KR100356611B1 - Purification Method and Apparatus for Nitrogen - Google Patents
Purification Method and Apparatus for Nitrogen Download PDFInfo
- Publication number
- KR100356611B1 KR100356611B1 KR1020000046417A KR20000046417A KR100356611B1 KR 100356611 B1 KR100356611 B1 KR 100356611B1 KR 1020000046417 A KR1020000046417 A KR 1020000046417A KR 20000046417 A KR20000046417 A KR 20000046417A KR 100356611 B1 KR100356611 B1 KR 100356611B1
- Authority
- KR
- South Korea
- Prior art keywords
- nitrogen
- column
- getter
- methane
- purification
- Prior art date
Links
Classifications
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
- B01J23/44—Palladium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/04—Purification or separation of nitrogen
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B21/00—Nitrogen; Compounds thereof
- C01B21/04—Purification or separation of nitrogen
- C01B21/0405—Purification or separation processes
- C01B21/0494—Combined chemical and physical processing
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2210/00—Purification or separation of specific gases
- C01B2210/0001—Separation or purification processing
- C01B2210/0003—Chemical processing
- C01B2210/0006—Chemical processing by reduction
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2210/00—Purification or separation of specific gases
- C01B2210/0001—Separation or purification processing
- C01B2210/0009—Physical processing
- C01B2210/0014—Physical processing by adsorption in solids
- C01B2210/0023—Physical processing by adsorption in solids in getters
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02C—CAPTURE, STORAGE, SEQUESTRATION OR DISPOSAL OF GREENHOUSE GASES [GHG]
- Y02C20/00—Capture or disposal of greenhouse gases
- Y02C20/20—Capture or disposal of greenhouse gases of methane
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/151—Reduction of greenhouse gas [GHG] emissions, e.g. CO2
Abstract
본 발명은 질소 정제방법 및 질소 정제장치에 관한 것이다.The present invention relates to a nitrogen purifying method and a nitrogen purifying apparatus.
본 발명의 질소 정제 방법은 Zr-V-Fe, Zr-Fe, Zr을 주성분으로 하는 게터 합금을 200-450℃ 온도에서 외부대기와 차단 혹은 고진공 상태에서 질소와 반응시켜 정제칼럼의 하부(2중 칼럼의 경우 하부의 칼럼)에 충진하고 상부에 Pd/Al2O3촉매를 충진 후(2중 칼럼의 경우 상부의 칼럼) 200-450℃ 온도에서 정제하고자 하는 질소스트림 중의 메탄성분을 산화시킨후 (필요시 메탄과 같은 당량의 산소공급필요) 상기 질소화된 게터에서 물, 이산화탄소, 일산화탄소, 산소등의 불순물을 제거하는 것으로 구성된다.In the nitrogen purification method of the present invention, a getter alloy containing Zr-V-Fe, Zr-Fe, and Zr as a main component is reacted with nitrogen in an external atmosphere at a temperature of 200-450 ° C. or in a high vacuum state, so that the lower part of the purification column After the column is filled with the bottom column) and the Pd / Al 2 O 3 catalyst at the top (column at the top of the double column), the methane component in the nitrogen stream to be purified at 200-450 ° C. is oxidized. It is necessary to supply oxygen, such as methane if necessary. The nitrogenated getter consists of removing impurities such as water, carbon dioxide, carbon monoxide and oxygen.
본 발명의 질소 정제장치는 Zr-V-Fe, Zr-Fe, Zr을 주성분으로 하는 게터 합금을 200-450℃ 온도에서 외부대기와 차단 혹은 고진공 상태에서 질소와 반응한 합금을 정제 칼럼하부에 Pd/Al2O3촉매를 상부에 충진하여 칼럼을 설치한 것 혹은 2개의 별도의 칼럼을 구성후 상부 칼럼에는 Pd/Al2O3를 충진하고 연결되는 하부 칼럼에는 질소화된 게터 합금을 충진한 것을 특징으로 한다.The nitrogen purifying apparatus according to the present invention has a getter alloy containing Zr-V-Fe, Zr-Fe, and Zr as a main component at a temperature of 200-450 ° C. with an external atmosphere, or an alloy reacted with nitrogen in a high vacuum state at the bottom of the purification column. / Al 2 O 3 catalyst at the top of the column was installed or two separate columns after the top column was filled with Pd / Al 2 O 3 and the connected lower column was filled with the nitrogenized getter alloy It is characterized by.
