KR20020016256A - Preparation of dioxin removal adsorbent from coke breeze - Google Patents

Preparation of dioxin removal adsorbent from coke breeze Download PDF

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KR20020016256A
KR20020016256A KR1020000049479A KR20000049479A KR20020016256A KR 20020016256 A KR20020016256 A KR 20020016256A KR 1020000049479 A KR1020000049479 A KR 1020000049479A KR 20000049479 A KR20000049479 A KR 20000049479A KR 20020016256 A KR20020016256 A KR 20020016256A
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adsorbent
exhaust gas
powdered coke
coke
coke breeze
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KR100391561B1 (en
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김제영
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신현준
재단법인 포항산업과학연구원
홍상복
포스코신기술연구조합
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
    • B01D53/04—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography with stationary adsorbents
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/46—Removing components of defined structure
    • B01D53/68—Halogens or halogen compounds
    • B01D53/70—Organic halogen compounds
    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing

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  • Engineering & Computer Science (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Health & Medical Sciences (AREA)
  • Biomedical Technology (AREA)
  • Environmental & Geological Engineering (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Organic Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Treating Waste Gases (AREA)

Abstract

PURPOSE: A method of preparing an adsorbent for dioxin removal using coke breeze is provided to apply coke breeze that is generated as byproduct in steelmaking industries instead of costly activated carbon. CONSTITUTION: The preparation method of an adsorbent for dioxin removal using coke breeze includes the steps of: (i) blending coke breeze having a particle size distribution of less than 1μm with binders such as coal tar pitch and petroleum pitch at a weight ratio of 9 : 1; (ii) forming the blend into the shape of pellet; (iii) heat-treating the blend at 200deg.C for 30min for solidification and further heating at 250deg.C for 30min for surface oxidation.

Description

분코크스를 이용한 유해성 배기가스 처리제 제조방법{Preparation of dioxin removal adsorbent from coke breeze}Manufacturing method of hazardous exhaust gas treatment agent using powder coke {Preparation of dioxin removal adsorbent from coke breeze}

본 발명은 분 코크스를 이용한 유해성 배기가스 처리제 제조방법, 보다 상세하게는 제철소에서 발생되는 미세한 입자로 된 분 코크스를 원료로 하여 이에 친화적인 성질을 가진 바인더를 혼합하여 과립형태로 성형한 후 이를 이용하여 소각로 및 연소 배기가스의 출구에서 배출되는 대기오염물질 특히 무기질의 유해성 물질 및 유기염소화합물(다이옥신)을 흡착 제거하기 위한 분 코크스를 이용한 유해성 배기가스 처리제 제조방법에 관한 것이다.The present invention is a method for producing a harmful exhaust gas treatment agent using powdered coke, more specifically, powdered coke made of fine particles generated in steel mills as a raw material mixed with a binder having a friendly property to form a granule form and then used The present invention relates to a method for preparing a hazardous exhaust gas treatment agent using powdered coke for adsorption and removal of air pollutants, especially inorganic harmful substances and organic chlorine compounds (dioxin), discharged from an incinerator and an outlet of combustion exhaust gas.

일반적으로, 배기가스중에 포함된 유해 성분을 제거하는 방법은 제거하고자 하는 물질의 성분에 따라 여러 가지가 이용되고 있으며, 분진을 제거하는 경우에는 필터를 이용하거나 집진기를 이용하는 방법이 가장 보편적으로 실시되고 있으나, 그 배기가스중에 함유된 유해 성분을 제거하기 위해서는 대상이 되는 물질에 따라 다양한 방법을 선택하고 있다.In general, a variety of methods for removing harmful components contained in the exhaust gas are used according to the components of the material to be removed, and when removing dust, a filter or a dust collector is most commonly used. However, in order to remove harmful components contained in the exhaust gas, various methods are selected according to the target material.

예컨데, 배기가스중의 대표적인 유해 성분으로는 질소화합물과 유황화합물이 있으며, 이러한 물질을 제거하기 위해서는 촉매를 이용하거나 습식방법을 이용하는방법이 보편화 되었다.For example, the representative harmful components in the exhaust gas are nitrogen compounds and sulfur compounds, and in order to remove such substances, a method using a catalyst or a wet method has become common.

그러나 유해성이 강력한 것으로 알려진 수은이나 다이옥신과 같은 유기염소화합물을 제거하기 위해서는 상기의 어느 한 방법만으로는 어려웠다.However, in order to remove organochlorine compounds, such as mercury and dioxins, which are known to be highly harmful, it has been difficult by any of the above methods.

