KR100635719B1 - A method for oxidizing mercury in exhaust gas - Google Patents

A method for oxidizing mercury in exhaust gas Download PDF

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KR100635719B1
KR100635719B1 KR1020050039331A KR20050039331A KR100635719B1 KR 100635719 B1 KR100635719 B1 KR 100635719B1 KR 1020050039331 A KR1020050039331 A KR 1020050039331A KR 20050039331 A KR20050039331 A KR 20050039331A KR 100635719 B1 KR100635719 B1 KR 100635719B1
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mercury
oxide
exhaust gas
chromium
combustion exhaust
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Korean (ko)
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박경일
백점인
송광철
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한국전력공사
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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
    • B01D53/34—Chemical or biological purification of waste gases
    • B01D53/74—General processes for purification of waste gases; Apparatus or devices specially adapted therefor
    • B01D53/86—Catalytic processes
    • B01D53/8665—Removing heavy metals or compounds thereof, e.g. mercury
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2255/00—Catalysts
    • B01D2255/20—Metals or compounds thereof
    • B01D2255/207—Transition metals
    • B01D2255/20784—Chromium
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/60—Heavy metals or heavy metal compounds
    • B01D2257/602—Mercury or mercury compounds

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Abstract

A method for oxidizing mercury in combustion exhaust gas, which is excellent in oxidation activity and economic efficiency when changing metal mercury contained in combustion exhaust gas exhausted from a large boiler into mercury chloride, is provided. A method for oxidizing mercury in combustion exhaust gas comprises mercury in the combustion exhaust gas into mercury chloride in the presence of a chromium oxide catalyst supported with a magnesium oxide-aluminum oxide prepared by coprecipitating a magnesium salt, an aluminum salt and a chromium salt at a ratio of 1:1:1 and drying the coprecipitated material at 110 deg.C. The chromium oxide supported with the magnesium oxide-aluminum oxide is prepared by adding a magnesium salt, an aluminum salt, a chromium salt and a precipitant into water to form a precipitate and calcining the precipitate to a temperature from 300 to 700 deg.C under an air atmosphere.

Description

연소 배기가스 중의 수은의 산화방법{A method for oxidizing mercury in exhaust gas}A method for oxidizing mercury in exhaust gas

도 1은 수은 산화 촉매의 성능을 시험하는 장치의 구성을 개략적으로 나타낸 도면.BRIEF DESCRIPTION OF THE DRAWINGS The figure which shows schematically the structure of the apparatus which tests the performance of a mercury oxidation catalyst.

<도면의 주요 부분에 대한 부호의 설명><Explanation of symbols for the main parts of the drawings>

11: 금속 수은 발생장치 12: 운반가스 공급장치11: metal mercury generator 12: carrier gas supply

13: 공기항온조 14: 수은농도분석기13: air thermostat 14: mercury concentration analyzer

15: 활성탄 16: 3-웨이-밸브15: activated carbon 16: 3-way valve

17: 고정층 반응기 18: 냉각기17: fixed bed reactor 18: cooler

본 발명은 연소 배기가스 중의 수은의 산화방법에 관한 것으로서, 더욱 상세하게는 크롬 산화물을 촉매로 이용하여 연소 배기가스 중에 포함된 수은을 산화시키는 방법에 관한 것이다.The present invention relates to a method of oxidizing mercury in combustion exhaust gas, and more particularly, to a method of oxidizing mercury contained in combustion exhaust gas using chromium oxide as a catalyst.