Description
본 발명은 질소 정제 방법 및 정제 장치에 관한 것이다. 특히, 본 발명은 질소정제용 합금을 질소화시킨 게터를 사용하고, Pd/Al2O3촉매를 사용하여 메탄을 이산화탄소와 물로 산화시켜 기타의 불순물과 함께 상기 질소화된 게터로 흡착, 제거하는 것을 특징으로 한다.The present invention relates to a nitrogen purifying method and a purifying apparatus. In particular, the present invention uses a getter obtained by nitrifying an alloy for nitrogen purification, and oxidizing methane to carbon dioxide and water using a Pd / Al 2 O 3 catalyst to adsorb and remove the nitrogenized getter together with other impurities. It is characterized by.
질소는 전자산업, 화공업, 철강 및 조선업 등의 분야에서 점차 그 수요가 증가하고 있는 유용한 가스이다. 압축기를 사용해서 공기를 압축하고, 그 압축공기가 액화 가스가 될때까지 단열 팽창을 반복한 다음, 순소 높은 액화 질소를 만들기위해 고압 상태에서 분별 증류하는 방법은 공업과정에서 실시되고 있는 일반적인 질소 제조방법이다. 액화상태 또는 가스상태로 용기에 충전되어 시판되고 있다. 질소는 대표적인 불활성 가스이며 금속의 열처리 가공, 반도체 제조공정 등에서 대기 가스로서 상술한 여러 분야에서 널리 사용되고 있다. 특히, 전자산업등의 초정밀 미세가공에 사용되는 경우에는, 가공 공정에 들어가기 직전에 정제도를 높이기 위해 불순물을 제거하여 고순도를 확보할 것이 요구된다. 특히, 공업 생산공정에서 대량 사용하는 경우에는 액화 질소를 기화시켜 배관을 통해 공급한다. 이 때, 기화된 질소 중에 함유되는 산소, 일산화탄소, 이산화탄소, 수소, 탄화수소, 물 등의 불순물을 어떻게 신속, 확실하게 제거 하느냐는 문제에 직면하게 된다. 이중 탄화수소는 반도체중의 수율에 직접적인 영향을 미칠 정도로 필히 제거되어져야 할 성분이다.Nitrogen is a useful gas with increasing demand in the electronics, chemicals, steel and shipbuilding industries. Compressors are used to compress air, repeat adiabatic expansion until the compressed air is a liquefied gas, and fractional distillation under high pressure to produce purely high liquefied nitrogen. to be. It is filled with a container in a liquefied state or gaseous state and is commercially available. Nitrogen is a representative inert gas and is widely used in the above-mentioned fields as atmospheric gases in metal heat treatment processing, semiconductor manufacturing processes and the like. In particular, when used for ultra-precision micromachining, such as the electronics industry, it is required to secure high purity by removing impurities in order to increase the degree of purification immediately before entering the processing process. In particular, in the case of mass use in an industrial production process, liquefied nitrogen is vaporized and supplied through piping. At this time, there is a problem of how to quickly and reliably remove impurities such as oxygen, carbon monoxide, carbon dioxide, hydrogen, hydrocarbons and water contained in vaporized nitrogen. The double hydrocarbon is a component that must be removed to a degree that directly affects the yield in the semiconductor.
이러한 불순물을 제거하여, 질소를 고도로 정제하기 위하여 지금까지 각종의 질소 가스 정제 장치가 시판 되어 사용되고있다.Various nitrogen gas purification apparatuses have been commercially available and used so far to remove such impurities and to highly refine nitrogen.
시판되고 있는 가스 정제 장치에서는, 니켈, 크롬 및 동 등의 금속산화물의 산화 촉매를 이용하여 일산화탄소, 탄화수소, 수소 등을 산화하여 이산화탄소 및 물로 변화시킨 후 비석 활자체 (MOLECULAR SIEVE)나 활성탄 등을 사용하여 불순물을 흡착, 제거함으로써 가스의 정제가 행해졌다.Commercially available gas refiners use carbon monoxide, hydrocarbons, hydrogen, etc. to oxidize carbon monoxide, hydrocarbons, hydrogen, etc. using oxidation catalysts of metal oxides such as nickel, chromium, and copper, and then use MOLECULAR SIEVE or activated carbon. The gas was purified by adsorbing and removing impurities.
