KR20010016595A - Preparation method and use of Metal(Cu, Zn, Cr, v, Mo, Ti, Fe etc)-Impregnated activated carbon fiber for removal of toxicity, noxious gas - Google Patents
Preparation method and use of Metal(Cu, Zn, Cr, v, Mo, Ti, Fe etc)-Impregnated activated carbon fiber for removal of toxicity, noxious gas Download PDFInfo
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- 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
- D01F9/145—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues
- D01F9/155—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from pitch or distillation residues from petroleum pitch
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- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/02—Heat treatment
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- D—TEXTILES; PAPER
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- 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
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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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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Abstract
Description
본 발명은 금속 함유 및 금속 첨착 활성탄소섬유를 이용한 독성 및 유해성 가스의 제거를 위한 것으로, 군사용으로 사용되는 독성 가스로부터 호흡기를 보호해 주는 흡착제로서 방독면의 정화통에 충전하여 사용할 수 있을 뿐만 아니라 일반 산업시설에서 발생되는 황화수소, 염소가스 등과 같은 유해성가스를 효과적으로 제거하기 위하여 흡착탑에 충전하여 사용할 수 있는 흡착제거용 금속 함유 및 금속 첨착 활성탄소섬유의 제조방법과 그 용도에 관한 것이다.The present invention is for the removal of toxic and harmful gases using metal-containing and metal-impregnated activated carbon fibers, as an adsorbent to protect the respiratory organs from toxic gases used for military purposes, as well as filling the gas tank of the gas mask can be used in general industry The present invention relates to a method for preparing adsorption-removing metal-containing and metal-impregnated activated carbon fibers that can be used in an adsorption tower to effectively remove harmful gases such as hydrogen sulfide, chlorine gas, and the like, and their use.
군사용으로 사용되는 독성 가스로는 혈액작용제, 신경작용제, 질식작용제, 수포작용제가 있다. 이들 독성가스를 제거하기 위하여 2차 세계대전부터 활성탄에 은, 크롬, 구리를 첨착하여 사용하고 있으며, 황이나 인산을 첨착한 첨착활성탄은 암모니아 또는 아민같은 기체를 흡착하는데 이용되고 있다. 또한, 가성소다나 탄산나트륨, 요오드화칼륨이 첨착된 첨착활성탄은 황화수소, 메틸메르캅탄 가스를 흡착하는데 이용되고 있다. 그러나, 이들 첨착활성탄은 본 발명제품보다 흡착용량이 낮아 군사용 독성가스 제거를 위하여 정화통에 충진하였을 경우, 원하는 정화성능을 발휘하기 위해서는 전체적으로 두께가 두껍고 무게가 무거워지게 되어 방독면을 착용하였을 때 행동에 지장을 주게 되는 등 불편함이 크다. 또한, 일반 산업시설에서 사용되는 흡착탑에 충진하였을 경우는 충진량이 많아 흡착탑이 커지며 이에 따라 유지비가 많아지는 등 많은 단점을 가지게 된다. 한편, 최근에 활성탄의 장점을 지니면서 흡착특성이 월등한 활성탄소섬유가 개발되어 다양한 분야에 수요를 창출하고 있다. 활성탄소섬유는 활성탄에 비해 기체상 오염물질의 제거효율이 우수하여 적은 양으로도 활성탄과 같은 흡착용량을 나타낼 수 있고 쉽게 재생하여 사용할 수 있다. 특히 금속을 첨착하면 선택적 흡착이 가능하다. 따라서 본 발명은 활성탄소섬유 제조시 금속을 각각 또는 혼합하여 함유시키거나, 첨착시킴으로써 독성 및 유해성 가스의 제거에 효과적인 흡착기능성 신소재의 제조방법 및 용도에 관한 것이다.Toxic gases used for military purposes include blood agents, nerve agents, choking agents, and blisters. In order to remove these toxic gases, World War II has been using silver, chromium and copper impregnated with activated carbon. Impregnated activated carbon impregnated with sulfur or phosphoric acid is used to adsorb gases such as ammonia or amine. In addition, impregnated activated carbon impregnated with caustic soda, sodium carbonate or potassium iodide is used to adsorb hydrogen sulfide and methyl mercaptan gas. However, these impregnated activated carbons have a lower adsorption capacity than the present invention, so that when they are filled in the septic tank to remove toxic gas for military use, the overall thickness becomes heavy and heavy to show the desired purification performance. The discomfort is great. In addition, in the case of being filled in the adsorption tower used in the general industrial facilities, there are many disadvantages such as a large amount of filling and a large adsorption tower, thereby increasing the maintenance cost. Meanwhile, recently, activated carbon fibers having the advantages of activated carbon and superior adsorption characteristics have been developed to create demand in various fields. Activated carbon fiber has better removal efficiency of gaseous contaminants than activated carbon, so it shows the same adsorption capacity as activated carbon and can be easily recycled and used. In particular, by adhering metal, selective adsorption is possible. Therefore, the present invention relates to a method for producing and using an adsorption functional new material which is effective in removing toxic and harmful gases by incorporating or impregnating metals in the production of activated carbon fibers, or by impregnating them.
