KR100584251B1 - Manufacturing method of activated carbon from high carbon contents fly ash by using combinated benefication process - Google Patents
Manufacturing method of activated carbon from high carbon contents fly ash by using combinated benefication process Download PDFInfo
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- KR100584251B1 KR100584251B1 KR1020030077016A KR20030077016A KR100584251B1 KR 100584251 B1 KR100584251 B1 KR 100584251B1 KR 1020030077016 A KR1020030077016 A KR 1020030077016A KR 20030077016 A KR20030077016 A KR 20030077016A KR 100584251 B1 KR100584251 B1 KR 100584251B1
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- C01B32/00—Carbon; Compounds thereof
- C01B32/30—Active carbon
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- C01B32/318—Preparation characterised by the starting materials
- C01B32/33—Preparation characterised by the starting materials from distillation residues of coal or petroleum; from petroleum acid sludge
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
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- C01B32/336—Preparation characterised by gaseous activating agents
Abstract
본 발명은 공기분급 후, 부유선광하는 복합정제공정에 의해 석탄회로부터 고품위의 미연분을 분리하고, 이를 활성화시키는 복합정제공정에 의한 고탄소 석탄회로부터의 활성탄의 제조방법에 관한 것으로서, 석탄회로부터 미연분을 분리하여 수증기활성화시켜 활성탄을 제조함에 있어서, (1) 석탄회를 공기분급법에 의해 공기분급한 후, 공기분급에 의해 분리회수된 1차회수물을 다시 기포제로 파인오일 또는 메틸이소부틸카비놀(MIBC ; methylisobutylcarbinol)을 사용하고, 포집제로서 폐식용유를 사용하여 부유선광하여 포집된 2차회수물을 수집하는 복합정제공정에 의한 복합정제단계; (2) 상기 복합정제단계에서 수득된 2차회수물에 야자각 또는 유연탄 등의 탄소원을 더 혼합한 후, 이를 탄화시키는 탄화단계; 및 (3) 상기 탄화단계에서 탄화된 탄화물을 수증기활성화시키는 활성화단계;들을 포함하여 이루어짐을 특징으로 한다.The present invention relates to a method for producing activated carbon from high carbon coal ash by a complex purification process in which a high-quality fine powder is separated from coal ash by a complex refining process of flotation after air classification, and activated. In the production of activated charcoal by separating and steam activating, (1) the coal ash was classified by air by air classification method, and then the primary recovery product separated and recovered by air classification was again used as a foaming agent for fine oil or methyl isobutyl carbinol. A complex refining step using a complex refining process using (MIBC; methylisobutylcarbinol) and collecting the collected secondary collection by flotation using waste cooking oil as a collecting agent; (2) a carbonization step of further mixing a carbon source such as coconut shell or bituminous coal into the secondary recovery product obtained in the complex purification step, and then carbonizing it; And (3) an activation step of steam activating the carbide carbonized in the carbonization step.
석탄회, 플라이애쉬, 공기분급, 부유선광, 복합정제공정, 활성탄Fly ash, fly ash, air classification, flotation, combined refining process, activated carbon
Description
본 발명은 복합정제공정에 의한 고탄소 석탄회로부터의 활성탄의 제조방법에 관한 것이다. 보다 상세하게는 본 발명은 공기분급 후, 부유선광하는 복합정제공정에 의해 석탄회로부터 고품위의 미연분을 분리하고, 이를 활성화시키는 복합정제공정에 의한 고탄소 석탄회로부터의 활성탄의 제조방법에 관한 것이다.The present invention relates to a method for producing activated carbon from high carbon coal ash by a complex refining process. More specifically, the present invention relates to a method for producing activated carbon from high carbon coal ash by a complex refining process by separating high-grade fine dust from coal ash by a complex refining process by flotation after air classification.