또 수소 흡착형 합금인 Ti-Mn계, Ti-Fe계, 회토류 -Ni계 합금 등도 사용되고 있으나, 정제 성능이 떨어지는 단점이 있었다.In addition, Ti-Mn-based, Ti-Fe-based, and rare earth-Ni-based alloys, which are hydrogen adsorption alloys, are also used, but have a disadvantage of poor refining performance.
미국 특허 제4,306,887호에는 15-30중량%의 철과, 70-85%중량%의 지르코늄으로 된, 질소를 흡착하지 않고 다른 불순물을 선택적으로 흡착하는 철-지르코늄 게터 합금을 게시하고 있다.U.S. Patent 4,306,887 discloses an iron-zirconium getter alloy of 15-30% by weight of iron and 70-85% by weight of zirconium, which selectively adsorbs other impurities without adsorbing nitrogen.
본 발명의 발명자는 상기 미국특허의 게터 함금을 가공하여 질소 가스의 정제능을 향상시고자 노력한 결과 본 발명을 완성하였다.The inventor of the present invention has completed the present invention as a result of trying to improve the purifying ability of nitrogen gas by processing the getter alloy of the US patent.
따라서, 본 발명의 목적은 메탄, 일산화탄소, 이산화탄소 등의 불순물을 동시에 제거할 수 있는 질소 정제방법 및 정제장치를 제공하는 것이다.Accordingly, it is an object of the present invention to provide a nitrogen purifying method and a purifying apparatus capable of simultaneously removing impurities such as methane, carbon monoxide and carbon dioxide.
본 발명의 다른 목적은 종래의 게터 합금에 비해 개선된 정제능을 갖는 게터 합금의 가공방법을 제공하는 것이다.Another object of the present invention is to provide a method for processing a getter alloy having an improved refining capacity compared to a conventional getter alloy.
도 1은 본 발명의 질소 정제 장치로 처리하기 전의 질소 가스를 분석한 가스 크로마토그램.BRIEF DESCRIPTION OF THE DRAWINGS Fig. 1 is a gas chromatogram analyzing nitrogen gas before treatment with a nitrogen purifying apparatus of the present invention.
도 2는 본 발명의 질소 정제 장치로 처리한 후의 질소 가스를 분석한 가스 크로마토그램.2 is a gas chromatogram analyzing the nitrogen gas after treatment with the nitrogen purifying apparatus of the present invention.
상기 본 발명의 목적은 Zr-V-Fe, Zr-Fe, Zr을 주성분으로 하는 게터 합금을 200-450℃ 온도에서 외부대기와 차단 혹은 고진공 상태에서 질소와 반응시켜 정제칼럼의 하부(2중 칼럼의 경우 하부의 칼럼)에 충진하고 상부에 Pd/Al2O3촉매를 충진 후(2중 칼럼의 경우 상부의 칼럼) 200-450℃ 온도에서 정제하고자 하는 질소스트림 중의 메탄성분을 산화시킨후 (필요시 메탄과 같은 당량의 산소공급필요) 상기 질소화된 게터에서 물, 이산화탄소, 일산화탄소, 산소등의 불순물을 제거하는 것으로 구성되는 질소 정제방법에 의해 달성된다.An object of the present invention is a lower (double column) of a purified column by reacting a getter alloy mainly composed of Zr-V-Fe, Zr-Fe, Zr with external air at a temperature of 200-450 ° C. or with nitrogen in a high vacuum state. In the bottom column) and Pd / Al 2 O 3 catalyst at the top (column at the top in the case of a double column) after oxidation of the methane component in the nitrogen stream to be purified at 200-450 ° C ( If necessary, the supply of oxygen equivalent to methane) is achieved by a nitrogen purification method consisting of removing impurities such as water, carbon dioxide, carbon monoxide and oxygen from the nitrogenized getter.
