KR100451820B1 - Removal method of oxygen in coke oven gas - Google Patents

Removal method of oxygen in coke oven gas Download PDF

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KR100451820B1
KR100451820B1 KR10-2002-0052148A KR20020052148A KR100451820B1 KR 100451820 B1 KR100451820 B1 KR 100451820B1 KR 20020052148 A KR20020052148 A KR 20020052148A KR 100451820 B1 KR100451820 B1 KR 100451820B1
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cog
oxygen
ordination
nitrite
cyclohexylamine
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KR20040020539A (en
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이현
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주식회사 포스코
주식회사 유니테크
재단법인 포항산업과학연구원
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    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
    • C10K1/00—Purifying combustible gases containing carbon monoxide
    • C10K1/08—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors
    • C10K1/10—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors with aqueous liquids
    • C10K1/103—Purifying combustible gases containing carbon monoxide by washing with liquids; Reviving the used wash liquors with aqueous liquids alkali- or earth-alkali- or NH4 salts or inorganic acids derived from sulfur
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10B—DESTRUCTIVE DISTILLATION OF CARBONACEOUS MATERIALS FOR PRODUCTION OF GAS, COKE, TAR, OR SIMILAR MATERIALS
    • C10B45/00—Other details
    • C—CHEMISTRY; METALLURGY
    • C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
    • C10K—PURIFYING OR MODIFYING THE CHEMICAL COMPOSITION OF COMBUSTIBLE GASES CONTAINING CARBON MONOXIDE
    • C10K1/00—Purifying combustible gases containing carbon monoxide
    • C10K1/002—Removal of contaminants

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Combustion & Propulsion (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

본 발명은 코크오븐가스중에 함유된 산소를 제거하는 방법에 관한 것으로,The present invention relates to a method for removing oxygen contained in the coke oven gas,

코크스 제조과정에서 발생하는 COG(코크오븐가스)중의 산소를 제거하는 방법에 있어서,In the method for removing oxygen in the COG (coke oven gas) generated during the coke manufacturing process,

안수중에 시클로헥실아민을 최소 0.5중량%이상 함유시켜 용해하고, 상기 안수 1리터당 아질산염을 최소 3g이상 함유시켜 용해하는 단계; 및At least 0.5% by weight of cyclohexylamine is dissolved in ordination, and at least 3 g of nitrite is dissolved per liter of ordination; And

상기 시클로헥실아민과 아질산염이 함유된 안수를 흡수탑에서 분사하는 한편, 상기 흡수탑에서 COG와 상기 안수가 접촉되도록 COG를 흡수탑에 통과시켜 산소를 제거하는 단계;를 포함함을 특징으로 하는 COG중에 함유된 산소 제거 방법이 제공된다.Spraying the ordination containing the cyclohexylamine and nitrite in the absorption tower, while passing the COG through the absorption tower to contact the COG and the ordination in the absorption tower to remove oxygen; The oxygen removal method contained in the inside is provided.

본 발명의 방법은 안수에 시클로헥실아민과 아질산염을 함유시킴으로써 COG 중 산소를 선택적으로 제거할 수 있어 COG 폭발의 위험성을 감소시키며, 또한 COG중의 산소농도 과다로 인하여 배관내에서 배송시 발생하는 COG배관의 부식을 억제할 수 있는 효과가 있다.The method of the present invention can selectively remove oxygen in COG by incorporating cyclohexylamine and nitrite in the ordination to reduce the risk of COG explosion, and also to reduce the risk of COG explosion. There is an effect that can suppress corrosion.

Description

코크오븐가스중에 함유된 산소 제거 방법{REMOVAL METHOD OF OXYGEN IN COKE OVEN GAS}Oxygen removal method in coke oven gas {REMOVAL METHOD OF OXYGEN IN COKE OVEN GAS}

본 발명은 COG에 함유된 산소를 제거하는 방법에 관한 것으로, 보다 상세하게는 COG내의 함유된 산소를 시클로헥실아민과 아질산염이 함유된 안수를 이용하여 화학적흡착 및 화학반응을 통해 효율적으로 제거하는 방법에 관한 것이다.The present invention relates to a method for removing oxygen contained in COG, and more particularly, to efficiently remove oxygen contained in COG by chemical adsorption and chemical reaction using ordination containing cyclohexylamine and nitrite. It is about.