활성탄은 유기물이나 무기물과 같은 오염물질을 제거하기 위한 필터용 등으로 활용되고 있다. 활성탄은 넓은 표면적, 특징적인 기공 크기, 기공의 형상, 기공들의 분포, 고흡착용량, 표면의 화학적인 특성 등의 여러 특성들을 가지기 때문에 흡착성 증대에 영향을 주는 것으로 밝혀졌다. 또한, 이들 특성들을 이용하여 독특하고 다양한 흡착제로 사용되어 왔으며, 여기에 화학적, 물리적 특성들을 부가하여 여러 화학공정들에 이용되고 있다.Activated carbon is used for filters for removing contaminants such as organics and inorganics. Activated carbon has been found to affect adsorption because it has various properties such as large surface area, characteristic pore size, pore shape, pore distribution, high adsorption capacity, and surface chemical properties. In addition, these properties have been used as unique and various adsorbents, and chemical and physical properties have been added to them and used in various chemical processes.
한편, 활성탄의 제조의 원료의 회수방법의 하나로 석탄회 정제공정에서 발생되는 고탄소 석탄회의 정제방법으로서 기존의 정제방법은 건식법과 습식법으로 대 별되어 사용되어 왔다. 건식법은 보편적으로 알려진 공기분급법으로, 습식법은 부유선광법으로 알려져 있으며, 각각 별도로 수행되어 왔다. 그러나, 이러한 종래의 건식법 또는 습식법은 단독으로는 고품위의 미연분의 분리가 어렵고, 효율이 낮으며, 그에 따라 수득되는 활성탄 역시 그 품위가 낮아 용도에 상당한 제한이 가해지는 단점이 있었다.On the other hand, as a method of recovering the raw materials for the production of activated carbon, as a method for refining high-carbon coal ash generated in the coal ash refining process, conventional refining methods have been used separately from dry and wet methods. The dry method is a commonly known air classification method, and the wet method is known as flotation, and has been performed separately. However, such a conventional dry method or wet method alone has a disadvantage in that it is difficult to separate fine ash of high quality, and its efficiency is low, and thus the activated carbon obtained as a result is of low quality and has a significant limitation on its use.
본 발명의 목적은 공기분급 후, 부유선광하는 복합정제공정에 의해 석탄회로부터 고품위의 미연분을 분리하고, 이를 활성화시키는 복합정제공정에 의한 고탄소 석탄회로부터의 활성탄의 제조방법을 제공하는 데 있다.It is an object of the present invention to provide a method for producing activated carbon from high carbon coal ash by a complex purification step of separating high-grade fine coal from coal ash by a complex refining process of flotation after air classification.
본 발명에 따른 복합정제공정에 의한 고탄소 석탄회로부터의 활성탄의 제조방법은, 석탄회로부터 미연분을 분리하여 수증기활성화시켜 활성탄을 제조함에 있어서, (1) 석탄회를 공기분급법에 의해 공기분급한 후, 공기분급에 의해 분리회수된 1차회수물을 다시 기포제로 파인오일 또는 메틸이소부틸카비놀(MIBC ; methylisobutylcarbinol)을 사용하고, 포집제로서 폐식용유를 사용하여 부유선광하여 포집된 2차회수물을 수집하는 복합정제공정에 의한 복합정제단계; (2) 상기 복합정제단계에서 수득된 2차회수물에 야자각 또는 유연탄 등의 탄소원을 더 혼합한 후, 이를 탄화시키는 탄화단계; 및 (3) 상기 탄화단계에서 탄화된 탄화물을 수증기활성화시키는 활성화단계;들을 포함하여 이루어진다.In the method for producing activated carbon from high carbon coal ash by the complex refining process according to the present invention, in the production of activated carbon by separating steam from coal ash and steam activation, (1) after classifying the coal ash by air classification method Secondary collections were collected by flotation using the primary oil recovered and separated by air classification as fine foaming oil or methylisobutylcarbinol (MIBC; methylisobutylcarbinol) as a collecting agent. Complex purification step by a complex purification process to collect the; (2) a carbonization step of further mixing a carbon source such as coconut shell or bituminous coal into the secondary recovery product obtained in the complex purification step, and then carbonizing it; And (3) an activation step of steam activating the carbide carbonized in the carbonization step.
