KR20020037609A - The method of manufacturing about adsorbent for harmful gas removal - Google Patents

The method of manufacturing about adsorbent for harmful gas removal Download PDF

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KR20020037609A
KR20020037609A KR1020000067631A KR20000067631A KR20020037609A KR 20020037609 A KR20020037609 A KR 20020037609A KR 1020000067631 A KR1020000067631 A KR 1020000067631A KR 20000067631 A KR20000067631 A KR 20000067631A KR 20020037609 A KR20020037609 A KR 20020037609A
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adsorbent
impregnated
adsorption
inorganic
harmful gas
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이후근
장길남
김성렬
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이후근
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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
    • 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
    • B01D53/48—Sulfur compounds
    • B01D53/52—Hydrogen sulfide
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2253/00—Adsorbents used in seperation treatment of gases and vapours
    • B01D2253/10—Inorganic adsorbents
    • B01D2253/112—Metals or metal compounds not provided for in B01D2253/104 or B01D2253/106
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D2257/00—Components to be removed
    • B01D2257/30—Sulfur compounds
    • B01D2257/304—Hydrogen sulfide

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

Abstract

PURPOSE: A manufacturing method of adsorbent for removing harmful gas is provided, which can be used for an extended time thus extending exchanging time of adsorbent. The inorganic adsorbent excellent in removing efficiency does not cause any fire thus reducing fire accident. CONSTITUTION: The harmful gas removing adsorbent is manufactured as the follows: adsorb metal salt such as Cu by 10-50 %, K and Mn to inorganic adsorbent to remove TEOS or SiH4.

Description

유해가스 제거용 흡착제 제조방법{The method of manufacturing about adsorbent for harmful gas removal}The method of manufacturing about adsorbent for harmful gas removal

산업화와 더불어 대기 배출오염원과 그 종류가 다양해지고 있어 점차 인체에 유해한 대기 오염물질에 대한 관심도가 높아지고 있다. 특히 시 구역이 점차 확대됨에 따라 환경 기초시설이 주거지역과 근접하게 됨에 따라 발생하는 악취는 2차 공해를 유발하여 주변 인접지역의 주요 악취물질로는 황화수소와 암모니아로 보고되고 있다. 또한 반도체 공정 중에 존재하는 유해가스는 공정상에 문제가 발생하여 유해가스를 제거해야 할 필요성이 있다.With the industrialization and the diversification of air pollutants and their types, there is a growing interest in air pollutants that are harmful to human body. In particular, as the urban area gradually expands, the odor generated as the environmental infrastructure approaches the residential area causes secondary pollution, and the main odorous substances in neighboring areas are reported as hydrogen sulfide and ammonia. In addition, the harmful gas present during the semiconductor process is problematic in the process, it is necessary to remove the harmful gas.

악취를 방지하는 방법으로는 크게 두 가지로 구분할 수 있는데 첫 번째는 농도를 감소시켜 악취를 약하게 하여 처리하는 방법과 두 번째는 악취를 만들어내는 물질을 변화시켜 불쾌감을 느끼지 않는 냄새로 만드는 방법이 있다. 첫 번째 방법에는 악취를 배출원에서부터 감소하는 방법으로 연소, 흡착, 흡수 기술을 이용하여악취물질을 제거하거나 대량의 공기를 이용하여 악취를 희석하는 방법이 있다. 이러한 방법중에서도 흡착법은 유지관리가 쉽고 광범위한 가스를 흡착 제거할 수 있으므로 널리 이용되고 있다.There are two ways to prevent odors. The first method is to reduce the concentration to weaken the odor, and the second is to change the substance that produces the odor to make the smell unpleasant. . The first method is to reduce odor from the source, by removing the odor substance using combustion, adsorption, and absorption techniques or by diluting the odor using a large amount of air. Among these methods, the adsorption method is widely used because it is easy to maintain and can adsorb and remove a wide range of gases.

흡착제를 이용한 흡착은 흡착제의 표면과 흡착질이 물리적 또는 화학적인 인력에 의하여 결합하는 현상으로 혼합된 흡착질에서 일정 성분을 선택적으로 분리 또는 정제하는데 이용되는 기술로서 대기 및 수질오염물질의 제거, 휘발성 용제의 회수, 혼합물의 분리 및 정제 등에 광범위하게 이용되고 있다.Adsorption using adsorbents is a phenomenon in which the surface of adsorbent and adsorbate are bonded by physical or chemical attraction, which is used to selectively separate or purify certain components from mixed adsorbate, remove air and water pollutants, and remove volatile solvent. It is widely used for recovery, separation and purification of mixtures.