본 발명은 목적은 또한, Zr-V-Fe, Zr-Fe, Zr을 주성분으로 하는 게터 합금을 200-450℃ 온도에서 외부대기와 차단 혹은 고진공 상태에서 질소와 반응한 합금을정제 칼럼하부에 Pd/Al2O3촉매를 상부에 충진하여 칼럼을 설치한 것 혹은 2개의 별도의 칼럼을 구성후 상부 칼럼에는 Pd/Al2O3를 충진하고 연결되는 하부 칼럼에는 질소화된 게터 합금을 충진한 것을 특징으로 하는 질소 정제 장치에 의해 달성된다.It is also an object of the present invention to provide a Pd-containing alloy obtained by reacting a getter alloy mainly composed of Zr-V-Fe, Zr-Fe, Zr with external atmosphere at 200-450 ° C or reacting with nitrogen in a high vacuum state. / Al 2 O 3 catalyst at the top of the column was installed or two separate columns after the top column was filled with Pd / Al 2 O 3 and the connected lower column was filled with the nitrogenized getter alloy It is achieved by a nitrogen purifier characterized in that.
이하 본 발명을 보다 상세하게 설명한다.Hereinafter, the present invention will be described in more detail.
질소 정제용 Zr-V-Fe, Zr-Fe, Zr을 주성분으로 하는 게터를 상온에서 용기에 넣는다. 용기는, 질소 가스가 접촉하게 되는 장치의 내벽 주분은 가스 흡착이 최소화 되도록 표면이 치밀하고 매끄럽게 연마된 금속으로 만들며 부식에 의해서 분말이 생기는 일이 없는 것이 좋다. 그러한 금속재료의 예로 스테인레스 강과 하스텔로이(HASTELL0Y), 인코로이(INCOLOY) 및 모넬 금속(MONEL METAL)등을 들수 있으나, 이것들에 한정되는 것은 아니며, 상기의 조건에 적합한 금속재료이면 그밖의 것도 적절히 선택, 사용할 수 있다.A getter mainly containing nitrogen purifying Zr-V-Fe, Zr-Fe and Zr is placed in a container at room temperature. The container is preferably made of metal whose surface is dense and smoothly polished to minimize gas adsorption, and that powder is not formed by corrosion. Examples of such metal materials include stainless steel, HASTELL0Y, INCOLOY, and MONEL METAL. However, the metal materials are not limited to these, and other metals suitable for the above conditions may be appropriately selected. , Can be used.
200-450℃로 가열한 다음, 그 온도를 유지하면서 시판용 순도(99.9999%이상)의 질소 기체를 용기에 도입시킨다. 이 질소 가스 도입은 0.1 내지 10 절대 압력 범위의 편리한 압력으로 수행한다. 반응은 외부대기와 차단 혹은 고진공 상태에서행해진다. 질소가 흡수됨에 따라 합금이 질소화되어 황금색으로 변색하게 된다. 반응이 완료되면, 질소 반응 용기중에 남아 있는 기체를 간단하게 펌핑시키거나 퍼어징시켜 제거할 수 있다.After heating to 200-450 ° C., nitrogen gas of commercial purity (99.9999% or more) is introduced into the vessel while maintaining the temperature. This nitrogen gas introduction is carried out at a convenient pressure in the range of 0.1 to 10 absolute pressures. The reaction takes place in external atmosphere or in a high vacuum. As nitrogen is absorbed, the alloy becomes nitrogenous and discolors to golden. Once the reaction is complete, the gas remaining in the nitrogen reaction vessel can be removed by simply pumping or purging.