이하, 본 발명을 구체적인 실시예를 참조하여 상세히 설명한다.Hereinafter, the present invention will be described in detail with reference to specific examples.
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본 발명에 따른 복합정제공정에 의한 고탄소 석탄회로부터의 활성탄의 제조방법은, 석탄회로부터 미연분을 분리하여 수증기활성화시켜 활성탄을 제조함에 있어서, (1) 석탄회를 공기분급법에 의해 공기분급한 후, 공기분급에 의해 분리회수된 1차회수물을 다시 기포제로 파인오일 또는 메틸이소부틸카비놀(MIBC ; methylisobutylcarbinol)을 사용하고, 포집제로서 폐식용유를 사용하여 부유선광하여 포집된 2차회수물을 수집하는 복합정제공정에 의한 복합정제단계; (2) 상기 복합정제단계에서 수득된 2차회수물에 야자각 또는 유연탄 등의 탄소원을 더 혼합한 후, 이를 탄화시키는 탄화단계; 및 (3) 상기 탄화단계에서 탄화된 탄화물을 수증기활성화시키는 활성화단계;들을 포함하여 이루어짐을 특징으로 한다.In the method for producing activated carbon from high carbon coal ash by the complex refining process according to the present invention, in the production of activated carbon by separating steam from coal ash and steam activation, (1) after classifying the coal ash by air classification method Secondary collections were collected by flotation using the primary oil recovered and separated by air classification as fine foaming oil or methylisobutylcarbinol (MIBC; methylisobutylcarbinol) as a collecting agent. Complex purification step by a complex purification process to collect the; (2) a carbonization step of further mixing a carbon source such as coconut shell or bituminous coal into the secondary recovery product obtained in the complex purification step, and then carbonizing it; And (3) an activation step of steam activating the carbide carbonized in the carbonization step.
상기 (1)의 복합정제단계는 석탄회를 공기분급법에 의해 공기분급한 후, 공기분급에 의해 분리회수된 1차회수물을 다시 기포제로 파인오일 또는 메틸이소부틸카비놀(MIBC ; methylisobutylcarbinol)을 사용하고, 포집제로서 폐식용유 또는 디젤유를 사용하여 부유선광하여 포집된 2차회수물을 수집하는 복합정제공정에 의하여 정제하는 단계로서, 공기분급에 의해 1차적으로 회분들을 제거하고, 미연분의 함량이 높은 1차회수물을 먼저 회수한 다음, 계속해서 상기 1차회수물을 부유선광에 의해 미연분을 더욱 정제하여 미연분의 함량을 높인 고탄소함량, 고품위의 미연분을 탄소원으로 수득하는 점에 특징이 있는 것이다. 상기에서 1차회수에 이용되 는 공기분급은 당업자에게는 공지된 통상의 공기분급기(air classifier)에 의한 다중 자연낙하 공기분급방식에 의하여 수행될 수 있다. 상기 다중 자연낙하 공기분급방식은 통상 조분, 미분 및 초미분의 3중 자연낙하 공기분급방식으로 수행될 수 있다. 이 다중 자연낙하 공기분급방식은 건식법의 대표적인 방법으로 다른 건식 공기분급장치 및 방법 또한 사용될 수 있음은 당업자에게는 당연히 이해될 수 있는 것이다. 또한, 상기 부유선광은 당업자에게는 공지된 통상의 포말부선공정이 사용될 수 있으며, 이를 위한 바람직한 부선기 형태는 공지의 덴버형(Denver Sub-B type) 부선기가 사용될 수 있으며, 이는 국내외 유수의 제조업자들에 의해 상용적으로 제공된느 것을 구입하여 사용할 수 있을 정도로 공지된 것이다. 상기 부유선광은 습식법의 대표적인 방법으로 다른 습식 부유선광장치 및 방법 또한 사용될 수 있음은 당업자에게는 당연히 이해될 수 있는 것이다. 특히, 상기 포집제로는 바람직하게는 폐식용유가 사용될 수 있다. 폐식용유는 음식의 조리 등에서 사용되고 난 후, 수집되는 것으로서, 경제적인 효용이 다한 것으로서, 주로 공업용 오일 및 재생연료 등의 원료로 사용되는 것으로서, 본 발명에서 포집제로 사용되는 경우, 생산비를 절감하면서도 미연분의 포집에 효과적으로 이용된다.In the complex refining step of (1), after classifying coal ash by air classification method, fine oil or methyl isobutyl carbinol (MIBC) is recovered as the foaming agent and the primary recovery water separated and recovered by air classification. It is purified by a complex refining process that collects the collected secondary recovery by flotation by using waste cooking oil or diesel oil as a collecting agent, and removes ashes by air classification. After recovering the primary recoveries with a