습식 처리법은 배기가스와 세척액이 충전탑에서 서로 향류 방향으로 흐르면서 기-액 접촉을 통하여 유독가스를 중화시키거나 흡수 처리하는 방법이다. 여기서 세척액은 일반적으로 NaOH 와 같은 염기성 수용액이다. 이러한 습식 처리방법은 배기가스 처리 장치가 반응 생성물로 막히게 되거나 가스 제거 효율이 급격히 떨어지는 문제점을 안고 있다.The wet treatment is a method of neutralizing or absorbing toxic gases through gas-liquid contact while exhaust gas and washing liquid flow in the countercurrent direction in the packed column. The wash solution here is generally a basic aqueous solution such as NaOH. This wet treatment method has a problem that the exhaust gas treatment apparatus is blocked by the reaction product or the gas removal efficiency is sharply reduced.

건식 처리법은 유독가스를 고온으로 열분해하는 방법과 흡착제를 이용하여 흡착 제거하는 방법으로 구분된다. 흡착제를 이용한 흡착식 가스 스크러버에는 유독성 가스를 제거하기 위하여 흡착제를 가스 스크러버 캐니스터에 충전한다. 흡착제로는 일반적으로 활성탄[일본특허번호 61-35849(1986)]과 NaOH, Ca(OH)2, Mg(OH)2와 같은 염기성물질[일본특허번호 61-61619(1986)]을 사용하고, 활성탄과 염기성 물질을 혼합하여 사용하는 경우도 있다[미국특허번호 5322674(1994)]. 또한 본 발명자가 발명한 방사성 유기요오드를 제거하기 위한 TEDA/KI 첨착활성탄 제조방법[한국특허번호 72819(1994)]과 황화수소 제거용으로 개발한 KI를 첨착한 활성탄[한국특허번호 216985(1999)]이 흡착제로 사용되어지고 있다.Dry treatment is classified into a method of pyrolyzing toxic gas at a high temperature and a method of adsorption and removal using an adsorbent. The adsorbent gas scrubber using an adsorbent is filled with a gas scrubber canister to remove toxic gases. As the adsorbent, generally, activated carbon [Japanese Patent No. 61-35849 (1986)] and basic substances such as NaOH, Ca (OH) 2 and Mg (OH) 2 are used (Japanese Patent No. 61-61619 (1986)). In some cases, a mixture of activated carbon and a basic substance is used (US Pat. No. 5322674 (1994)). In addition, TEDA / KI impregnated activated carbon manufacturing method for removing radioactive organic iodine invented by the inventor [Korean Patent No. 72819 (1994)] and activated carbon impregnated with KI developed for removing hydrogen sulfide [Korean Patent No. 216985 (1999)]. It is used as this adsorbent.

흡착식에 사용되고 있는 황산이나, 인산이 첨착된 염기성 가스용 첨착활성탄은 암모니아 또는 아민같은 기체를 흡착하는데 이용되고, 가성소다나 탄산나트륨이 첨착된 산성가스용 첨착활성탄은 황화수소 등 산성가스를 흡착하는데 이용되고 있으나 흡착식에 사용되고 있는 첨착활성탄은 상온에서 흡착이 유리한 반면에 고온에서 사용할 경우 발화가 되어 화재의 위험성이 존재할 뿐만 아니라, 흡착열에 의해 발화가 일어날 수 있는 단점을 가지고 있다.The impregnated activated carbon for sulfuric acid or basic gas impregnated with phosphoric acid used for adsorption is used to adsorb gas such as ammonia or amine, and the impregnated activated carbon for acid gas impregnated with caustic soda or sodium carbonate is used to adsorb acid gas such as hydrogen sulfide. However, the impregnated activated carbon used in the adsorption is advantageous in adsorption at room temperature, but when used at a high temperature, it is ignited, there is a risk of fire, and has the disadvantage of ignition by heat of adsorption.

