KR20190046555A - Inorganic adsorbent for removal of hydrogen sulfide in nitrogen base - Google Patents
Inorganic adsorbent for removal of hydrogen sulfide in nitrogen base Download PDFInfo
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Abstract
Description
본 발명은 질소 조건에서의 황화수소 제거용 무기 흡착제에 관한 것으로서, 보다 상세하게는, 바이오가스를 생산하는 과정 또는 설비와 같은 질소 조건에서 황화수소의 흡착성능을 향상시킬 수 있는 질소 조건에서의 황화수소 제거용 무기 흡착제에 관한 것이다.The present invention relates to an inorganic adsorbent for removing hydrogen sulfide at a nitrogen condition, and more particularly, to an inorganic adsorbent for removing hydrogen sulfide at a nitrogen condition capable of improving the adsorption performance of hydrogen sulfide under a nitrogen condition such as a process or a facility for producing biogas To an inorganic adsorbent.
악취는 황화수소, 메르캅탄류, 아민류 기타 자극성 있는 기체상 물질이 사람의 후각을 자극하여 불쾌감과 혐오감을 주는 냄새로, 인체에 미치는 위험성보다는 정신적, 심리적 피해를 끼치는 감각공해로서, 이러한 악취물질 중에서 황화수소는 바이오가스의 생산시에도 부수적으로 발생하고 있다. 바이오가스는 유기물질의 분해로 얻어진 가스로서 일반적으로 유기성폐기물의 혐기성소화를 통해 생성된 메탄가스(CH4)를 일컫는다. 이러한 바이오가스에는 sulfide, disulfide, thiol 등의 여러가지 황 화합물이 포함되고 있고, 고농도의 황화수소는 독성을 가지고, 저농도에서는 유기황화합물과 마찬가지로 강한 악취물질로 분류된다. Odor is a sensory pollution that causes mental and psychological harm rather than a danger to human body by the smell that hydrogen sulfide, mercaptans, amines and other irritating gaseous substances stimulate the smell of people by giving offensive and repulsive feeling. Among these odor substances, Are also incidental to the production of biogas. Biogas is a gas obtained by the decomposition of organic matter and generally refers to methane gas (CH4) produced by anaerobic digestion of organic waste. These biogas contain various sulfur compounds such as sulfide, disulfide, and thiol. High concentrations of hydrogen sulfide are toxic, and at low concentrations they are classified as strong odor substances as organic sulfur compounds.
이러한 황화수소는 대부분이 금속과 반응성이 크며, 응축된 수분에 용해되면 부식성이 있어 장치에 손상을 줄 수 있고, 황화수소와 접촉하는 윤활유는 오염되며 그에 따라 필요 이상으로 오일 교환을 자주 해 주어야 하며, 연소되면 법 규제 대상인 황산염 등 황산화물로 되고 부식성이 큰 특징을 갖는다. Most of these hydrogen sulphides are highly reactive with metals and are corrosive when dissolved in condensed water, which can damage the equipment, and the lubricating oil in contact with the hydrogen sulfide is contaminated, requiring frequent oil changes more than necessary, Sulfuric acid, sulfuric acid, and so on.
따라서 바이오가스를 사용하기 위해서는 생산된 바이오가스에서 황화수소를 제거하여야 하는데, 이러한 황화수소를 제거하기 위한 방법으로는, 소화조 내에서 황화수소를 제거하기 위하여 공기/산소를 주입하거나 철염을 주입하는 방법, 소화 후에는 철산화물 또는 수산화물을 이용하여 흡착하는 방법, 용매를 이용하여 흡수하는 방법, 반투과성막을 통하여 바이오가스로부터 분리하는 방법, 산화할 수 있는 특정 박테리아를 이용하는 생물여과 방법, 활성탄소로 흡착하는 방법들이 사용된다.Therefore, in order to use biogas, it is necessary to remove hydrogen sulfide from the produced biogas. Examples of the method for removing hydrogen sulfide include a method of injecting air / oxygen or iron salt to remove hydrogen sulfide in the digester, Methods of adsorption using iron oxide or hydroxide, adsorption using a solvent, separation from a biogas through a semi-permeable membrane, biofiltration using a specific oxidizable bacteria, and adsorption with activated carbon are used .