독일에서 제안된 방법중 가장 효율적으로 다이옥신과 수은 및 무기유해성분을 제거하게 된 기술로, 활성탄 및 활성코크스를 이용하여 흡착법으로 제거하는 방법이 제안되어 있으며 상업적으로도 널리 활용되고 있다(B,Neukirchen, VGB Kraftwerkstechnik, Vol.72, pp.572-575, H.Regler, VGB Kraftwerkstechnik, Vol.73, pp.709-714, W.Thielen et al. VGB Kraftwerkstechnik, Vol.73, pp.519-524).It is the technology that removes dioxin, mercury and inorganic harmful substances most efficiently among the proposed methods in Germany, and it is proposed to remove by activated adsorption using activated carbon and activated coke and is widely used commercially (B, Neukirchen) , VGB Kraftwerkstechnik, Vol. 72, pp. 572-575, H. Regler, VGB Kraftwerkstechnik, Vol. 73, pp. 709-714, W. Thielen et al. VGB Kraftwerkstechnik, Vol. 73, pp. 519-524) .

상기 독일에서 개발된 방법은 배기가스중 다이옥신과 염소화합물 및 수은 등과 같은 물질을 제거하기 위하여 갈탄 또는 역청탄을 이용하여 활성탄 또는 활성코크스를 제조한 후 흡착제로 사용하는 방법이며, 흡착제를 이동상에서 순환시키면서 재생 및 재활용하는 방법을 사용하고 있다.The method developed in Germany is a method of producing activated carbon or activated coke using lignite or bituminous coal to remove substances such as dioxins, chlorine compounds and mercury from the exhaust gas and then using them as adsorbents. Recycling and recycling are used.

그러나, 상기 방법은 이동상을 이용하므로 비표면적이 큰 활성탄을 제조하여 사용할 때 경도가 낮아서 분화현상이 일어나므로, 경도를 높이기 위해서 활성화를 초기단계로 하여 비표면적이 낮은 것을 제조하여 사용해야 되는 번거러움과 그리고 원료로서 역청탄 및 갈탄을 이용하므로 흡착제의 일정량을 계속적으로 회수 및 재충전해야 됨으로 인한 운전비용이 비싼 문제점이 있었다.However, since the method uses a mobile phase, differentiation occurs due to low hardness when the activated carbon having a large specific surface area is used. Therefore, the need for manufacturing a low specific surface area using activation as an initial step to increase hardness is high. Since bituminous coal and lignite are used as raw materials, there is a problem in that operating costs are high due to the continuous recovery and recharging of a predetermined amount of the adsorbent.

본 발명은 위와 같은 종래의 배기가스중 유해 성분의 제거에 따른 문제점을감안하여 안출한 것으로, 그 목적은 제철소에서 부산물로 생산되는 분 코크스를 원료로 하여 제조된 흡착제를 이용하여 유해성 배기가스를 제거할 수 있는 분 코크스를 이용한 유해성 배기가스 처리제 제조방법을 제공하는 것이다.The present invention has been made in view of the problems caused by the removal of harmful components in the conventional exhaust gas as described above, the object is to remove the harmful exhaust gas using an adsorbent prepared from the powdered coke produced as by-products in steel mills as raw materials It is to provide a method for producing a harmful exhaust gas treatment agent using minute coke.

이러한 목적을 달성하기 위한 본 발명은, 제철소에서 발생하는 분코크스를 필러로 이용하고 바인더로서는 석탄타르 핏치,석유 핏치 및 유기성 계통의 바인더를 사용하여 과립상 및 구형상으로 성형한 후 이를 약 200℃에서 30분간 열처리 및 고형화 하여 흡착제를 제조하며, 제조된 흡착제는 공기중에서 약 250℃에서 약 30분간 열처리 하여 표면을 산화시키며, 이를 반응기에 장입한 후 배기가스를 통과시킴으로써, 배기가스중에 함유된 다이옥신과 수은 및 무기염화물 등의 유해 물질을 제거함을 특징으로 한다.In order to achieve the above object, the present invention uses a powdered coke generated in a steel mill as a filler, and a coal tar pitch, a petroleum pitch, and an organic binder, which are formed into granular and spherical shapes, and then about 200 ° C. The adsorbent is prepared by heat treatment and solidification for 30 minutes at, and the prepared adsorbent is heat treated at about 250 ° C. for about 30 minutes in order to oxidize the surface. And to remove harmful substances such as mercury and inorganic chlorides.