본 발명은 기존의 활성탄 또는 첨착활성탄을 사용하는 방법보다 무기흡착제에 금속염을 첨착시킨 흡착제가 유해가스의 흡착성능이 수배 이상 뛰어나 흡착탑의 운전성능을 향상시킬 수 있을 뿐만 아니라 무기흡착제를 담체로 사용하기 때문에 발화가 일어나지 않아 화재의 위험성이 없으므로 무기흡착제에 금속염을 첨착하여 유해가스의 흡착성능을 향상시키는 방법을 제공함에 있다.According to the present invention, the adsorbent in which a metal salt is impregnated with an inorganic adsorbent is more than several times better than the conventional method using activated carbon or impregnated activated carbon, thereby improving the operating performance of the adsorption tower as well as using the inorganic adsorbent as a carrier. Therefore, there is no risk of fire because ignition does not occur, thereby providing a method of improving the adsorption performance of harmful gases by attaching a metal salt to the inorganic adsorbent.

산업화와 더불어 대기 배출오염원과 그 종류가 다양해지고 있어 점차 인체에 유해한 대기 오염물질에 대한 효율적인 처리기술의 개발이 요구되고 있고, 특히 반도체 공정 중에서 문제가 되는 유해가스를 제거하기 위한 흡착제로 보다 우수한 특성을 보유하는 제품이 요구되므로 본 발명에서는 첨착활성탄 보다는 운전 효율성이 우수한 무기흡착제에 금속염을 첨착하여 흡착제를 제조하는 것으로 이하 본 발명의 바람직한 실시 예를 흡착성능검사 결과와 연계하여 설명하면 다음과 같다.With the industrialization and the diversification of air pollutants and their types, it is required to develop efficient treatment technology for air pollutants that are harmful to human body.In particular, it is an excellent adsorbent for removing harmful gases that are problematic in semiconductor processes. In order to produce an adsorbent by adhering a metal salt to an inorganic adsorbent having a higher operating efficiency than an impregnated activated carbon, the present invention is described below in connection with an adsorption performance test result.

실시예 1Example 1

무기흡착제의 수분을 제거하기 위하여 130℃의 오븐에서 3시간 이상 건조시킨 후 데시게이터에 보관한다. 증류수에 첨착용 시약 CuSO4를 넣고 용해시킨 후, 무기흡착제를 첨착용액이 들어있는 비이커에 넣고 1 시간동안 함침시킨다. 함침이 끝난 흡착제는 90℃의 오븐에서 2시간 건조 후 110℃의 오븐에서 12시간이상 마무리 건조한다. 건조가 끝난 흡착제(KSAC-01)는 데시게이터에 보관한다. 첨착이 끝난 후에는 초기 흡착제의 무게와 첨착 후 흡착제의 무게비로서 흡착제의 첨착율을 계산한다.In order to remove moisture of the inorganic adsorbent, it is dried in an oven at 130 ° C. for at least 3 hours and stored in a desiccator. After dissolving the impregnated reagent CuSO 4 in distilled water, the inorganic adsorbent was placed in a beaker containing the impregnated solution and impregnated for 1 hour. The impregnated adsorbent is dried in an oven at 90 ° C. for 2 hours and then dried in an oven at 110 ° C. for at least 12 hours. The dried adsorbent (KSAC-01) is stored in a desiccator. After the deposition, the adhesion ratio of the adsorbent is calculated as the ratio of the weight of the initial adsorbent to the weight of the adsorbent after the deposition.

첨착 무기흡착제의 암모니아의 흡착성능을 확인하기 위하여 고정층 칼럼에 충전시킨 후 흡착온도와 유속을 일정하게 유지시킨 후 고순도의 암모니아 가스를 공급하여 파과곡선과 흡착성능을 측정하였다. 암모니아 가스에 대한 실험조건은 표 1에 나타내었다. 암모니아 가스의 분석은 검지관을 이용하여 분석하였다. 또한 흡착제의 흡착성능을 첨착함량의 변화에 따라 첨착율을 10%, 30%, 50%로 달리하여 흡착성능시험을 확인하였다.In order to confirm the adsorption performance of the ammonia adsorbent of the impregnated inorganic adsorbent, the adsorption temperature and the flow rate were kept constant, and then the breakthrough curve and the adsorption performance were measured by supplying high-purity ammonia gas. The experimental conditions for ammonia gas are shown in Table 1. The analysis of ammonia gas was analyzed using a detection tube. In addition, the adsorption performance of the adsorbent was changed by the deposition rate of 10%, 30%, 50% according to the change of the deposition content was confirmed the adsorption performance test.