본 발명은 핏치에 금속을 적정량 첨가하여 용융방사한 후 산화, 탄화, 스팀 활성화를 거쳐 표면적이 넓고, 흡착력이 매우 우수한 섬유상 흡착제(활성탄소섬유)의 발명과 동시에 일반 활성탄소섬유에 금속을 첨착시킴으로써 특정 유해가스에 알맞은 흡착제를 제조하고자 한다. 또한, 그의 미세공 평균직경을 기존 활성탄소섬유보다 확대시켜 촉매의 담체로 사용할 수 있도록 하며 여러 금속을 첨가하여 다양한 종류의 독성 및 유해성 가스에 알맞는 흡착제를 제조하고 응용하는 기술을 포함한다.In the present invention, by adding a proper amount of metal to the pitch and melt spinning, through the oxidation, carbonization, and steam activation, the surface area is wide and the adsorption power of the fibrous adsorbent (activated carbon fiber) at the same time by attaching the metal to the general activated carbon fiber It is intended to prepare an adsorbent suitable for a specific harmful gas. In addition, the micropore average diameter of the active carbon fiber is expanded to be used as a carrier of the catalyst, and various metals are added to include various techniques for preparing and applying adsorbents suitable for various types of toxic and harmful gases.
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원료핏치의 개질, 개질핏치와 각각의 금속 산화물 또는 여러 가지 금속 산화물이 혼합된 것, 혼합 핏치의 용융방사, 방사섬유의 산화공정, 활성화공정으로 구성되어 있다.It consists of the modification of the raw material pitch, the mixture of the modified pitch and each metal oxide or various metal oxides, the melt spinning of the mixed pitch, the oxidation process of the spinning fiber, and the activation process.
분자량 분포가 일정하고, 연화점이 높은 핏치에 일정농도의 금속산화물 각각 또는 혼합하여 첨가하고 용융방사가 잘 되도록 혼합한다. 용융방사된 핏치섬유는 산화공정을 거쳐 불융화되고, 탄화공정을 거쳐 탄소섬유로 만든다. 이 금속 함유 탄소섬유를 고온의 질소와 스팀 혼합가스로 활성화하여 다공성 섬유상 흡착제를 제조하게 된다. 흡착능력은 비표면적이 크고, 미세공이 표면에 노출되어 있어야 하므로 활성화시에 온도와 시간 및 스팀의 혼합비율을 조절하여 여러 등급의 금속 함유 활성탄소섬유를 제조할 수 있으며, 금속산화물의 조합에 따라 여러 종류의 활성탄소섬db를 제조할 수 있다.The molecular weight distribution is constant, and each pitch or a mixture of metal oxides is added to the pitch with a high softening point, and mixed so as to melt melt spinning well. The melt-spun pitch fibers are infused through an oxidation process and carbonized through a carbonization process. This metal-containing carbon fiber is activated with hot nitrogen and steam mixed gas to produce a porous fibrous adsorbent. Adsorption capacity has a large specific surface area and micropores should be exposed on the surface, so it is possible to manufacture various grades of metal-containing activated carbon fibers by controlling the mixing ratio of temperature, time and steam at the time of activation. Various kinds of activated carbon island db can be prepared.
이하, 본 발명의 바람직한 실시 예에 따른 독성 및 유해성 가스의 제거 및 정수, 촉매를 위한 금속(Cu, Zn, Cr, v, Mo, Ti, Fe 등) 함유 및 금속 첨착 활성탄소섬유의 제조방법에 대하여 설명한다.Hereinafter, to remove and purify toxic and harmful gases according to a preferred embodiment of the present invention, containing metals (Cu, Zn, Cr, v, Mo, Ti, Fe, etc.) for the catalyst and the method of producing metal-impregnated activated carbon fibers Explain.