정제칼럼의 하부(2중 칼럼의 경우 하부의 칼럼)에 상기 공정에 의해 질소화된 게터를 충진하고 상부에 Pd/Al2O3촉매를 충진 후(2중 칼럼의 경우 상부의 칼럼)200-450℃ 온도에서 정제하고자 하는 질소스트림 중의 메탄성분을 산화시킨다. 사용되는 촉매의 양은 정제되는 질소 스트리임에 포함되는 메탄의 함량에 따라 달라질 수 있으며, 게터 합금 중량에 대해 0.001-10중량%의 양으로 사용한다. 메탄의 함량이 높은 경우, 필요에 따라 메탄과 같은 당량의 산소를 공급할 수 있다. 메탄은 산화되어 이산화탄소와 물로 분해된다. 산화된 이산화탄소와 물, 그리고 불순물로 함유된 일산화탄소와 산소 등은 하부에 설치된 게터에 의해 흡착, 제거된다.After filling the lower part of the purification column (the lower column in the case of a double column) with the nitrogenized getter and the Pd / Al 2 O 3 catalyst in the upper part (the upper column in the case of a double column) The methane component in the nitrogen stream to be purified is oxidized at 450 ° C. The amount of catalyst used may vary depending on the amount of methane included in the nitrogen stream being purified and is used in an amount of 0.001-10% by weight relative to the getter alloy weight. If the content of methane is high, it is possible to supply the same amount of oxygen as methane if necessary. Methane is oxidized and broken down into carbon dioxide and water. Oxidized carbon dioxide and water, and carbon monoxide and oxygen contained as impurities are adsorbed and removed by a getter installed at the bottom.
기존의 질소화된 게터를 사용했을 경우는 정제하고자하는 질소 스트림중 메탄 및 하이드로 카본류 등은 제거가 불가능 하였으나 본 발명에서처럼 상부에는 Pd/Al2O3하부에는 질소화된 게터를 연결하여 200-450도 범위에서 사용하면 질소스트림중의 메탄,물,산소,일산화탄소,이산화탄소등의 불순물을 제거할 수 있다.In the case of using a conventional nitrogenated getter, it was impossible to remove methane and hydrocarbons from the nitrogen stream to be purified, but as in the present invention, the upper part of the Pd / Al 2 O 3 was connected to a nitrogenized getter 200- When used in the 450 degree range, impurities such as methane, water, oxygen, carbon monoxide and carbon dioxide in the nitrogen stream can be removed.
이하 실시예룰 통해 본 발명을 보다 상세하게 설명한다.Hereinafter, the present invention will be described in more detail with reference to the following examples.
실시예 1Example 1
이탈리아공화국 밀라노 소재의 사에즈 게터스사(SAES Getters S.P.A.)에서 제조 판매하고 있는 22-25% 중량비의 철과 75-78%의 지르코늄을 합금한 게터로서, 3㎜의 직경과 4㎜의 높이로 이루어진 주상소립체(柱狀小粒體) 형태의 Zr-Fe 게터 400g을 총 약 1ℓ 유리 용적 및 압력 측정 변환기와 상호 교환된 소형 가압 용기에 놓았다. 진공 펌프를 사용하여 공기를 25밀리-토르 미만으로 배기시키고, 진공 펌프의 밸브를 빼고, 약 1300토르 절대압으로 질소를 첨가한 시간에 대한 함수로서 압력 변화를 기록하여 질소 흡수를 관찰하였다. 반응이 완결된 후, 공기 안정화반응을 수행하였다.A getter made of 22-25% by weight iron and 75-78% zirconium, manufactured by SAES Getters SPA, Milan, Italy, with a diameter of 3 mm and a height of 4 mm. 400 g of Zr-Fe getter in the form of columnar particles were placed in a small pressurized container interchanged with a total of about 1 liter glass volume and pressure measuring transducer. Nitrogen absorption was observed by evacuating air to less than 25 milli-Tor using a vacuum pump, removing the valve from the vacuum pump, and recording the pressure change as a function of the time of adding nitrogen at about 1300 Torr absolute pressure. After the reaction was completed, air stabilization was performed.