이하, 본 발명의 분 코크스를 이용한 유해성 배기가스 처리제 제조방법을 상세히 설명한다.Hereinafter, the manufacturing method of the hazardous waste gas processing agent using the powdered coke of this invention is demonstrated in detail.

제철소에서 부산물로 얻어지는 분코크스를 필러로 이용하고 이에 첨가되는 바인더로서는 석탄타르 핏치,석유 핏치 등의 유기성 계통의 물질을 사용하여 과립상 및 구형상으로 성형한 후 이를 약 200℃에서 30분간 열처리 및 고형화 하여 흡착제를 제조하며, 제조된 흡착제는 공기중에서 약 250℃에서 약 30분간 열처리 하여 표면을 산화시키며, 상기 방법에 의해 만들어진 흡착제는 고정상 반응기에 장입한 후 배기가스를 통과시킴으로써, 배기가스중에 함유된 유해 물질을 제거하게 된다.The powdered coke obtained as a by-product from the steel mill is used as a filler, and as a binder added thereto, organic granules such as coal tar pitch and petroleum pitch are formed into granular and spherical shapes, followed by heat treatment at about 200 ° C. for 30 minutes and The adsorbent prepared is solidified to prepare an adsorbent, and the prepared adsorbent is heat treated at about 250 ° C. for about 30 minutes to oxidize the surface. The adsorbent produced by the above method is charged into a fixed bed reactor and then passed through the exhaust gas to be contained in the exhaust gas. This will remove harmful substances.

상기 흡착제로 사용하기 위한 분 코크스는 세공이 거의 없은 것이 바람직하나, 이 자체만으로는 흡착제의 역할을 제대로 하지 못하므로 분 코크스를 바인더로 성형한 후 열처리 하여 바인더와 분 코크스의 입자사이에 비표면적이 낮은 상태에서 일부에 세공이 형성되도록 한다.It is preferable that the powdered coke for use as the adsorbent has almost no pores, but by itself, the powdered coke does not function properly as the adsorbent. The pores are formed in a part in the state.

다이옥신과 같은 물질은 일반적으로 350℃이하의 온도에서는 기상으로 존재하지 않고 결정상으로 존재하기 때문에 흡착제의 세공에 의해서 흡착되는 것은 아니며, 흡착제의 표면에 부착되는 형태로 제거되므로, 다른 발명에서 사용한 활성탄과 활성코크스를 사용하지 않고 세공도 많지 않으며 비표면적이 낮은 본 발명에서 제조되는 형태의 흡착제에 의해 충분히 제거된다.Since materials such as dioxins generally do not exist in the gas phase but in the crystalline phase at temperatures below 350 ° C., they are not adsorbed by the pores of the adsorbent and are removed in the form of adhering to the surface of the adsorbent. It is sufficiently removed by the adsorbent of the type produced in the present invention without using activated coke, having few pores and having a low specific surface area.

상기 흡착제를 산화시키는 것은 표면에 산소관능기를 부여하여 배기가스중에 포함된 수분과의 친화성을 향상시킴으로서, 일부 수분중에 함유된 유해성분과 흡착제의 접촉성을 향상시켜 제거효율을 향상시키기 위한 방법을 제공하기 위한 것이다.Oxidizing the adsorbent provides an oxygen functional group to the surface to improve affinity with moisture contained in the exhaust gas, thereby providing a method for improving the removal efficiency by improving the contact between the adsorbent and the harmful components contained in some moisture. It is to.

본 발명에서의 흡착제는 다른 발명에서 시행한 방법인 이동상의 방법을 사용하지 않으면서 고정상 반응기를 이용하여 일정기간 사용한 후 이를 완전히 폐기시키게 되어 원료가격도 저렴하며, 배기가스중 유해 성분의 농도가 완전히 파괴될 때까지 사용할 수 있는 방법이다.The adsorbent in the present invention is completely discarded after using the fixed bed reactor for a certain period of time without using the mobile phase method, which is a method implemented in another invention, and the raw material price is low, and the concentration of harmful components in the exhaust gas is completely It can be used until destroyed.

이하 실시예를 통하여 본 발명을 상세히 설명한다.Hereinafter, the present invention will be described in detail through examples.