석탄과 같은 화석연료에는 연료 자체에 수은이나 비소와 같은 인체에 유해한 미량의 유해 대기 오염물질이 포함되어 있다. 화석연료를 고온의 보일러에서 연소 시키면 원료 중의 중금속 중 수은과 같이 휘발성이 큰 물질은 증기상의 형태로 일부가 대기로 배출된다. 대기로 배출된 미량의 유해 대기 오염물질은 자연계의 순환과정이나 먹이사슬을 거쳐 인체에 축적되고 각종 질병을 유발하게 된다. 수은의 경우 대기로 배출된 후 자연계의 순환과정에서 메틸수은의 형태로 먹이사슬 피라미드의 최상층에 있는 인체에 축적되면 신경계통과 뇌에 손상을 주며, 특히 태아나 유아에게는 심각한 장애를 유발하는 원인이 된다고 알려져 있다. 따라서, 세계 각국은 수은의 배출원인 쓰레기나 폐기물 소각장에 대해 규제치를 마련하고 이를 준수하도록 하고 있다. 최근 들어 인간 활동으로 인해 대기 중으로 유출되는 수은의 가장 큰 배출원이 전기 에너지를 얻기 위하여 대량의 석탄을 연소하고 있는 화력발전소임을 인지하게 되었다. 따라서, 지금까지는 화력발전소에서 배출되는 수은을 비롯한 미량의 유해 대기 오염물질에 대해 배출 농도가 낮아 규제대상에서 제외하여 왔지만 절대량으로 보았을 때 이를 무시할 수가 없어 대책마련이 필요하게 되었다.Fossil fuels such as coal contain traces of harmful air pollutants, such as mercury and arsenic, in the fuel itself. When fossil fuels are burned in a high temperature boiler, some of the heavy metals in the raw materials, such as mercury, are released to the atmosphere in the form of steam. Trace amounts of harmful air pollutants released into the atmosphere accumulate in the human body through natural circulation and food chains and cause various diseases. When mercury is released into the atmosphere and accumulates in the human body on the top layer of the food chain pyramid in the form of methylmercury in the natural circulation, it damages the nervous system and the brain. Known. As a result, countries around the world have established and are required to comply with regulations on waste and waste incinerators, which are sources of mercury. Recently, the largest source of mercury released into the atmosphere due to human activity has been recognized as a thermal power plant that burns large amounts of coal to obtain electrical energy. Therefore, until now, trace amounts of harmful air pollutants, including mercury emitted from thermal power plants, have been excluded from the regulation because of low concentrations.

발전소나 제철소 등에서 운영 중인 대형 보일러의 연소 배기가스 중에는 석탄 연소 시 수은을 비롯한 미량의 유해 대기 오염물질이 포함되어 있다. 이 중 수은은 형태에 따라 크게 금속 수은(Hg)과 염화 수은(Hg2Cl2 또는 HgCl2) 두 가지 형태로 존재한다. 석탄 연소과정 중 발생하는 수은의 대부분은 금속 수은의 형태로 존재하는데, 이것은 물에 불용성이어서 제거하기가 쉽지 않다. 현재 활성탄 흡착제와 같은 물질을 사용하여 제거하는 노력이 진행되고 있지만, 비용이 많이 들어 경제적인 측면에서 문제점이 드러나고 있다. 이와 반대로 염화 수은은 수용성이어서 후단의 습식 공정을 통해 쉽게 제거될 수 있다.The combustion flue of large boilers operating in power plants and steel mills contains trace amounts of harmful air pollutants, including mercury, when burning coal. Among these, mercury is present in two types, mercury metal (Hg) and mercuric chloride (Hg 2 Cl 2 or HgCl 2 ). Most of the mercury generated during the combustion of coal is in the form of metallic mercury, which is insoluble in water and difficult to remove. At present, efforts have been made to remove materials using activated carbon adsorbents, but problems are found in economic terms due to the high cost. Mercury chloride, on the other hand, is water soluble and can be easily removed through the subsequent wet process.

최근 미국의 URS사가 개발한 Pd 계열의 촉매는 수은 산화 활성이 90% 이상이지만, 귀금속을 사용하기 때문에 비용이 많이 소요되는 단점이 있다.Recently, the Pd-based catalyst developed by URS in the United States has a mercury oxidation activity of more than 90%, but has a disadvantage of being expensive due to the use of precious metals.

본 발명은 상기와 같은 문제점을 해결하기 위한 것으로서, 본 발명의 목적은 대형 보일러에서 배출되는 연소 배기가스 중에 포함된 금속 수은을 염화수은으로 바꾸는데 있어서 산화 활성이 우수하고, 경제성이 뛰어난 연소 배기가스 중의 수은의 산화방법을 제공함에 있다.The present invention has been made to solve the above problems, and an object of the present invention is to convert metallic mercury contained in combustion exhaust gas discharged from a large boiler into mercuric chloride, which has excellent oxidation activity and economical efficiency. To provide a method of oxidation of mercury.