실시 예Example
1. NCB(Naphtha Cracking Bottom) oil을 개질반응기에 넣고 약 400℃까지 열처리하면서 개질하여 등방성의 전구체(precursor)핏치를 얻는다. 여기에 Cr 화합물을 각각 0.1wt%∼20wt%가 되도록 첨가하고 완전히 혼합한다. 이 혼합물을 250℃∼450℃에서 방사하여 핏치섬유를 얻는다. 이 핏치섬유를 공기중의 산소를 이용하여 산화공정을 거침으로서 불융화하고, 800℃∼1700℃에서 탄화하여 탄소섬유를 얻는다. 이 탄소섬유를 700℃∼1500℃에서 질소와 스팀의 혼합가스로 활성화하여 Cr 함유 활성탄소섬유를 제조한다. 제조된 ACF를 반응관에 넣고 일정농도의 신경 모의 작용제, 혈액 모의 작용제, 황화수소 가스 등을 이용하여 실험을 실시하며, 반응관을 통과한 가스의 농도는 GC(Gas Chromatograph; FID,TCD,FPD)를 이용하여 확인한다.1. Put Naphtha Cracking Bottom (NCB) oil in the reforming reactor and heat-treat it to about 400 ℃ to obtain isotropic precursor pitch. Cr compounds are added to 0.1 wt% to 20 wt%, respectively, and mixed thoroughly. This mixture is spun at 250 ° C to 450 ° C to obtain pitch fibers. This pitch fiber is infusified by undergoing an oxidation step using oxygen in the air, and carbonized at 800 ° C to 1700 ° C to obtain carbon fiber. The carbon fiber is activated with a mixed gas of nitrogen and steam at 700 ° C to 1500 ° C to produce Cr-containing activated carbon fiber. Put the prepared ACF into the reaction tube and conduct experiment using a certain concentration of nerve simulation agent, blood simulation agent, hydrogen sulfide gas, etc., and the concentration of gas passing through the reaction tube is GC (Gas Chromatograph; FID, TCD, FPD) Check with.
2. NCB(Naphtha Cracking Bottom) oil을 개질반응기에 넣고 약 400℃까지 열처리하면서 개질하여 등방성의 전구체(precursor)핏치를 얻는다. 여기에 Ag, Cu, Cr 화합물을 각각 0.1wt%∼20wt%가 되도록 첨가하고 완전히 혼합한다. 이 혼합물을 250℃∼450℃에서 방사하여 핏치섬유를 얻는다. 이 핏치섬유를 공기중의 산소를 이용하여 산화공정을 거침으로서 불융화하고, 800℃∼1700℃에서 탄화하여 탄소섬유를 얻는다. 이 탄소섬유를 700℃∼1500℃에서 질소와 스팀의 혼합가스로 활성화하여 Ag, Cu, Cr 함유 활성탄소섬유를 제조한다. 제조된 ACF를 반응관에 넣고 일정농도의 신경 모의 작용제, 혈액 모의 작용제, 황화수소 가스 등을 이용하여 실험을 실시하며, 반응관을 통과한 가스의 농도는 GC(Gas Chromatograph; FID,TCD,FPD)를 이용하여 확인한다.2. Put Naphtha Cracking Bottom (NCB) oil in the reforming reactor and heat-treat it to about 400 ℃ to obtain isotropic precursor pitch. Ag, Cu, and Cr compounds are added thereto so as to be 0.1wt% to 20wt%, and mixed thoroughly. This mixture is spun at 250 ° C to 450 ° C to obtain pitch fibers. This pitch fiber is infusified by undergoing an oxidation step using oxygen in the air, and carbonized at 800 ° C to 1700 ° C to obtain carbon fiber. The carbon fiber is activated with a mixed gas of nitrogen and steam at 700 ° C to 1500 ° C to produce Ag, Cu, Cr-containing activated carbon fiber. Put the prepared ACF into the reaction tube and conduct experiment using a certain concentration of nerve simulation agent, blood simulation agent, hydrogen sulfide gas, etc., and the concentration of gas passing through the reaction tube is GC (Gas Chromatograph; FID, TCD, FPD) Check with.