석탄을 이용한 건류공정을 통한 코크스 제조과정에서 COG(coke oven gas, 이하 'COG'라고 한다.), 타르 및 수분이 발생되는데, 이러한 생성물중에서 타르 및 수분은 액상상태로 회수 처리되며, 가스상태인 COG는 포집되어 제철소내의 에너지원으로 사용된다. 그러나, COG 중에는 산소가 일부 함유되어 있어 에너지원의 발열량에 도움이 되지 않으며, 산소가 COG중에 함유되어 있으면, 폭발의 위험이 내재하게 된다.Coke oven gas (COG), tar, and water are generated during the coke manufacturing process using a coal distillation process using coal. Among these products, tar and water are recovered and processed in a liquid state. COG is collected and used as an energy source in steel mills. However, some oxygen is contained in the COG, which does not contribute to the calorific value of the energy source. If the oxygen is contained in the COG, the risk of explosion is inherent.

COG를 정제하는데 안수를 사용하여 유화수소 등을 제거하는데 산소성분은 제거가 어렵다. 또한 COG중에 함유된 산소는 불순물로 작용하는 유화수소를 제거하는데 방해물질로 알려지고 있다.Ordination is used to purify COG to remove hydrogen, etc., but it is difficult to remove oxygen. In addition, oxygen contained in COG is known to be an obstacle to the removal of hydrogen sulfide as an impurity.

또한, 종래의 방법으로는 COG중의 산소를 제거하기 위해서는 고체의 산소흡착제를 사용하는 경우가 있는데 이는 노화가 빨리 일어나서 공정상에서는 어려움이 많다. 또한 이물질의 부착으로 인하여 효율성이 저하되는 단점이 있다.In addition, in the conventional method, a solid oxygen adsorbent may be used to remove oxygen in COG, which is difficult to process due to rapid aging. In addition, there is a disadvantage that the efficiency is reduced due to the attachment of foreign matter.

이에 본 발명의 목적은 시클로헥실아민과 아질산염을 안수에 용해하여 COG내에 함유되어있는 산소를 효과적으로 제거하는 방법을 제공하는 것이다.Accordingly, an object of the present invention is to provide a method for effectively removing oxygen contained in COG by dissolving cyclohexylamine and nitrite in ordination.

도 1은 시클로헥실아민의 농도별 처리후 COG중 산소농도를 측정한 결과이며,1 is a result of measuring the oxygen concentration in COG after treatment of each concentration of cyclohexylamine,

도 2는 아질산염의 농도별 처리후 COG중 산소농도를 측정한 결과이며, 그리고Figure 2 is the result of measuring the oxygen concentration in COG after treatment for each concentration of nitrite, and

도 3은 시클로헥실아민과 아질산염을 모두 사용하여 농도별로 처리한 후 COG중의 산소농도를 측정한 결과이다.3 is a result of measuring the oxygen concentration in COG after treatment by concentration using both cyclohexylamine and nitrite.

본 발명의 일견지에 의하면, 코크스 제조과정에서 발생하는 COG(코크오븐가스)중의 산소를 제거하는 방법에 있어서,According to one aspect of the present invention, in the method for removing oxygen in the COG (coke oven gas) generated during the coke production process,

안수중에 시클로헥실아민을 최소 0.5중량%이상 함유시켜 용해하고, 상기 안수 1리터당 아질산염을 최소 3g이상 함유시켜 용해하는 단계; 및At least 0.5% by weight of cyclohexylamine is dissolved in ordination, and at least 3 g of nitrite is dissolved per liter of ordination; And

상기 시클로헥실아민과 아질산염이 함유된 안수를 흡수탑에서 분사하는 한편, 상기 흡수탑에서 COG와 상기 안수가 접촉되도록 COG를 흡수탑에 통과시켜 산소를 제거하는 단계;를 포함함을 특징으로 하는 COG중에 함유된 산소 제거 방법이 제공된다.Spraying the ordination containing the cyclohexylamine and nitrite in the absorption tower, while passing the COG through the absorption tower to contact the COG and the ordination in the absorption tower to remove oxygen; The oxygen removal method contained in the inside is provided.