상기 목적을 달성하기 위하여, 본 발명은 크롬 산화물 촉매의 존재 하에 연소 배기가스 중의 수은을 염화 수은으로 산화시키는 연소 배기가스 중의 수은의 산화방법을 제공한다.In order to achieve the above object, the present invention provides a method of oxidizing mercury in combustion exhaust gas in which mercury in combustion exhaust gas is oxidized to mercuric chloride in the presence of a chromium oxide catalyst.

본 발명에 따른 크롬 산화물(Cr2O3)은 저가의 전이금속 산화물이기 때문에 경제적으로 활용가치가 높으며, 다른 전이금속 산화물과는 달리 귀금속과 대등한 수은 산화 활성을 나타낸다.Since chromium oxide (Cr 2 O 3 ) according to the present invention is a low-cost transition metal oxide, its economic value is high, and unlike other transition metal oxides, chromium oxide (Cr 2 O 3 ) exhibits mercury oxidation activity equivalent to that of noble metals.

하기 식 1과 같이 상기 크롬 산화물 촉매의 존재 하에 수은을 함유한 연소 배기 가스에 수은 염소화제를 첨가하면 금속 수은이 염화 수은으로 산화된다. 수은 염소화제로는 HCl 등을 이용할 수 있다. 본 발명의 크롬 산화물 촉매는 수은 산화 반응을 활성화시켜 고효율로 금속 수은을 염화 수은으로 전환시킨다.When mercury chlorination agent is added to the combustion exhaust gas containing mercury in the presence of the chromium oxide catalyst as shown in Equation 1, metallic mercury is oxidized to mercury chloride. As a mercury chlorinating agent, HCl etc. can be used. The chromium oxide catalyst of the present invention activates the mercury oxidation reaction to convert metallic mercury to mercuric chloride with high efficiency.

Figure 112006064180212-pat00003
(1)
Figure 112006064180212-pat00003
(One)

상기 크롬 산화물은, 마그네슘 산화물, 알루미늄 산화물 중에서 선택된 적어도 하나를 담체로 이용하여, 상기 담체 상에 담지될 수 있다. 상기 담체에 대해 크롬 산화물이 15∼60중량% 담지될 수 있다. 담체를 사용할 경우 활성 물질을 보다 작은 크기로 분산시킬 수 있어서 산화 속도의 증가 효과가 나타난다.The chromium oxide may be supported on the carrier using at least one selected from magnesium oxide and aluminum oxide as a carrier. 15 to 60% by weight of chromium oxide may be supported in the carrier. The use of a carrier can disperse the active material into smaller sizes, resulting in an increase in the rate of oxidation.

본 발명의 산화 촉매인 크롬 산화물은 크롬염과 침전제를 물에 첨가하여 침전물을 형성하고, 상기 침전물을 공기 분위기 하에서 300∼700℃의 온도로 소성하여 제조될 수 있다. 먼저, 크롬의 질산염, 황산염, 초산염, 염화물 중에서 선택된 크롬염과 침전제를 동시에 물에 넣으면서 침전시킨다. 상기 침전제로는 NaOH, NH4OH 등을 사용할 수 있다. 얻어진 침전물 용액을 추가로 에이징(aging) 처리한 후 여과시킨다. 여과 후 공기 분위기에서 300∼700℃로 소성 처리하면 크롬 산화물이 얻어진다. 크롬 산화물의 분산도를 높이기 위해 담체로 마그네슘 산화물과 알루미늄 산화물을 사용할 수 있으며, 이를 위해 상기 크롬염에 마그네슘염과 알루미늄염을 첨가하여 소성 처리하면 마그네슘 산화물-알루미늄 산화물에 담지된 크롬 산화물을 얻을 수 있다.Chromium oxide, which is an oxidation catalyst of the present invention, may be prepared by adding a chromium salt and a precipitant to water to form a precipitate, and firing the precipitate at a temperature of 300 to 700 ° C. in an air atmosphere. First, the chromium salt and the precipitant selected from nitrates, sulfates, acetates and chlorides of chromium are simultaneously precipitated while being put into water. As the precipitant, NaOH, NH 4 OH, or the like may be used. The precipitate solution obtained is further aged after aging and filtered. After filtration, calcination at 300 to 700 占 폚 in an air atmosphere yields chromium oxide. Magnesium oxide and aluminum oxide can be used as a carrier to increase the dispersibility of chromium oxide. For this purpose, when magnesium and aluminum salts are added to the chromium salt and calcined, chromium oxide supported on magnesium oxide-aluminum oxide can be obtained. have.