3. 활성탄소섬유(ACF)1.5g 을 105℃의 오븐에서 24시간 이상 건조시킨 다음 증류수 200㎖∼300㎖에 3wt%∼15wt%의 금속 산화물을 교반기에서 녹인다. 그런 후에, 비이커에 건조된 ACF를 넣고, 금속 산화물을 녹인 증류수를 부어준다. 1∼10시간동안 첨착시킨 후, 진공펌프를 이용하여 수분을 제거시키고 첨착된 ACF를 오븐에 넣고, 24시간이상 건조시킨다. 건조된 ACF를 반응관에 넣고 일정농도의 신경 모의 작용제, 혈액 모의 작용제, 황화수소 가스 등을 이용하여 실험을 실시하며, 반응관을 통과한 가스의 농도는 GC(Gas Chromatograph; FID,TCD,FPD)를 이용하여 확인한다.3. After 1.5 g of activated carbon fiber (ACF) is dried in an oven at 105 ° C. for at least 24 hours, 3 wt% to 15 wt% of metal oxide is dissolved in 200 ml to 300 ml of distilled water in a stirrer. After that, the dried ACF is placed in a beaker and distilled water in which the metal oxide is dissolved is poured. After 1 to 10 hours of deposition, the water is removed using a vacuum pump and the attached ACF is placed in an oven and dried for at least 24 hours. The dried ACF is placed in a reaction tube and experimented with a certain concentration of nerve simulation agent, blood simulation agent, hydrogen sulfide gas, etc., and the concentration of the gas passing through the reaction tube is GC Check with.
전술한 바와 같은 본 발명은 군사용으로 사용되는 방독 마스크 정화통의 성능을 향상시키고 무게를 줄임으로써 방독면을 착용하였을 경우 행동에 지장을 주게되는 불편을 덜 수 있을 것이다. 또한, 현재 군에서 사용되는 방독 마스크 정화통은 화학작용제의 종류에 따라 특정 정화통으로 교체해야 하는데 본 발명을 이용하므로써 기존의 정화통 크기로 여러 작용제를 동시에 제거할 수 있는 정화통을 만들 수 있다.As described above, the present invention may reduce the inconvenience of disturbing the behavior when wearing a gas mask by improving the performance and reducing the weight of the gas mask cleaning container used for military use. In addition, the gas mask mask can be used in the present group should be replaced with a specific filter according to the type of chemical agent, by using the present invention can be made of a container that can remove several agents at the same size of the existing container at the same time.
또한, 일반 산업시설에서 발생되는 황화수소, 염소가스 등을 제거하기 위해 흡착능이 우수한 금속 함유 활성탄소섬유 및 금속 첨착 활성탄소섬유를 사용하므로 일반 활성탄소섬유나 첨착활성탄에 비해 운전시간을 수십배 이상 증가시킬 수 있으며, 충진량이 줄여 소형의 흡착탑을 이용하므로 이에 따른 유지비를 줄일 수 있다.In addition, the use of metal-containing activated carbon fibers and metal-impregnated activated carbon fibers with excellent adsorptive capacity to remove hydrogen sulfide, chlorine gas, etc., generated in general industrial facilities, can increase operating time by several orders of magnitude more than ordinary activated carbon fibers or impregnated activated carbon. In addition, since the filling amount is reduced, a small adsorption tower may be used, thereby reducing maintenance costs.
또한, 금속 함유 활성탄소섬유 및 금속 첨착 활성탄소섬유는 기존의 첨착활성탄에 비해 흡착능력이 우수하고 장기간 사용이 가능하므로 흡착제의 교체주기를 연장하며, 재생 사용이 가능하여 폐흡착제의 발생으로 인한 폐기물의 양을 감소할 수 있다.In addition, metal-containing activated carbon fibers and metal-impregnated activated carbon fibers have better adsorption capacity and can be used for a longer period of time than conventional impregnated activated carbons, thus extending the replacement cycle of the adsorbent and recycling the waste due to the generation of waste adsorbents. Can reduce the amount of
또한, 금속 입자를 포함시켜 미세공의 크기를 중기공 규모로 확대하여 분자량이 큰 물질도 효과적으로 분리할 수 있으므로 환경오염물질의 흡착제거에 탁월한 효과를 보일 것이다.In addition, by including the metal particles to increase the size of the micropores to the mesoporous scale, it is possible to effectively separate the material having a large molecular weight will have an excellent effect on the adsorption removal of environmental pollutants.