이러한 방법들 중에서 본 발명은 활성탄소로 흡착하는 방법을 개선한 것으로서, 일반적으로 활성탄소는 활성 알루미나, 제올라이트 및 실리카겔을 포함하여 구성되고, 공기중에서는 산화철 계열의 물질을 첨가시켜 황화수소의 흡착율을 증대시키고 있다.Among these methods, the present invention is an improvement of a method of adsorbing by activated carbon. Generally, the activated carbon is composed of activated alumina, zeolite and silica gel, and the adsorption rate of hydrogen sulfide is increased by adding an iron oxide- have.
그러나 공기중에서 거의 100%에 가깝게 우수한 황화수소 흡착성능을 나타내는 산화철 계열의 무기 흡착제는 바이오가스가 생성되는 소화조 내와 같은 질소(N2) 조건에서는 황화수소의 흡착율이 55% 이상 저하되는 한계가 있었다. 따라서 질소 조건에서 황화수소에 대한 흡착량을 증대시킬 수 있는 무기 흡착제의 개발이 요구되었다. However, iron oxide based inorganic adsorbents showing almost the same adsorption capacity of hydrogen sulfide as in almost 100% of the air have a limitation in that the adsorption rate of hydrogen sulfide is reduced by 55% or more under nitrogen (N 2 ) conditions as in the digester in which biogas is produced. Therefore, it is required to develop an inorganic adsorbent capable of increasing adsorption amount to hydrogen sulfide under nitrogen condition.
본 발명은 상기와 같은 문제점을 해결하기 위해 안출된 것으로서, 본 발명의 목적은, 바이오가스를 생산하는 과정 또는 설비와 같은 질소 조건에서 황화수소의 흡착성능을 향상시킬 수 있는 질소 조건에서의 황화수소 제거용 무기 흡착제를 제공하는 데 있다.SUMMARY OF THE INVENTION The present invention has been made in order to solve the above problems, and it is an object of the present invention to provide a method and apparatus for removing hydrogen sulfide at a nitrogen condition capable of improving the adsorption performance of hydrogen sulfide under a nitrogen condition, And an inorganic adsorbent.
상기한 바와 같은 목적을 달성하기 위한 본 발명의 특징에 따르면, 본 발명은, 질소 조건에서의 황화수소 제거용 무기 흡착제에 관한 것으로, 구리화합물, 수산화칼슘, 알루미나, 분말형 활성탄 및 탄산칼륨을 포함하여 구성되고, 보다 구체적으로는, 상기 구리화합물은 30~40중량%, 상기 수산화칼슘(Ca(OH)2)은 15~20중량%, 상기 알루미나는 10~15중량%, 상기 분말형 활성탄은 15~25중량%이고, 상기 탄산칼륨(K2CO3)은 15~25중량%으로 구성된다.According to an aspect of the present invention, there is provided an inorganic adsorbent for removing hydrogen sulfide in a nitrogen atmosphere. The inorganic adsorbent includes a copper compound, calcium hydroxide, alumina, powdered activated carbon, and potassium carbonate. (Ca (OH) 2 ) is 15 to 20% by weight, the alumina is 10 to 15% by weight, the powdered activated carbon is 15 to 25% by weight, and more specifically, the copper compound is 30 to 40% By weight, and the potassium carbonate (K 2 CO 3 ) is 15 to 25% by weight.
이때 상기 구리화합물은 산화구리(Ⅰ)(Cu2O), 산화구리(Ⅱ)(CuO), 탄산구리(Cu2CO3), 수산화구리(Cu(OH)2) 중 어느 하나인 것이 바람직하다.In this case, the copper compound is preferably any one of copper oxide (Ⅰ) (Cu 2 O) , copper oxide (Ⅱ) (CuO), copper carbonate (Cu 2 CO 3), copper hydroxide (Cu (OH) 2) one .
또한 상기 탄산칼륨은 분말상으로 가공되어 혼합되는 것이 바람직하다.Further, it is preferable that the above-mentioned potassium carbonate is processed and mixed in a powder form.