실시예 1:Example 1:

1mm 이하의 입도를 가진 미분 코크스와 석탄타르 핏치를 중량비로 90:10으로혼합한 후 펠렛 형태로 성형한 다음 이를 약 200℃에서 열처리한 후 다시 공기분위기에서 250℃로 30분간 열처리하여 흡착제를 제조하였다.After mixing the fine powder coke and coal tar pitch with a particle size of less than 1mm in a weight ratio of 90:10, and forming a pellet, heat-treated at about 200 ℃ and then heat treated at 250 ℃ in an air atmosphere for 30 minutes to prepare an adsorbent It was.

제조된 흡착제는 소정의 형상이 유지되었으며, 이 제조된 흡착제를 고정상 반응기에 장입한 후 소각로 배기가스의 출구에 설치하여 배기가스중 다이옥신 제거율을 조사한 결과, 반응기 입구에서 다이옥신의 농도가 0.775ngTEQ/Nm3 이었으나 반응기를 거친 후 출구에서의 다이옥신의 농도는 0.027ngTEQ/Nm3 으로 나타났다.The prepared adsorbent was maintained in a predetermined shape, and charged into the fixed bed reactor and installed at the outlet of the incinerator exhaust gas. However, after passing through the reactor, the concentration of dioxins at the outlet was found to be 0.027ngTEQ / Nm3.

실시예 2:Example 2:

1mm 이하의 입도를 가진 미분 코크스와 석유 핏치를 중량비로 90:10으로 혼합한 후 구형으로 성형하고, 이를 제 1실시예와 동일 조건으로 열처리 및 산화처리한 후 고정상 반응기에 충진하여 소각로의 배기가스 출구에서 다이옥신 제거실험을 한 결과, 입구농도가 0.65ngTEQ/Nm3 이었으나 반응기를 거친 후 출구에서 측정된 농도는 0.032ngTEQ/Nm3 이었다.The fine powder coke and petroleum pitch having a particle size of 1mm or less are mixed at a weight ratio of 90:10, and then formed into a spherical shape.Then, after heat treatment and oxidation treatment under the same conditions as in the first embodiment, the gas is filled in a fixed-bed reactor and the exhaust gas of the incinerator is incinerated. As a result of dioxin removal experiment at the outlet, the inlet concentration was 0.65ngTEQ / Nm3, but the concentration measured at the outlet after passing through the reactor was 0.032ngTEQ / Nm3.

실시예 3:Example 3:

상기 제 1실시예와 동일한 원료를 이용하되 바인더로 페놀수지를 사용하고 중량비로 95:5로 혼합한 후 펠렛형태로 성형하고, 이를 200℃에서 약 4시간 열처리한 후 산화반응 없이 고정상 반응기에 충진한 다음 제 1실시예의 조건과 같이 배기가스처리 실험을 한 결과, 입구에서의 다이옥신 농도는 0.78ngTEQ/Nm3 이었으나 출구에서는 0.11ngTEQ/Nm3 이었다.Using the same raw material as the first embodiment, but using a phenolic resin as a binder and mixed in a weight ratio of 95: 5, and then molded into a pellet form, and then heat-treated at 200 ℃ for about 4 hours and filled in a fixed bed reactor without oxidation reaction Then, as a result of the exhaust gas treatment experiment as in the conditions of the first embodiment, the dioxin concentration at the inlet was 0.78ngTEQ / Nm3, but it was 0.11ngTEQ / Nm3 at the outlet.

이와 같은 본 발명의 분 코크스를 이용한 유해성 배기가스 처리제 제조방법은 미세한 분 코크스를 필러로 하되 이에 유기물을 바인더로 사용하여 성형체를 제조한 후 열처리를 거쳐 흡착제를 제조한 다음 고정상 반응기에 장착하여 배기가스를 통과시킴으로써, 다이옥신제거 등의 유해 성분을 약 90% 이상 제거할 수 있는 효과가 있다.Such a method for preparing a hazardous exhaust gas treatment agent using powdered coke according to the present invention uses a fine powdered coke as a filler, prepares a molded body using organic matter as a binder, prepares an adsorbent through heat treatment, and mounts it in a fixed bed reactor to exhaust gas. By passing through, there is an effect that can remove about 90% or more of harmful components such as dioxin removal.

또한 기존의 활성탄과 같은 고가의 흡착제를 사용하지 않고도 제철소의 부산물을 이용하여 다이옥신을 제거함으로써 자원을 재활용할 수 있는 경제적인 효과와 더불어 유해 성분의 제거효율을 향상시킬 수 있는 장점이 있다.In addition, by removing dioxins using by-products of steel mills without the use of expensive adsorbents such as activated carbon, there is an economical effect to recycle resources as well as the removal efficiency of harmful components.