표 1 암모니아 흡착성능시험 조건Table 1 Ammonia adsorption performance test conditions

Column dia(mm)Column dia (mm) 1818 Flow rate(L/min)Flow rate (L / min) 55 Input conc.(ppm)Input conc. (Ppm) 300300 Sample weight(g)Sample weight (g) 55

무기흡착제에서 첨착율 변화에 따른 암모니아의 흡착성능시험과 기존의 첨착활성탄과 흡착성능을 비교한 그림 1에 나타내었다. 그림 1 에서 보는 바와 같이 암모니아 흡착량은 첨착활성탄에 비해 약 3배정도 증가되었고, Cu 첨착량이 증가함에 따라 흡착성능이 증가하였다. Cu의 양을 50% 이상을 할 경우 용액에 Cu를 용해시키기가 어렵고, 작업이 용이하지가 않으므로 그 이상의 첨착량을 사용하는 것은 바람직하지 않다. 그림 2의 결과에 의하면 무기흡착제 1L에 암모니아 가스가 100L 이상 흡착되는 것을 알수 있어 첨착무기흡착제의 흡착효율성이 주목된다.The adsorption performance test of ammonia according to the deposition rate of inorganic adsorbent and the adsorption performance of conventional impregnated activated carbon are shown in Fig. 1. As shown in Fig. 1, the amount of ammonia adsorption increased about three times compared to the impregnated activated carbon, and the adsorption performance increased as the amount of Cu impregnation increased. When the amount of Cu is 50% or more, it is difficult to dissolve Cu in the solution and the operation is not easy. Therefore, it is not preferable to use more deposition amount. According to the results of Figure 2, it can be seen that more than 100L of ammonia gas is adsorbed on 1L of inorganic adsorbent, so that the adsorption efficiency of the impregnated inorganic adsorbent is noted.

실시예 2Example 2

실시예 1과 같이 무기흡착제의 수분을 제거하고, 첨착용 시약 KMnO4를 용해하여 첨착무기 흡착제를 제조하였다.As in Example 1, the moisture of the inorganic adsorbent was removed, and the impregnated reagent KMnO 4 was dissolved to prepare an impregnated inorganic adsorbent.

반도체에서 자주 사용되는 TEOS와 SiH4가스에 대한 첨착무기흡착제의 흡착성능의 실험조건을 표 2에 나타내었다. 실험방법으로는 첨착 무기흡착제(KSAK-02,KSAK-03)의 TEOS와 SiH4의 흡착성능을 확인하기 위하여 고정층 칼럼에 충전시킨 후 흡착온도와 유속을 일정하게 유지시킨 후 TEOS, SiH4를 공급하여 파과곡선을 측정하였다(그림 2, 그림 3). TEOS의 분석은 검지관을 이용하여 분석하였고, SiH4의 검지방법은 Chemkey(model : TLD-1)를 이용하여 분석하였다.Table 2 shows the experimental conditions of the adsorption performance of the impregnated inorganic adsorbent on TEOS and SiH 4 gas which are frequently used in semiconductors. In order to confirm the adsorption performance of TEOS and SiH 4 of the impregnated inorganic adsorbents (KSAK-02, KSAK-03), the adsorption temperature and the flow rate were kept constant, and then TEOS and SiH 4 were supplied. The breakthrough curve was measured (Fig. 2, Fig. 3). The analysis of TEOS was carried out using a detector tube, and the detection method of SiH 4 was analyzed using Chemkey (model: TLD-1).

표 2 흡착성능시험 조건Table 2 Adsorption Performance Test Conditions

구분division TEOSTEOS SiH4 SiH 4 Column dia(mm)Column dia (mm) 1818 1818 Flow rate(L/min)Flow rate (L / min) 55 55 Input conc.(ppm)Input conc. (Ppm) -- 167167 Sample weight(g)Sample weight (g) 2525 55