본 발명에 따른 질소 조건에서의 황화수소 제거용 무기 흡착제에 따르면, 바이오가스를 생산하는 과정 또는 설비와 같은 질소 조건에서 황화수소의 흡착성능을 향상시킬 수 있는 효과가 있다. According to the inorganic adsorbent for removing hydrogen sulfide in the nitrogen condition according to the present invention, the adsorption performance of hydrogen sulfide can be improved under a nitrogen condition such as a process or equipment for producing biogas.
도 1은 황화수소 제거 성능을 발휘하는 활성물질을 검증하기 위한 실험결과를 나타내는 그래프,
도 2는 산화구리(Ⅱ)(CuO)의 함량에 따른 황화수소의 흡착성능을 나타내는 그래프이다.1 is a graph showing experimental results for verifying an active material exhibiting hydrogen sulfide removal performance,
2 is a graph showing the adsorption performance of hydrogen sulfide according to the content of copper (II) oxide (CuO).
이하, 첨부된 도면을 참조하여 본 발명에 따른 황화수소 제거용 무기 흡착제의 구성을 자세히 설명한다.Hereinafter, the structure of the inorganic adsorbent for removing hydrogen sulfide according to the present invention will be described in detail with reference to the accompanying drawings.
본 발명에 따른 황화수소 제거용 무기 흡착제는 구리화합물 20~40중량%, 수산화칼슘(Ca(OH)2) 15~25중량%, 알루미나 10~30중량%, 분말형 활성탄 15~25중량%, 벤토나이트 3~7중량%, 및 탄산칼륨(K2CO3) 8~30중량%를 포함하여 구성된다. The inorganic adsorbent for removing hydrogen sulfide according to the present invention comprises 20 to 40 wt% of a copper compound, 15 to 25 wt% of calcium hydroxide (Ca (OH) 2 ), 10 to 30 wt% of alumina, 15 to 25 wt% of powdery activated carbon, To 7% by weight, and potassium carbonate (K 2 CO 3 ) in an amount of 8 to 30% by weight.
상기 구성요소 중에서 활성탄은, 종래기술에서도 언급한 바와 같이, 황화수소의 흡착 성능이 우수한 것으로 알려진 재료로서, 본 발명에서도 이들 재료를 활용하되, 보다 향상된 흡착성능을 발휘 및 유지하기 위해서 다양한 활성물질을 연구하였고, 그 결과로서 상기와 같은 구성요소들의 배합을 얻을 수 있게 되었다. Among the above-mentioned constituent elements, as mentioned in the prior art, activated carbon is a material known to have excellent adsorption performance of hydrogen sulfide. In the present invention, however, these active materials are utilized, And as a result, a combination of the above-described components can be obtained.
그리고 수산화칼슘과 알루미나에서 황화수소의 제거 효능은 특별히 발견되지 않지만, 흡착제의 강도 향상을 위하여 수산화칼슘이 첨가되고, 또한 알루미나는 활성알루미나 및 수산화알루미나 중에서 사용 가능하지만, 수산화칼슘과 더불어 강도향상에 기여할 뿐만 아니라 원가 절감이 가능한 수산화알루미나를 사용하는 것이 보다 바람직하다.Although the effect of removing hydrogen sulfide from calcium hydroxide and alumina is not particularly found, calcium hydroxide is added to improve the strength of the adsorbent, and alumina can be used in activated alumina and alumina hydroxide. However, in addition to calcium hydroxide, It is more preferable to use alumina hydroxide which can be used.
한편, 탄산칼륨(K2CO3)은 황화수소 제거 효능을 향상시킬 수 있는 활성물질로 확인된 재료로서, 분말상으로 가공되어 혼합되고, 전체 중량비에서 8~30중량% 범위 내에서 우수한 성능을 발휘하는 것으로 나타났다.On the other hand, potassium carbonate (K 2 CO 3 ) is a material identified as an active material capable of improving the hydrogen sulfide removal efficiency. It is processed and mixed in powder form, and exhibits excellent performance within a range of 8 to 30 wt% Respectively.