high content of powder, the first recoverables are further purified by flotation to further refine the unburned fractions, and the high carbon content and the high quality unburned fractions are used as the carbon source. It is characteristic in the point obtained. The air classification used for the first recovery in the above may be performed by a multiple natural fall air classification method by a conventional air classifier known to those skilled in the art. The multiple natural fall air classification system may be performed by a triple natural drop air classification system of coarse powder, fine powder and ultra fine powder. It will be apparent to those skilled in the art that this multiple natural falling air classification system can also be used as a representative method of the dry method. In addition, the floating beneficiation may be used a conventional foam barge process known to those skilled in the art, the preferred barge type for this may be a known Denver sub-B type barge, which is a leading domestic and foreign manufacturers It is known enough to be able to purchase and use what is commercially provided by them. It will be apparent to those skilled in the art that the floating beneficiation may also be used with other wet flotation apparatuses and methods as a representative method of the wet process. In particular, as the collecting agent, waste cooking oil may be preferably used. The waste cooking oil is collected after being used in the cooking of food, and has been used economically. It is mainly used as a raw material for industrial oils and renewable fuels. It is effectively used for the collection of minutes.
상기 (2)의 활성화단계는 상기 복합정제단계에서 수득된 2차회수물을 탄화시키는 단계로서, 공지의 활성탄 제조에서의 탄화공정과 동일 또는 유사한 것으로서, 당업자에게는 용이하게 이해될 수 있는 것이다. 탄화단계는 탄소원에 무산소 또는 불충분한 산소 존재 조건 하에서 가열에 의해 탄소원으로부터 탄소의 함량을 높이는 것으로 이해될 수 있다. 상기 (2)의 탄화단계에서 상기 2차회수물에 야자각 또 는 유연탄 등의 탄소원을 더 혼합할 수 있다. 이들 야자각 또는 유연탄 등의 탄소원은 목적하는 활성탄의 품위의 조절 및 활성탄의 수율 등의 향상을 위해 임의의 양으로 첨가될 수 있으며, 바람직하게는 상기 2차회수물과 야자각 또는 유연탄 등의 탄소원은 등량으로 혼합될 수 있다.The activation step of (2) is a step of carbonizing the secondary recovery product obtained in the complex purification step, the same or similar to the carbonization process in the production of known activated carbon, which can be easily understood by those skilled in the art. The carbonization step can be understood to increase the content of carbon from the carbon source by heating under conditions of oxygen free or insufficient oxygen in the carbon source. In the carbonization step of (2), a carbon source such as coconut shell or bituminous coal may be further mixed with the secondary recovery water. These carbon sources, such as coconut shell or bituminous coal, may be added in any amount in order to control the quality of the activated activated carbon and to improve the yield of the activated carbon. Preferably, the secondary sources and carbon sources such as palm shell or bituminous coal are used. Silver may be mixed in equal amounts.