이하, 본 발명에 대하여 상세히 설명한다.EMBODIMENT OF THE INVENTION Hereinafter, this invention is demonstrated in detail.

본 발명은 코크스 제조과정에서 발생되는 COG중에 함유되어 있는 산소를 효율적으로 제거하는 방법에 관한 것으로, 본 발명자들은 안수에 시클로헥실아민과 아질산나트륨을 용해시켜 이것을 COG와 접촉시키는 경우 화학적 흡착 및 화학적 반응으로 COG중에 함유된 산소가 선택적으로 제거됨을 예기치않게 발견하였다.The present invention relates to a method for efficiently removing the oxygen contained in the COG generated during the coke production process, the present inventors dissolve cyclohexylamine and sodium nitrite in the ordination and the chemical adsorption and chemical reaction when contacted with COG Unexpectedly found that the oxygen contained in the COG was selectively removed.

본 발명에 따라, 코크스 제조과정에서 발생하는 COG 중에 산소를 제거하기 위해서 기존에 사용하는 안수에, 시클로헥실아민이 최소 0.5중량%로 함유되도록 용해시키고 또한 아질산나트륨이 안수 1리터당 최소 3g으로 함유되도록 용해시킨다.According to the present invention, cyclohexylamine is dissolved in at least 0.5% by weight in the existing ordination to remove oxygen in the COG generated during coke production, and sodium nitrite is contained in at least 3 g per liter of ordination. Dissolve.

시클로헥실아민은 산소와 친화성이 강하여 산소를 화학적으로 흡착한다. COG중의 산소는 시클로아민의 환형고리내 이온과의 화학적 흡착으로 그리고 시클로헥실아민의 아미노기와 일부 반응하여 흡착된다. 따라서 이러한 화학흡착 현상을 이용하여 COG중의 산소를 선택적으로 제거하는 것이 가능하다.Cyclohexylamine has a high affinity with oxygen and chemically adsorbs oxygen. Oxygen in COG is adsorbed by chemical adsorption of cycloamines with ions in the cyclic ring and in part by reaction with amino groups of cyclohexylamines. Therefore, it is possible to selectively remove oxygen in the COG using this chemisorption phenomenon.

아질산염은 화학반응에 의해 산소를 제거하며, 그 화학반응은 하기 반응식 1과 같다. 아질산염은 바람직하게 아질산나트륨을 사용한다.Nitrite removes oxygen by a chemical reaction, and the chemical reaction is shown in Scheme 1 below. Nitrite preferably uses sodium nitrite.

NO2 -+ 1/2O2→NO3 - NO 2 - + 1 / 2O 2 → NO 3 -

즉, 아질산나트륨과 코크스오븐중의 산소가 반응하게 되는 경우, 아질산나트륨의 아질산 이온이 산소와 반응하여 질산이온이 되어 COG중의 산소를 제거한다.That is, when sodium nitrite reacts with oxygen in the coke oven, nitrite ions of sodium nitrite react with oxygen to form nitrate ions to remove oxygen in COG.

상기 반응을 통하여 COG중의 산소를 선택적으로 제거하는 것이 가능하다.It is possible to selectively remove oxygen in COG through the reaction.