도 1은 수은 산화 촉매의 성능을 시험하는 장치의 구성을 개략적으로 나타낸 도면이다.1 is a view schematically showing the configuration of an apparatus for testing the performance of a mercury oxidation catalyst.

수은 산화 촉매를 도 1에 도시한 고정층 반응기(17)에 넣고 공기항온조(13) 를 150℃로 일정하게 유지시킨다. 금속 수은 발생장치(11)에서 일정 농도로 발생한 수은을 운반가스 공급장치(12)에서 공급되는 10ppm HCl이 함유된 질소로 희석하여 고정층 반응기(17)로 주입시키고 수은을 산화시킨 후, 반응기를 빠져나온 가스를 냉각기(18)를 이용하여 온도를 낮추고, 가스의 일부를 수은농도분석기(14)에서 샘플링하여 수은의 농도를 분석한다. 100mg의 산화 촉매가 충진된 고정층 반응기(17)를 통과하기 전의 가스 중의 수은 농도는 3-웨이-밸브(3-way-valve)(16)를 이용하여 수은농도분석기(14)로 공급하여 측정하였으며, 반응기 통과 전 후의 수은 농도의 차를 계산함으로써 반응기에 충진된 산화촉매의 수은 산화 성능을 얻을 수 있다.The mercury oxidation catalyst was placed in the fixed bed reactor 17 shown in FIG. 1 and the air thermostat 13 was kept at 150 deg. The mercury generated at a constant concentration in the metallic mercury generator 11 is diluted with nitrogen containing 10 ppm HCl supplied from the carrier gas supply device 12, injected into the fixed bed reactor 17, and the mercury is oxidized. The temperature of the released gas is lowered by using the cooler 18, and a part of the gas is sampled by the mercury concentration analyzer 14 to analyze the concentration of mercury. The mercury concentration in the gas before passing through the fixed bed reactor (17) filled with 100 mg of oxidation catalyst was measured by supplying it to the mercury concentration analyzer (14) using a 3-way-valve (16). By calculating the difference in the mercury concentration before and after the passage of the reactor, the mercury oxidation performance of the oxidation catalyst filled in the reactor can be obtained.

이하, 실시예 및 비교예를 통하여 본 발명을 상세히 설명한다. 그러나 하기 실시예는 본 발명의 일 실시예일 뿐 본 발명이 하기 실시예에 한정되는 것은 아니다.Hereinafter, the present invention will be described in detail through Examples and Comparative Examples. However, the following examples are only examples of the present invention and the present invention is not limited to the following examples.