상기 (3)의 활성화단계는 상기 탄화단계에서 탄화된 탄화물을 수증기활성화시키는 단계로서, 공지의 활성탄 제조에서의 수증기활성화공정과 동일 또는 유사한 것으로서, 당업자에게는 용이하게 이해될 수 있는 것이다. 수증기활성화단계는 탄화물에 고온, 고압의 수증기를 공급한 후, 건조시켜 탄화물에 다량의 공극들을 형성시키는 것으로서, 이들 수증기활성화에 의한 공극들의 형성에 의해 활성탄 특유의 정제효과, 탈색효과, 탈취효과, 촉매효과 등이 발현될 수 있게 된다.The activation step of (3) is a step of steam activating the carbonized carbide in the carbonization step, the same or similar to the steam activation process in the production of known activated carbon, which can be easily understood by those skilled in the art. The steam activation step is to supply a high temperature and high pressure steam to the carbide, and then dry to form a large amount of pores in the carbide, by the formation of pores by the steam activation, the purification effect of the activated carbon, decolorizing effect, deodorizing effect, The catalytic effect can be expressed.
이하에서 본 발명의 바람직한 실시예 및 비교예들이 기술되어질 것이다.Hereinafter, preferred embodiments and comparative examples of the present invention will be described.
이하의 실시예들은 본 발명을 예증하기 위한 것으로서 본 발명의 범위를 국한시키는 것으로 이해되어져서는 안될 것이다.The following examples are intended to illustrate the invention and should not be understood as limiting the scope of the invention.
실시예 1Example 1
본 실시예에서 사용되는 비산회는 대한민국 서천 소재 석탄회 정제공장에서 수득한 것으로서, 이를 분석한 결과, 13.7%의 미연분(강열감량 기준)과 86.3%의 회분으로 구성됨을 확인하였다.The fly ash used in this example was obtained from a coal ash refining plant in Seocheon, Korea. As a result of the analysis, it was confirmed that the ash was composed of 13.7% unburned ash (based on the loss of ignition) and 86.3% ash.
상기 비산회를 우선 공기분급하였으며, 공기분급의 결과를 하기 표 1에 나타내었다.The fly ash was first classified into air, and the results of air classification are shown in Table 1 below.
상기 공기분급에서 조분으로 수득된 1차회수물을 원시료로 하여 하기 표 2의 조건에 따라 부유선광 하였으며, 그 결과를 하기 표 2에 나타내었다.The primary recovery obtained as a crude powder in the air classification as a raw material was flotation according to the conditions of Table 2 below, the results are shown in Table 2 below.
상기한 바에 의거, 본 발명에 따른 복합정제공정에 의해 미연분 함량 71 내지 76%의 고품위의 탄소원으로서의 미연분을 2차회수물로 회수할 수 있음을 확인할 수 있었다.Based on the above, it was confirmed that the fine powder as a high quality carbon source having a fine powder content of 71 to 76% by the complex purification process according to the present invention can be recovered as a secondary recovery.
계속해서, 상기에서 수득된 2차회수물로서의 미연분을 탄화시켜 수득된 탄화품의 물성을 분석하여 그 결과를 하기 표 3에 나타내었으며, 또한 이 탄화품을 수증기활성화시키는 활성화조건 및 활성화 실험결과를 하기 표 4 및 표 5에 나타내었다.Subsequently, the physical properties of the carbonized product obtained by carbonizing the fine powder as a secondary recovery product obtained above are shown in Table 3 below, and the activation conditions and the activation test results for steam activating this carbonized product are shown. Table 4 and Table 5 below.