바람직하게, 상기 시크로헥실아민을 0.5∼2.5중량%로 함유시키는 것이 산소를 선택적으로 흡착시키는데는 효과적이며, 아질산염은 안수 1리터당 3-6g함유시켜 제조한 안수를 사용하는 경우 효과적이다. 즉, 시클로헥실아민이 안수에 0.5중량%미만으로 함유되는 경우에는 산소와의 충분한 흡착성을 나타내지못하며, 또한 2.5중량%이상으로 함유되는 경우에는 산소 흡착성이 더이상 증가하지않아 경제적이지 못하여 비효율적이며 그리고 아질산염은 안수 1리터당 3g미만으로 함유되는 경우에는 산소제거효과가 미약하며 6g이상으로 함유되는 경우에는 더 이상 산소제거효과가 증가하지않아 불필요하여 비경제적이다.Preferably, containing 0.5 to 2.5% by weight of the cyclohexylamine is effective for selectively adsorbing oxygen, and nitrite is effective when using ordinal water prepared by containing 3-6 g per liter of ordination. In other words, when cyclohexylamine is contained in less than 0.5% by weight, it does not show sufficient adsorption with oxygen, and when it is contained in more than 2.5% by weight, oxygen adsorption is no longer increased, so it is not economical, which is inefficient and nitrite. If less than 3g per 1 liter of ordination, the oxygen removal effect is insignificant. If it is contained more than 6g, the oxygen removal effect is not increased anymore, so it is uneconomical.

이러한 시클로헥실아민과 아질산염이 함유된 안수를 흡수탑에서 분사하고, 흡수탑에서 COG와 상기 안수가 접촉되도록 COG를 흡수탑에 통과시킴으로써 상술한 바와 같은 반응을 통해 COG중의 산소가 제거된다.The oxygen in the COG is removed through the reaction as described above by spraying the ordination containing the cyclohexylamine and nitrite in the absorption tower, and passing the COG through the absorption tower so that the COG and the ordination contact the absorption tower.

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

실시예 1Example 1

본 실시예에서는 안수중에 시클로헥실아민을 함유시켜 COG중에 함유된 산소제거를 위한 실험을 실시하였다. 안수중에 시클로헥실아민을 0.5중량%에서 3중량%까지 0.5중량% 간격으로 변화시키면서 첨가시켜 시클로헥실아민이 함유된 안수를제조하고, 이를 흡수탑에서 분사시켜 COG에 통과시키면서 초기의 COG중의 산소농도가 제거되는 양을 측정하였다. 초기에 COG중에 함유된 산소농도는 1.2%가 함유된 시료이다.In this example, the experiment was carried out to remove oxygen contained in COG by containing cyclohexylamine in ordination. Cyclohexylamine is added in the ordination at 0.5 wt% to 3 wt% at 0.5 wt% intervals to prepare ordination containing cyclohexylamine, which is sprayed through an absorption tower and passed through the COG to the initial oxygen concentration in the COG. Was measured. Initially, the oxygen concentration in COG is a sample containing 1.2%.

안수중에 함유된 시클로헥실아민의 농도별로 처리후의 COG중 산소농도를 하기 도 1에 나타내었다. 도 1에 나타낸 바와 같이, 시클로헥실아민을 첨가하지 않는 경우는 COG중의 산소가 거의 제거되지 않았지만, 0.5중량%이상이 함유된 경우는 상당한 산소흡착제거의 효과를 나타내었다. 또한, 시클로헥실아민이 3중량%이상의 농도로 함유된 경우에서는 시클로헥실아민의 부가적인 첨가량에 비해 더 이상 산소제거효과가 증가하지않아, 시클로헥실아민은 0.5~2.5중량%의 농도로 함유되는 것이 보다 바람직함을 알 수 있다.Oxygen concentration in COG after treatment for each concentration of cyclohexylamine contained in ordination is shown in FIG. 1. As shown in FIG. 1, when cyclohexylamine was not added, oxygen in COG was hardly removed, but when 0.5 wt% or more was contained, significant oxygen adsorption removal was shown. In addition, when cyclohexylamine is contained at a concentration of 3% by weight or more, the oxygen removal effect is no longer increased compared to the additional amount of cyclohexylamine, and cyclohexylamine is contained at a concentration of 0.5 to 2.5% by weight. It is understood that more preferable.