TEOS에 대한 흡착시험은 첨착무기흡착제와 다른 흡착제(K-약재)를 비교하였다. 그림 2에서 보는 바와 같이 첨착무기흡착제가 K-약재에 비해 15배 이상 우수한 흡착성능을 보이고 있다. 또한 첨착무기흡착제를 대기중에서 3일간 방치한 후 TEOS 흡착성능을 측정한 결과를 보면 흡착성능이 거의 비슷한 결과를 나타내고 있다. 그림 3는 SiH4에 대한 흡착성능 시험 결과를 나타낸 것이다. 첨착무기흡착제가 SiH4에 대해서도 다른 흡착제(N-약재)에 비해 우수한 흡착성능 보이고 있는 것을 볼 수 있다. 흡착제에 대한 SiH4의 흡착량은 흡착제 1L에 대해 약 38L의 SiH4을 흡착할 수 있다.Adsorption tests on TEOS compared the impregnated inorganic adsorbents with other adsorbents (K-medicinal agents). As shown in Figure 2, the impregnated inorganic adsorbent shows more than 15 times better adsorption performance than K-medicinal agent. In addition, the results of measuring the adsorption performance of TEOS after leaving the impregnated inorganic adsorbent in the air for 3 days showed almost similar results. Figure 3 shows the adsorption performance test results for SiH 4 . It can be seen that the impregnated inorganic adsorbent shows superior adsorption performance with respect to SiH 4 as compared with other adsorbents (N-medicinal agents). The adsorption amount of SiH 4 for the adsorbent can adsorb the SiH 4 to approximately 38L for the adsorbent 1L.

본 발명은 기존에 사용하고 있는 첨착활성탄에 비해 흡착성능이 우수한 흡착제를 사용하므로 장기간 사용이 가능하므로 흡착제의 교체 주기를 연장하여 폐 흡착제의 발생으로 인한 폐기물의 양을 감소할 수 있을 뿐만 아니라 첨착활성탄은 화재의 위험성이 존재하고 있는데 무기흡착제는 발화가 일어나지 않아 화재의 위험성이 없다. 또한 첨착활성탄에 비해 흡착성능이 우수한 무기흡착제를 사용하여 유해가스에 의한 대기오염을 억제할 수 있다.Since the present invention uses an adsorbent that has superior adsorption performance compared to the conventionally used impregnated activated carbon, it can be used for a long time, so that the replacement cycle of the adsorbent can be extended to reduce the amount of waste due to the generation of waste adsorbent as well as the impregnated activated carbon. Has the danger of fire. Inorganic adsorbents do not ignite, so there is no risk of fire. In addition, by using an inorganic adsorbent having excellent adsorption performance compared to impregnated activated carbon, it is possible to suppress air pollution by harmful gases.

본 발명은 상술한 특정의 바람직한 실시 예에 한정되지 아니하며, 청구범위에서 청구하는 본 발명의 요지를 벗어남이 없이 당해 발명이 속하는 기술분야에서 통상의 지식을 가진 자라면 누구든지 다양한 변형 실시가 가능한 것은 물론이고, 그와 같은 변경은 청구범위 기재의 범위 내에 있게 된다.The present invention is not limited to the above-described specific preferred embodiments, and various modifications can be made by those skilled in the art without departing from the gist of the present invention as claimed in the claims. Of course, such changes will fall within the scope of the claims.

Claims (3)

무기흡착제에 금속염을 첨착하여 유해가스를 제거하는 방법How to remove harmful gas by attaching metal salt to inorganic adsorbent 제 1 항에 있어서,The method of claim 1, 무기흡착제에 Cu 첨착율을 10-50%로 유지하여 첨착 무기흡착제를 제조하는 방법Method for preparing an impregnated inorganic adsorbent by maintaining Cu deposition rate in the inorganic adsorbent at 10-50% 제 1 항에 있어서,The method of claim 1, TEOS 또는 SiH4를 제거하기 위한 흡착제 제조에서 무기흡착제에 K, Mn을 첨착하는 방법Method of attaching K and Mn to inorganic adsorbents in the preparation of adsorbents for removing TEOS or SiH 4
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KR970064708A (en) * 1996-03-07 1997-10-13 가나이 쯔도무 Deodorant adsorbent and odor removal method using the same
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JPS553871A (en) * 1978-06-27 1980-01-11 Toho Rayon Co Ltd Adsorbent for removal of poisonous gas containing sulfur
JPS60235637A (en) * 1984-05-09 1985-11-22 Nippon Kasei Kk Adsorbent for gas
KR870010891A (en) * 1986-05-22 1987-12-18 이. 유진 인니스 Screening Adsorption Process by Zeolite
KR970064708A (en) * 1996-03-07 1997-10-13 가나이 쯔도무 Deodorant adsorbent and odor removal method using the same
KR20010000418A (en) * 2000-09-27 2001-01-05 김대승 Adsorption and deodorizing catalyst of malodors and a preparing method of the catalyst

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* Cited by examiner, † Cited by third party
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KR100522570B1 (en) * 2002-12-05 2005-10-19 이후근 A portable air cleaner purifying the contamination air

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