상기한 실시예들을 종합한 결과, 본 발명에 따르면 고탄소 석탄회(플라이애쉬)로부터고품위의 탄소함량을 갖는 미연분을 분리, 정제하고, 그로부터 고품위의 활성탄을 제조할 수 있음을 확인할 수 있었다. 특히, 본 발명에 따르면 미연분 함량 71 내지 76%의 고품위의 탄소원으로서의 미연분을 2차회수물로 회수되며, 이는 종래와 같이 공기분급방법 단독에 의한 회수율이 50%인 것에 비하면 월등히 높은 회수가 가능하며, 습식회수방법 단독에 의한 회수율이 65 내지 66%인 것에 비해서도 더 높은 회수율을 나타내며, 이렇게 회수된 미연분을 원료로 하여 수득된 활성탄은 상용화된 숯(char ; 목재의 탄화에 의해 수득되는 것)과 흡착성능이 유사하며, 저농도 정수처리용, 저농도 폐수처리용, 농업비료용, 저급탈취용 등으로 사용될 수 있다.As a result of synthesizing the above-described embodiments, it was confirmed that according to the present invention, fine coal having a high carbon content can be separated and purified from high carbon coal ash (fly ash), and high quality activated carbon can be prepared therefrom. Particularly, according to the present invention, unburned ash as a high-quality carbon source having a fine ash content of 71 to 76% is recovered as a secondary recovery, which is much higher than the conventional recovery rate of 50% by the air classification method alone. It is possible to obtain a higher recovery rate compared with the recovery rate of 65 to 66% by the wet recovery method alone, and the activated carbon obtained from the recovered unburned dust as a raw material is obtained from carbonization of commercialized char (wood). ) And similar adsorption performance, can be used for low concentration water treatment, low concentration wastewater treatment, agricultural fertilizer, low deodorization.
따라서, 본 발명에 의하면 공기분급 후, 부유선광하는 복합정제공정에 의해 석탄회로부터 고품위의 미연분을 분리하고, 이를 활성화시키는 복합정제공정에 의한 고탄소 석탄회로부터의 활성탄의 제조방법을 제공하며, 그로부터 상용화된 숯(char ; 목재의 탄화에 의해 수득되는 것)과 흡착성능이 유사하며, 저농도 정수처리용, 저농도 폐수처리용, 농업비료용, 저급탈취용 등으로 사용될 수 있는 활성탄을 제공하는 효과가 있다.Therefore, according to the present invention, there is provided a method for producing activated carbon from high carbon coal ash by a complex refining process which separates high quality unburned powder from coal ash by a composite refining step of floating beneficiation after air classification, and thereby activates it. Its adsorption performance is similar to that of commercialized char (char obtained by carbonization of wood), and it has the effect of providing activated carbon that can be used for low concentration water treatment, low concentration wastewater treatment, agricultural fertilizer, and low deodorization. have.
또한 복합공정에 의한 고탄소석탄회에 야자각 Char 분말 각각 50% 혼합조립품은 요오드 흡착성능이 KS 2급 기준인 1,000㎎/g보다 20㎎/g이 높은 1,020㎎/g으로 나타나, 시중유통품인 석탄계 조립활성탄 요오드 흡착성능인 900∼1,000㎎/g과 유사하게 나타나므로 상품화가능성이 있는 것으로 판단된다.In addition, 50% mixed granules of Coconut Shell Char powder in high carbon coal by the composite process showed 1,020 mg / g, which is 20 mg / g higher than 1,000 mg / g of iodine adsorption. Since coal-based granular activated carbon iodine adsorption performance appears similar to 900 ~ 1,000mg / g, it is considered to be commercially available.
이상에서 본 발명은 기재된 구체예에 대해서만 상세히 설명되었지만 본 발명의 기술사상 범위 내에서 다양한 변형 및 수정이 가능함은 당업자에게 있어서 명백한 것이며, 이러한 변형 및 수정이 첨부된 특허청구범위에 속함은 당연한 것이다.Although the present invention has been described in detail only with respect to the described embodiments, it will be apparent to those skilled in the art that various modifications and variations are possible within the technical scope of the present invention, and such modifications and modifications are within the scope of the appended claims.
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| KR102241190B1 (en) * | 2020-09-09 | 2021-04-16 | 티에스에코텍 주식회사 | Deodorant including activated carbon manufactured by adsorbing microorganisms from coal ash |
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| US11369941B2 (en) | 2017-10-26 | 2022-06-28 | Posco Chemical Co., Ltd. | Method for preparing porous carbon material by using coal tar generated in COG process |
| KR102241190B1 (en) * | 2020-09-09 | 2021-04-16 | 티에스에코텍 주식회사 | Deodorant including activated carbon manufactured by adsorbing microorganisms from coal ash |
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