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Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR20020087917A (en) * | 2002-10-26 | 2002-11-23 | 유승곤 | A ctivated Carbon Fiber Lined NBC Protection Clothing/ Protective Cloth for Removal of Toxic Gases and Chemical Warfare Agents. |
KR20030022642A (en) * | 2001-09-11 | 2003-03-17 | 오원춘 | Activated carbon fiber having improved antibacterial characteristics |
KR100407806B1 (en) * | 2001-07-20 | 2003-11-28 | 재단법인 포항산업과학연구원 | ACTIVATED CARBON FIBER CATALYST FOR REMOVAL OF SOx AND PREPARATION METHOD OF THE SAME |
KR100490831B1 (en) * | 2002-09-05 | 2005-05-19 | (주)카보닉스 | METHOD OF PREPARING CATALYST FOR REMOVAL OF NOx |
KR100490832B1 (en) * | 2002-09-05 | 2005-05-19 | (주)카보닉스 | Method of preparing catalyst for removal of nox |
KR100558895B1 (en) * | 2004-08-05 | 2006-03-10 | 한국항공우주연구원 | Adsorbents for organic sulfur compounds, Method for manufacturing them and Method for desulfurizing of town gas using them |
KR20080057449A (en) * | 2006-12-20 | 2008-06-25 | 재단법인 포항산업과학연구원 | Preparation method of activated carbon fiber based catalyst for removal of nox and activated carbon fiber based catalyst repared thereby |
KR101486238B1 (en) * | 2012-10-25 | 2015-01-27 | (주)기련이엔씨 | Manufacturing method of metal impregnated active carbon fiber for target solvent voc killing |
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JPS51130327A (en) * | 1975-05-08 | 1976-11-12 | Toyobo Co Ltd | Activated carbon fibers containing metallic oxide |
JPS6485137A (en) * | 1987-09-26 | 1989-03-30 | Osaka Gas Co Ltd | Active carbon fiber capable of adsorbing nitric oxide and manufacture thereof |
JPH09296328A (en) * | 1996-05-07 | 1997-11-18 | Petoca:Kk | Microbicidal activated carbon fiber and its production |
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JPS51130327A (en) * | 1975-05-08 | 1976-11-12 | Toyobo Co Ltd | Activated carbon fibers containing metallic oxide |
JPS6485137A (en) * | 1987-09-26 | 1989-03-30 | Osaka Gas Co Ltd | Active carbon fiber capable of adsorbing nitric oxide and manufacture thereof |
JPH09296328A (en) * | 1996-05-07 | 1997-11-18 | Petoca:Kk | Microbicidal activated carbon fiber and its production |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
KR100407806B1 (en) * | 2001-07-20 | 2003-11-28 | 재단법인 포항산업과학연구원 | ACTIVATED CARBON FIBER CATALYST FOR REMOVAL OF SOx AND PREPARATION METHOD OF THE SAME |
KR20030022642A (en) * | 2001-09-11 | 2003-03-17 | 오원춘 | Activated carbon fiber having improved antibacterial characteristics |
KR100490831B1 (en) * | 2002-09-05 | 2005-05-19 | (주)카보닉스 | METHOD OF PREPARING CATALYST FOR REMOVAL OF NOx |
KR100490832B1 (en) * | 2002-09-05 | 2005-05-19 | (주)카보닉스 | Method of preparing catalyst for removal of nox |
KR20020087917A (en) * | 2002-10-26 | 2002-11-23 | 유승곤 | A ctivated Carbon Fiber Lined NBC Protection Clothing/ Protective Cloth for Removal of Toxic Gases and Chemical Warfare Agents. |
KR100558895B1 (en) * | 2004-08-05 | 2006-03-10 | 한국항공우주연구원 | Adsorbents for organic sulfur compounds, Method for manufacturing them and Method for desulfurizing of town gas using them |
KR20080057449A (en) * | 2006-12-20 | 2008-06-25 | 재단법인 포항산업과학연구원 | Preparation method of activated carbon fiber based catalyst for removal of nox and activated carbon fiber based catalyst repared thereby |
KR101486238B1 (en) * | 2012-10-25 | 2015-01-27 | (주)기련이엔씨 | Manufacturing method of metal impregnated active carbon fiber for target solvent voc killing |
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