<실시예 1><Example 1>

200㎖의 물에 질산크롬: 질산마그네슘: 질산알루미늄을 1:1:1 몰비로 첨가한 후 침전제로 NaOH를 전체 금속 산화물 농도의 1.9배 넣어 침전물을 형성하였다. 얻어진 침전물을 80℃에서 6시간 동안 에이징시킨 후 여과하고 세척하여 110℃에서 밤새 건조시켰다. 그런 다음 공기 분위기 하에서 450℃에서 밤새 소성시켜 마그네슘 산화물-알루미늄 산화물에 담지된 크롬 산화물을 얻었다. 45∼250㎛ 크기의 크롬 산화물 촉매 100mg을 도 1에 도시된 고정층 반응기에 충진시키고 반응기의 온도를 150℃로 유지한 상태에서 금속 수은 발생장치에서 일정한 농도로 발생하는 수은 을 운반가스 공급장치에서 공급되는 10ppm HCl이 함유된 질소로 희석시켜 공급하였다. 고정층 반응기 통과 전후의 수은 농도를 측정하여 얻은 수은 산화 효율을 표 1에 나타내었다.Chromium nitrate: magnesium nitrate: aluminum nitrate was added to 200 ml of water in a 1: 1: 1 molar ratio, and NaOH was added 1.9 times the total metal oxide concentration as a precipitant to form a precipitate. The precipitate obtained was aged at 80 ° C. for 6 hours, then filtered and washed to dry overnight at 110 ° C. It was then calcined overnight at 450 ° C. under an air atmosphere to obtain chromium oxide supported on magnesium oxide-aluminum oxide. 100 mg of a chromium oxide catalyst having a size of 45 to 250 μm was charged to the fixed bed reactor shown in FIG. 1, and the mercury generated at a constant concentration in the metallic mercury generator was supplied from the carrier gas supply device while maintaining the reactor temperature at 150 ° C. It was supplied diluted with nitrogen containing 10 ppm HCl. The mercury oxidation efficiency obtained by measuring the mercury concentration before and after passing through the fixed bed reactor is shown in Table 1.

수은 산화 효율(%) = (고정층 반응기 통과전 금속수은농도-고정층 반응기 통과후 금속수은농도)/(고정층 반응기 통과전 금속수은농도)*100Mercury oxidation efficiency (%) = (Metal mercury concentration before passing through the fixed bed reactor-Metal mercury concentration after passing through the fixed bed reactor) / (Metal mercury concentration before passing through the fixed bed reactor) * 100

<비교예 1>Comparative Example 1

질산크롬을 첨가하지 않고 질산마그네슘과 질산알루미늄을 2:1의 몰비로 사용하는 것을 제외하고는 실시예 1과 동일하게 실시하였다.The same procedure as in Example 1 was carried out except that magnesium nitrate and aluminum nitrate were used in a molar ratio of 2: 1 without adding chromium nitrate.

<비교예 2>Comparative Example 2

질산크롬 대신에 질산아연을 사용하여 실시예 1과 동일하게 실시하였다.Zinc nitrate was used instead of chromium nitrate to carry out the same procedure as in Example 1.

<비교예 3>Comparative Example 3

질산크롬 대신에 질산니켈을 사용하여 실시예 1과 동일하게 실시하였다.Nickel nitrate was used instead of chromium nitrate in the same manner as in Example 1.

<비교예 4><Comparative Example 4>

질산크롬 대신에 질산철을 사용하여 실시예 1과 동일하게 실시하였다.In the same manner as in Example 1 using iron nitrate instead of chromium nitrate.

<비교예 5>Comparative Example 5

질산크롬 대신에 질산구리를 사용하여 실시예 1과 동일하게 실시하였다.Copper nitrate was used instead of chromium nitrate in the same manner as in Example 1.

산화 촉매Oxidation catalyst 수은 산화 효율(%)Mercury Oxidation Efficiency (%) 실시예 1Example 1 Cr2O3/MgO-Al2O3 Cr 2 O 3 / MgO-Al 2 O 3 100100 비교예 1Comparative Example 1 MgO-Al2O3 MgO-Al 2 O 3 55 비교예 2Comparative Example 2 ZnO/MgO-Al2O3 ZnO / MgO-Al 2 O 3 1313 비교예 3Comparative Example 3 NiO/MgO-Al2O3 NiO / MgO-Al 2 O 3 2525 비교예 4Comparative Example 4 Fe2O3/MgO-Al2O3 Fe 2 O 3 / MgO-Al 2 O 3 4545 비교예 5Comparative Example 5 CuO/MgO-Al2O3 CuO / MgO-Al 2 O 3 8080