Claims (3)

제철소에서 부산물로 얻어지는 분코크스를 필러로 이용하고 이에 첨가되는 바인더로 유기성 계통의 물질을 사용하여 과립상 및 구형상으로 성형하며, 이 성형체를 약 200℃에서 30분간 열처리 및 고형화 한 후 다시 공기중에서 약 250℃에서 약 30분간 열처리 하여 표면을 산화시켜 흡착제를 제조하고, 상기 공정에 의해 만들어진 흡착제는 고정상 반응기에 장입하여 배기가스중에 포함된 유해 물질을 제거하게 됨을 특징으로 하는 분 코크스를 이용한 유해성 배기가스 처리제 제조방법.In the steel mill, the powdered coke obtained as a by-product is used as a filler, and the binder is added into the granular and spherical shapes by using an organic material. The molded body is heat treated and solidified at about 200 ° C. for 30 minutes, and then again in the air. Heat treatment at about 250 ℃ for about 30 minutes to oxidize the surface to prepare an adsorbent, and the adsorbent produced by the above process is charged into a fixed-bed reactor to remove the harmful substances contained in the exhaust gas harmful exhaust gas using the powdered coke, characterized in that Method for producing gas treating agent. 제 1항에 있어서, 상기 분 코크스의 입도가 1mm 이하이며, 상기 바인더를 석탄타르 핏치 또는 석유 핏치중 어느 하나를 사용하여 분 코크스와 석탄타르 핏치 또는 석유 핏치를 중량비로 90:10으로 혼합한 후 펠렛 형태로 성형한 것을 특징으로 하는 분 코크스를 이용한 유해성 배기가스 처리제 제조방법.The particle size of the powdered coke is 1 mm or less, and the binder is mixed with the powdered coke and the coal tar pitch or the oil pitch in a weight ratio of 90:10 using either coal tar pitch or petroleum pitch. A process for producing a noxious exhaust gas treatment agent using powdered coke, which is molded into pellets. 제 1항에 있어서, 상기 바인더가 페놀수지이며, 분 코크스와 페놀수지를 중량비로 95:5로 혼합한 후 펠렛형태로 성형하고, 이를 200℃에서 약 4시간 열처리한 후 산화반응 없이 흡착제를 제조함을 특징으로 하는 분 코크스를 이용한 유해성 배기가스 처리제 제조방법.The method of claim 1, wherein the binder is a phenolic resin, powdered coke and phenolic resin is mixed in a weight ratio of 95: 5, and then formed into a pellet, heat-treated at 200 ℃ for about 4 hours to prepare an adsorbent without oxidation reaction. A method for producing a harmful exhaust gas treatment agent using powdered coke, characterized in that.
KR10-2000-0049479A 2000-08-25 2000-08-25 Preparation of dioxin removal adsorbent from coke breeze KR100391561B1 (en)

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Publication number Priority date Publication date Assignee Title
KR100613255B1 (en) * 2001-12-22 2006-08-18 주식회사 포스코 Adsorbent for removal of dioxins
KR100622797B1 (en) * 2004-05-06 2006-09-14 한국전력공사 Adsorbent utilizing activated heavy-oil fly ashes for the removal of hazardous air pollutants from combustion flue gases and processing method thereof

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KR100644518B1 (en) 2005-11-01 2006-11-10 재단법인 포항산업과학연구원 The extraction method for halogenated organic compounds in waste water

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JPS6168312A (en) * 1984-09-11 1986-04-08 Mitsui Mining Co Ltd Production of molecular sieve comprising coal base carbonaceous material
JPH01270576A (en) * 1988-04-21 1989-10-27 Nippon Steel Corp Production of porous carbon material
US5968471A (en) * 1995-07-20 1999-10-19 Nippon Sanso Corporation Process for producing molecular sieve carbon
KR100226919B1 (en) * 1995-12-05 1999-10-15 이구택 Preparation of coke for metallurgy using powder coke
KR100228221B1 (en) * 1995-12-28 1999-11-01 이구택 Preparation of formed coke
KR100299446B1 (en) * 1996-12-20 2001-11-22 이구택 Manufacturing method of raw coke material using fine coke dust

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
KR100613255B1 (en) * 2001-12-22 2006-08-18 주식회사 포스코 Adsorbent for removal of dioxins
KR100622797B1 (en) * 2004-05-06 2006-09-14 한국전력공사 Adsorbent utilizing activated heavy-oil fly ashes for the removal of hazardous air pollutants from combustion flue gases and processing method thereof

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