이러한 활성탄, 수산화칼슘, 알루미나 및 탄산칼슘은 황화수소 제거를 위한 무기 흡착제를 구성하는 기본 구성요소이지만, 이러한 구성요소만으로 무기 흡착제를 제조하면 질소 조건에서 황화수소의 흡착율이 좋지 않다. 따라서 본원발명에서는 구리화합물을 상기 구성요소에 첨가하여 무기흡착제를 제조하고, 이 경우 공기중에서 황화수소의 흡착율을 증가시키는데 사용될 수 있는 철화합물을 첨가하는 경우에 비해 1.5~2.0배의 흡착성능 향상을 나타낸다.These activated carbon, calcium hydroxide, alumina and calcium carbonate are basic constituent elements of inorganic adsorbents for the removal of hydrogen sulfide. However, the adsorption of hydrogen sulfide at the nitrogen condition is not good when an inorganic adsorbent is produced by only these constituents. Therefore, in the present invention, an inorganic adsorbent is prepared by adding a copper compound to the above-mentioned components, and in this case, the adsorption performance is improved by 1.5 to 2.0 times as compared with the case of adding an iron compound which can be used for increasing the adsorption rate of hydrogen sulfide in air .
이러한 구리화합물로는, 산화구리(Ⅰ)(Cu2O), 산화구리(Ⅱ)(CuO), 탄산구리(Cu2CO3), 수산화구리(Cu(OH)2)가 예시될 수 있다. Examples of such a copper compound include copper (I) (Cu 2 O), copper (II) oxide (CuO), copper carbonate (Cu 2 CO 3 ) and copper hydroxide (Cu (OH) 2 ).
이하에서는 상기와 같은 구성을 갖는 무기 흡착제의 황화수소 흡착성능에 대한 실험결과를 설명한다.Experimental results on the hydrogen sulfide adsorption performance of the inorganic adsorbent having the above-described structure will be described below.
먼저 질소 조건에서 철화합물을 사용한 경우와 본 발명에서와 같이 구리화합물을 사용한 경우에 황화수소의 흡착 성능에 차이가 있는지에 대해 실험하였다.First, the adsorption performance of hydrogen sulfide was examined in the case of using iron compound in nitrogen condition and in case of using copper compound as in the present invention.
즉, 수산화칼슘, 알루미나, 분말 활성탄 및 벤토나이트의 배합비율은 고정한 상태에서 철화합물로서 Fe2O3 레진을 사용한 경우를 비교예 1, FeOOH 레진을 사용한 경우를 비교예 2로 하고, 구리화합물로서 산화구리(Ⅰ)(Cu2O) 레진을 사용한 경우를 실시예 1, 산화구리(Ⅱ)(CuO) 레진을 사용한 경우를 실시예 2, 탄산구리(Cu2CO3) 레진을 사용한 경우를 실시예 3, 수산화구리(Cu(OH)2) 레진을 사용한 경우를 실시예 4로 하여 황화수소의 제거 성능을 실험하였다. 실험은 질소 조건에서 상대습도 45%, 활성물질인 탄산칼륨을 18중량%로 하였고, 철화합물과 구리화합물은 30중량%을 첨가하여 실시하였다. That is, Comparative Example 1 in which Fe 2 O 3 resin was used as an iron compound, Comparative Example 2 in which FeOOH resin was used was used as the iron compound in a state where the mixing ratio of calcium hydroxide, alumina, powdered activated carbon and bentonite was fixed, (ⅰ) (Cu 2 O) subjected to the embodiment, if the case of using the resin used in example 1, the copper oxide (ⅱ) (CuO) resin example 2, copper carbonate (Cu 2 CO 3) when using resins example 3 , And copper hydroxide (Cu (OH) 2 ) resin was used as Example 4, the hydrogen sulfide removal performance was tested. The experiment was carried out under a nitrogen atmosphere at a relative humidity of 45%, potassium carbonate as an active material at 18 wt%, and an iron compound and a copper compound at 30 wt%.
그 결과, 도 1에 도시된 바와 같이, Fe2O3 레진을 첨가한 비교예 1의 경우에는 대략 40~50 흡착당량(Gas L/Resin L)을 나타내고, FeOOH 레진을 첨가하는 비교예 2의 경우에는 대략 20~30 흡착당량(Gas L/Resin L)을 나타나는 것으로 시험결과 확인되었다. As a result, as shown in Fig. 1, in the case of Comparative Example 1 in which Fe 2 O 3 resin was added, it was found that in Comparative Example 2 in which FeOOH resin was added in an amount of about 40 to 50 adsorption equivalents (Gas L / Resin L) (Gas L / Resin L) of about 20 to 30 adsorption equivalents.