비교예 1은 담체로 사용된 마그네슘 산화물-알루미늄 산화물로 이루어진 금속 산화물을 실험한 결과이며, 비교예 2 내지 5는 담체에 여러 종류의 전이금속 산화물을 담지하여 실험한 결과이다. 철 산화물을 담지한 비교예 4는 45%의 산화 효율을 나타내었으며, 구리 산화물을 담지한 비교예 5는 80%의 산화 효율 나타내었다. 본원 발명에 따른 크롬 산화물을 담지한 실시예 1은 100%의 산화 효율을 나타내어 뛰어난 수은 산화활성을 보였다.Comparative Example 1 is a result of experimenting with a metal oxide consisting of magnesium oxide-aluminum oxide used as a support, Comparative Examples 2 to 5 are the results of experiments by supporting a variety of transition metal oxide on the support. Comparative Example 4 carrying the iron oxide showed an oxidation efficiency of 45%, Comparative Example 5 carrying the iron oxide showed an oxidation efficiency of 80%. Example 1 carrying chromium oxide according to the present invention showed an oxidation efficiency of 100%, showing excellent mercury oxidation activity.

대량으로 배출되는 연소 배기가스 중에 미량으로 함유된 금속 수은을 제거가 용이한 염화 수은으로 바꾸기 위하여 산화 촉매를 사용하였다. 현재까지의 기술은 Pd 계열의 귀금속을 사용하기 때문에 고비용의 문제점이 발생하는데, 본 발명에서는 크롬 산화물을 금속 수은 산화 촉매로 사용하였다. 본 발명은 저가의 크롬 산화물을 사용하므로 경제적으로 제조할 수 있고, 화학 처리가 필요하지 않으므로 환경 친화적이다.An oxidation catalyst was used to convert metallic mercury contained in trace amounts in the large amount of combustion exhaust gas into mercuric chloride, which is easy to remove. The technology up to now uses a Pd-based noble metal, causing a problem of high cost. In the present invention, chromium oxide is used as a metal mercury oxidation catalyst. The present invention uses an inexpensive chromium oxide so that it can be manufactured economically and is environmentally friendly since no chemical treatment is required.

Claims (7)

삭제delete 삭제delete 삭제delete 마그네슘염, 알루미늄염 및 크롬염을 1:1:1로 공침하여 110℃에서 건조하여 제조된 마그네슘 산화물-알루미늄 산화물에 담지된 크롬 산화물 촉매의 존재하에 연소 배기가스 중의 수은을 염화 수은으로 산화시키는 것을 특징으로 하는 연소 배기가스 중의 수은의 산화방법.Oxidizing mercury in the combustion exhaust gas with mercuric chloride in the presence of a chromium oxide catalyst supported on magnesium oxide-aluminum oxide prepared by coprecipitating magnesium salts, aluminum salts and chromium salts at 1: 1: 1. A method of oxidizing mercury in combustion exhaust gas. 삭제delete 제4항에 있어서, 상기 마그네슘 산화물-알루미늄 산화물에 담지된 크롬 산화물이 마그네슘염, 알루미늄염, 크롬염과 침전제를 물에 첨가하여 침전물을 형성하고, 상기 침전물을 공기 분위기 하에서 300∼700℃의 온도로 소성하여 제조되는 것을 특징으로 하는 연소 배기가스 중의 수은의 산화방법.The method of claim 4, wherein the chromium oxide supported on the magnesium oxide-aluminum oxide is added to magnesium water, aluminum salt, chromium salt and a precipitant to form a precipitate, the precipitate is a temperature of 300 ~ 700 ℃ under air atmosphere A method of oxidizing mercury in combustion exhaust gas, which is produced by firing. 삭제delete
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US20040253158A1 (en) 2003-02-07 2004-12-16 Mitsubishi Heavy Industries, Ltd. Method for removing mercury in exhaust gas and system therefor

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US20030170159A1 (en) * 2001-08-09 2003-09-11 Shintaro Honjo Method and apparatus for removing mercury from waste gas
US20040253158A1 (en) 2003-02-07 2004-12-16 Mitsubishi Heavy Industries, Ltd. Method for removing mercury in exhaust gas and system therefor

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CN104165508A (en) * 2014-08-06 2014-11-26 贵州省万山银河化工有限责任公司 Air volume control device and method for mercury catalyst drying systems
CN104165508B (en) * 2014-08-06 2016-06-08 贵州省万山银河化工有限责任公司 A kind of mercury catalyst dehumidification system air quantity controller and control method thereof

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