또한 상기의 방법으로는 전체적인 산소농도를 0.5%이하로 유지시키기는 어렵다는 것을 알 수 있어서 다른 방법인 화학적 반응을 이용하는 것이 필요하다고 사료되어 아질산염을 이용하여 화학적 반응에 의한 산소를 제거하는 방법을 하기 실시예 2와 같이 실시하였다.In addition, it can be seen that it is difficult to maintain the overall oxygen concentration below 0.5% by the above method, so it is considered necessary to use another method, a chemical reaction. It implemented like Example 2.

실시예 2Example 2

본 실시예에서는 아질산나트륨에 의한 화학적 반응에 의한 산소제거하는 방법을 실시하였으며, 안수 리터당 아질산나트륨을 2g에서 7g까지 1g 단위로 안수중에 함유시켜, 각각의 용액을 제조한 후에 흡수탑에서 분사시켜 COG를 통과시키면서초기의 COG중의 산소농도가 제거되는 양을 측정하였다. 초기에 COG중에 함유된 산소농도는 1.2%가 함유된 시료이었다. 실시예 1과 같은 COG를 이용하여 실시한 결과로 COG중에 함유된 산소농도를 도 2에 나타내었다.In this embodiment, a method of removing oxygen by a chemical reaction with sodium nitrite was carried out, and sodium nitrite per liter of ordination was contained in ordinal water in 1 g units from 2 g to 7 g, and each solution was prepared and then sprayed in an absorption tower to produce COG. The amount of oxygen concentration in the initial COG was removed while passing through. Initially, the oxygen concentration in COG was a sample containing 1.2%. As a result of using the same COG as Example 1, the oxygen concentration contained in the COG is shown in FIG.

도 2에 나타낸 바와 같이, 아질산나트륨 2g이하에서는 산소제거효과가 크게 나타나지 않았으며, 3g이상에서 산소제거효과가 매우 크게 나타났다. 또한 7g 이상에서는 6g 첨가시와 거의 같은 효과를 나타내고 있어, 따라서 안수 리터당 아질산나트륨을 3g에서 6g까지 사용하는 것이 보다 바람직함을 알 수 있었다.As shown in FIG. 2, the oxygen removal effect was not significantly increased at 2 g or less of sodium nitrite, and the oxygen removal effect was very large at 3 g or more. In addition, at 7 g or more, the effect was almost the same as when 6 g was added. Therefore, it was found that it is more preferable to use sodium nitrite from 3 g to 6 g per liter of ordination.

실시예 3Example 3

실시예 3에서는 실시예 1과 2의 결과를 참조하여 하기 표 1과 같이 시클로헥실아민과 아질산염을 동시에 첨가하여 COG 정제에 사용후 산소농도를 비교하기 위해서 시험을 실시하였다. 실시예 3의 결과를 도 3에 나타내었다.In Example 3, with reference to the results of Examples 1 and 2, cyclohexylamine and nitrite were simultaneously added as shown in Table 1, and then tested to compare oxygen concentrations after use in COG purification. The result of Example 3 is shown in FIG.

구분division 시클로헥실아민농도(중량%)Cyclohexylamine concentration (% by weight) 아질산염 g수/안수리터Nitrite g water / laying on of hands 비교예1Comparative Example 1 0.10.1 1One 발명예1Inventive Example 1 0.50.5 33 발명예2Inventive Example 2 1.51.5 44 발명예3Inventive Example 3 2.52.5 66 발명예4Inventive Example 4 3.03.0 77

도 3에 나타낸 바와 같이, 비교예 1에서는 COG중의 산소제거효과가 미약하였으나, 본 발명의 범위내 농도를 갖는 경우인 발명예 2-4는 매우 효과적인 산소제거능을 나타냄을 알 수 있었다. 또한, 시클로헥실아민과 아질산염을 동시에 사용하는경우 산소제거효과는 단독으로 사용하는 경우보다(실시예 1 및 2) 크게 증대됨을 알 수 있었다.As shown in FIG. 3, in Comparative Example 1, the oxygen removal effect in COG was weak, but Inventive Example 2-4 having a concentration within the range of the present invention showed a very effective oxygen removal ability. In addition, when using the cyclohexylamine and nitrite at the same time it was found that the oxygen removal effect is significantly increased than when used alone (Examples 1 and 2).