반면에 산화구리(Ⅰ)(Cu2O)를 구리화합물로 사용하는 실시예 1의 경우에는, 대략 75.67 흡착당량(Gas L/Resin L)을 나타내었고, 산화구리(Ⅱ)(CuO)를 구리화합물로 사용하는 실시예 2의 경우에는, 대략 66.67 흡착당량(Gas L/Resin L)을 나타내었으며, 탄산구리(Cu2CO3)를 구리화합물로 사용하는 실시예 3의 경우에는, 대략 50.53 흡착당량(Gas L/Resin L)을 나타내었고, 수산화구리(Cu(OH)2)를 구리화합물로 사용하는 실시예 4의 경우에는, 대략 61.67 흡착당량(Gas L/Resin L)을 나타내었다. 따라서 구리화합물을 사용하는 경우가 철화합물을 사용하는 경우에 비해 적어도 13% 이상의 흡착성능 향상을 나타내고, 산화구리(Ⅰ)(Cu2O)를 사용하는 경우에는 69~184%의 흡착성능 향상을 확인할 수 있다.On the other hand, Example 1 using copper (I) (Cu 2 O) as a copper compound exhibited an adsorption equivalent of about 75.67 (Gas L / Resin L) and copper (II) In the case of Example 2, which was used as a compound, the adsorption equivalent (Gas L / Resin L) was approximately 66.67, and in the case of Example 3 using copper carbonate (Cu 2 CO 3 ) as the copper compound, approximately 50.53 adsorption (Gas L / Resin L), and in the case of Example 4 where copper hydroxide (Cu (OH) 2 ) was used as the copper compound, the adsorption equivalent amount (Gas L / Resin L) was approximately 61.67. Therefore, the use of a copper compound shows an improvement in adsorption performance by at least 13% compared to the case of using an iron compound, and an improvement in adsorption performance of 69 to 184% when copper (I) (Cu 2 O) Can be confirmed.
다음으로 무기 흡착제가 최고의 흡착성능을 발휘할 수 있는 구리화합물의 배합비를 확인하기 위한 실험을 소개한다.Next, we introduce an experiment to confirm the compounding ratio of the copper compound which can exhibit the best adsorption performance of the inorganic adsorbent.
본 실험에서는 구리화합물로서 산화구리(Ⅱ)(CuO) 레진을 사용하되, 활성탄은 17중량%로, 탄산칼륨은 18중량%로 배합비를 고정하고 황화수소의 흡착과 직접적인 관련이 없는 구성요소인 수산화칼슘과 알루미나의 배합비와 산화구리(Ⅱ)(CuO)의 배합비를 조정하여 산화구리(Ⅱ)(CuO)의 함량에 따른 황화수소의 흡착성능을 확인하였다. 조정된 배합비율은 다음의 [표 1]에 기재된 바와 같다.In this experiment, copper (II) oxide (CuO) resin was used as the copper compound. The amount of activated carbon was 17% by weight, the amount of potassium carbonate was 18% by weight, and the amount of calcium hydroxide, which is a component not directly related to the adsorption of hydrogen sulfide, The adsorption performance of hydrogen sulfide was confirmed by adjusting the compounding ratio of alumina and the mixing ratio of copper (II) oxide (CuO) according to the content of copper (II) oxide (CuO). The adjusted mixing ratio is as shown in the following [Table 1].
그 결과, 도 2에 도시된 바와 같이, 실시예 5는 66.67 흡착당량(Gas L/Resin L)을 나타내었고, 실시예 6은 86.33 흡착당량(Gas L/Resin L)을 나타내었으며, 실시예 7은 104.77 흡착당량(Gas L/Resin L)을 나타내었다. 이로써, 구리화합물인 산화구리(Ⅱ)(CuO)의 함유량이 증가할수록 황화수소의 흡착당량이 증가하는 것을 알 수 있다. As a result, as shown in FIG. 2, Example 5 showed an adsorption equivalent of 66.67 (Gas L / Resin L), Example 6 showed an adsorption equivalent of 86.33 (Gas L / Resin L) Showed an adsorption equivalent of 104.77 (Gas L / Resin L). As a result, it can be seen that the adsorption equivalent of hydrogen sulfide increases with an increase in the content of copper (II) oxide (CuO), which is a copper compound.
