었다.The stabilizing fiber of Example 1 was immersed in 0.5 M sodium hydroxide solution for 24 hours and treated in the same manner as in Example 1, whereby a fiber having physical properties of 63% yield and a specific surface area of 146 m 2 / g was prepared. .
상술한 바와같이, 본 발명은 폴리아크릴로니트릴 섬유를 원료로 하여 활성탄소섬유를 제조시 공기중에서 안정화시킨 폴리아크릴로니트릴 섬유를 수산화나트륨용액에 침적하여 건조시키고 불활성분위기에서 열처리하여 활성화 하므로서, 비표면적이 커 흡착성능이 우수한 활성탄소섬유를 제조할 수 있는 효과가 있다.As described above, the present invention is produced by activating polyacrylonitrile fiber stabilized in air when preparing activated carbon fiber by using polyacrylonitrile fiber as a raw material by dipping in sodium hydroxide solution and drying and heat treatment in an inert atmosphere. The surface area is large, there is an effect capable of producing an activated carbon fiber excellent in adsorption performance.
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| WO2015065034A1 (en) * | 2013-10-29 | 2015-05-07 | 코오롱인더스트리 주식회사 | Activated carbon fiber and preparation method therefor |
| CN105683428A (en) * | 2013-10-29 | 2016-06-15 | 可隆工业株式会社 | Activated carbon fiber and preparation method therefor |
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| KR100396078B1 (en) * | 1999-08-24 | 2003-08-27 | 재단법인 포항산업과학연구원 | Activated carbon fiber compounded with zeolite and fabricating method thereof |
| CN111235698B (en) * | 2020-03-24 | 2022-09-23 | 北华大学 | Preparation method and application of nitrogen-doped porous carbon fiber material |
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| WO2015065034A1 (en) * | 2013-10-29 | 2015-05-07 | 코오롱인더스트리 주식회사 | Activated carbon fiber and preparation method therefor |
| CN105683428A (en) * | 2013-10-29 | 2016-06-15 | 可隆工业株式会社 | Activated carbon fiber and preparation method therefor |
| JP2016535175A (en) * | 2013-10-29 | 2016-11-10 | コーロン インダストリーズ インク | Activated carbon fiber and method for producing the same |
| CN105683428B (en) * | 2013-10-29 | 2019-02-19 | 可隆工业株式会社 | Activated carbon fibre and preparation method thereof |
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