본 발명의 방법은 안수에 시클로헥실아민과 아질산염을 함유시킴으로써 COG 중 산소를 선택적으로 제거할 수 있어 COG의 폭발위험성을 감소시키며, 또한 COG중의 산소농도 과다로 인하여 배관내에서 배송시 발생하는 COG배관의 부식을 억제할 수 있는 효과가 있다. 또한 본 발명의 방법은 기존의 COG를 정제하는 안수에 적용하여 사용되므로 편리한 적용성을 갖는다.The method of the present invention can selectively remove oxygen in COG by incorporating cyclohexylamine and nitrite in the ordination to reduce the risk of explosion of COG, and also to reduce the risk of COG piping. There is an effect that can suppress corrosion. In addition, the method of the present invention has a convenient applicability since it is applied to ordination to purify existing COG.

Claims (3)

코크스 제조과정에서 발생하는 COG(코크오븐가스)중의 산소를 제거하는 방법에 있어서,In the method for removing oxygen in the COG (coke oven gas) generated during the coke manufacturing process, 안수중에 시클로헥실아민을 최소 0.5중량%이상 함유시켜 용해하고, 상기 안수 1리터당 아질산염을 최소 3g이상 함유시켜 용해하는 단계; 및At least 0.5% by weight of cyclohexylamine is dissolved in ordination, and at least 3 g of nitrite is dissolved per liter of ordination; And 상기 시클로헥실아민과 아질산염이 함유된 안수를 흡수탑에서 분사하는 한편, 상기 흡수탑에서 COG와 상기 안수가 접촉되도록 COG를 흡수탑에 통과시켜 산소를 제거하는 단계;를 포함함을 특징으로 하는 COG중에 함유된 산소 제거 방법.Spraying the ordination containing the cyclohexylamine and nitrite in the absorption tower, while passing the COG through the absorption tower to contact the COG and the ordination in the absorption tower to remove oxygen; Oxygen removal method contained in the process. 제 1항에 있어서, 상기 안수중에 시클로헥실아민은 0.5~2.5중량%로 그리고 아질산염은 안수 1리터당 3~6g 함유시켜 용해함을 특징으로 하는 COG중에 함유된 산소 제거 방법.The method for removing oxygen contained in COG according to claim 1, wherein the cyclohexylamine is 0.5 to 2.5% by weight and the nitrite is dissolved in 3 to 6 g per liter of ordination. 제 1항에 있어서, 상기 아질산염은 아질산나트륨임을 특징으로 하는 방법.The method of claim 1 wherein the nitrite is sodium nitrite.
KR10-2002-0052148A 2002-08-30 2002-08-30 Removal method of oxygen in coke oven gas KR100451820B1 (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61230792A (en) * 1985-04-03 1986-10-15 Nippon Kokan Kk <Nkk> Method for nitrating and denitriding coke oven gas liquid
KR880003161A (en) * 1985-08-26 1988-05-14 이.유진 인니스 Gas generation process with cascade heat recovery
JPS63278591A (en) * 1987-05-11 1988-11-16 Sumikin Chem Co Ltd Method for removing ammonia from thiocyanate solution obtained from desulfurization waste liquid

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS61230792A (en) * 1985-04-03 1986-10-15 Nippon Kokan Kk <Nkk> Method for nitrating and denitriding coke oven gas liquid
KR880003161A (en) * 1985-08-26 1988-05-14 이.유진 인니스 Gas generation process with cascade heat recovery
JPS63278591A (en) * 1987-05-11 1988-11-16 Sumikin Chem Co Ltd Method for removing ammonia from thiocyanate solution obtained from desulfurization waste liquid

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