이때 산화구리(Ⅱ)(CuO)의 첨가량이 30중량% 미만이거나 40중량%를 초과하는 경우에 대해 살펴보면, 도시되지는 않았지만, 산화구리(Ⅱ)(CuO)의 첨가량이 30중량% 미만이면 수산화칼슘 및 알루미나의 첨가량이 증대됨에 따라 무기 흡착제의 강도가 필요 이상으로 증대되어 오히려 흡착성능의 저하를 나타내었고, 산화구리(Ⅱ)(CuO)의 첨가량이 40중량%를 초과하는 경우에는 흡착성능은 다소 상승하나, 수산화칼슘 및 알루미나의 첨가량이 감소됨에 따라 무기 흡착제가 쉽게 파쇄되는 현상을 나타내었다. 따라서 산화구리(Ⅱ)(CuO)의 첨가량이 30~40중량% 범위일 때 황화수소의 흡착성능도 우수하면서도 무기 흡착제의 사용성도 우수한 것을 확인하였다.If the addition amount of copper (II) oxide (CuO) is less than 30 wt% or more than 40 wt%, though not shown, if the addition amount of copper (II) oxide (CuO) is less than 30 wt% (II) (CuO) was added in an amount of more than 40 wt%, the adsorption performance was somewhat higher than that of the adsorbent However, as the amount of calcium hydroxide and alumina was decreased, the inorganic adsorbent was easily broken. Therefore, it was confirmed that when the addition amount of copper (II) oxide (CuO) was in the range of 30 to 40 wt%, the adsorption performance of hydrogen sulfide was excellent, and the usability of the inorganic adsorbent was also excellent.
이상에서와 같이 본 발명의 권리는 위에서 설명된 실시예에 한정되지 않고 청구범위에 기재된 바에 의해 정의되며, 본 발명의 분야에서 통상의 지식을 가진 자가 청구범위에 기재된 권리범위 내에서 다양한 변형과 개작을 할 수 있다는 것은 자명하다.It will be apparent to those skilled in the art that various modifications and variations can be made in the present invention without departing from the spirit or scope of the invention as defined by the appended claims. It is obvious that you can do it.
Claims (4)
상기 구리화합물은 30~40중량%, 상기 수산화칼슘(Ca(OH)2)은 15~20중량%, 상기 알루미나는 10~15중량%, 상기 분말형 활성탄은 15~25중량%이고, 상기 탄산칼륨(K2CO3)은 15~25중량%인 것을 특징으로 하는 질소 조건에서의 황화수소 제거용 무기 흡착제.The method according to claim 1,
Wherein the copper compound is 30 to 40 wt%, the calcium hydroxide (Ca (OH) 2 ) is 15 to 20 wt%, the alumina is 10 to 15 wt%, the powdery activated carbon is 15 to 25 wt% (K 2 CO 3 ) is 15 to 25% by weight based on the total weight of the inorganic adsorbent.
상기 구리화합물은 산화구리(Ⅰ)(Cu2O), 산화구리(Ⅱ)(CuO), 탄산구리(Cu2CO3), 수산화구리(Cu(OH)2) 중 어느 하나인 것을 특징으로 하는 질소 조건에서의 황화수소 제거용 무기 흡착제.3. The method of claim 2,
The copper compounds, characterized in that any one of copper oxide (Ⅰ) (Cu 2 O) , copper oxide (Ⅱ) (CuO), copper carbonate (Cu 2 CO 3), copper hydroxide (Cu (OH) 2) one An inorganic adsorbent for removing hydrogen sulfide under nitrogen.
상기 탄산칼륨은 분말상으로 가공되어 혼합되는 것을 특징으로 하는 질소 조건에서의 황화수소 제거용 무기 흡착제.3. The method of claim 2,
Wherein the potassium carbonate is processed and mixed in a powder form to be mixed with the inorganic adsorbent for removing hydrogen sulfide at a nitrogen condition.
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