게터를 정제기 칼럼에 하부에 장착하고 상부에는 Pd/Al2O3촉매를 충진 하였다. 235.5ppm의 일산화탄소, 195.9ppm의 이산화탄소, 218.8의 메탄을 불순물로 포함하는 질소 가스의 정제를 400℃에서 시행하였다. 불순물이 포함된 질소 가스는 섭씨 25도의 온도와 6kg/cm2의 압력(게이지) 및 0.17ℓ/min. 유속으로 정제기로 도입된다. 질소 가스는 섭씨 400도로 유지된 게터층을 통과해서 배기구로부터 41kg/㎠(게이지)의 압력으로 배기되는데, 불순물에 대한 준위가 질소 가스가 관류하기 시작한지 40분 후에 여러가지 가스에 대해서 측정한다. 정제 전후의 데이타를 도 1 및 도 2에 표시하였다.The getter was mounted on the bottom of the purifier column and the top was filled with Pd / Al 2 O 3 catalyst. Purification of nitrogen gas containing 235.5 ppm carbon monoxide, 195.9 ppm carbon dioxide, and 218.8 methane as impurities was carried out at 400 ° C. Nitrogen gas with impurities contains a temperature of 25 degrees Celsius, a pressure (gauge) of 6 kg / cm2, and 0.17 l / min. It is introduced into the purifier at a flow rate. Nitrogen gas passes through a getter layer maintained at 400 degrees Celsius and is exhausted at a pressure of 41 kg / cm 2 (gauge) from the exhaust port. The level of impurities is measured for various gases 40 minutes after nitrogen gas starts to flow through. Data before and after purification are shown in FIGS. 1 and 2.
분석조건은 다음과 같았다.The analysis conditions were as follows.
분석기(GC): HP-5890 Series IIAnalyzer (GC): HP-5890 Series II
검출기 : FID(Methanizer)Detector: FID (Methanizer)
칼럼 : Porapak QColumn: Porapak Q
오븐 온도 : 35℃ 등온Oven Temperature: 35 ℃ Isothermal
검출 온도 : 250℃Detection temperature: 250 ℃
주입 A 온도 : 50℃Injection A temperature: 50 ℃
주입 B 온도 : 375℃Injection B Temperature: 375 ℃
캐리어 : He 20㎖/분Carrier: He 20ml / min
상기 본 발명의 실시예 및 도면에서 알 수 있는 바와 같이, 본 발명에 의해 제조된 게터 합금은 우수한 정제능을 나타낸다. 일산화탄소 가스, 이산화탄소 가스 그리고 메탄 가스를 거의 완전하게 제거하였다.As can be seen from the examples and drawings of the present invention, the getter alloy produced by the present invention shows excellent refining capacity. Carbon monoxide gas, carbon dioxide gas and methane gas were almost completely removed.
Claims (3)
Priority Applications (4)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020000046417A KR100356611B1 (en) | 2000-08-10 | 2000-08-10 | Purification Method and Apparatus for Nitrogen |
| TW089125007A TW539644B (en) | 2000-08-10 | 2000-11-24 | Apparatus and method for purifying nitrogen |
| JP2000370234A JP2002060209A (en) | 2000-08-10 | 2000-12-05 | Method and device for purifying nitrogen |
| FR0015786A FR2812823A1 (en) | 2000-08-10 | 2000-12-06 | Purification of nitrogen comprises use of combination of methane oxidation catalyst and nitrogen-saturated zirconium getter alloy |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| KR1020000046417A KR100356611B1 (en) | 2000-08-10 | 2000-08-10 | Purification Method and Apparatus for Nitrogen |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| KR20020013059A KR20020013059A (en) | 2002-02-20 |
| KR100356611B1 true KR100356611B1 (en) | 2002-10-18 |
Family
ID=19682686
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| KR1020000046417A KR100356611B1 (en) | 2000-08-10 | 2000-08-10 | Purification Method and Apparatus for Nitrogen |
Country Status (4)
| Country | Link |
|---|---|
| JP (1) | JP2002060209A (en) |
| KR (1) | KR100356611B1 (en) |
| FR (1) | FR2812823A1 (en) |
| TW (1) | TW539644B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR102588567B1 (en) * | 2021-07-16 | 2023-10-16 | 주식회사 원익홀딩스 | METHOD OF REMOVING SURFACE IMPURITY OF Zr-BASED GETTER |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS623006A (en) * | 1985-06-28 | 1987-01-09 | 大陽酸素株式会社 | Nitrogen super purification facilities and purification process |
| IT1227219B (en) * | 1988-09-26 | 1991-03-27 | Getters Spa | APPARATUS AND RELATED METHOD TO REMOVE GASEOUS IMPURITIES FROM INERT GASES AND ENSURE EXTREMELY LOW HYDROGEN LEVELS |
| DE3926015A1 (en) * | 1989-08-05 | 1991-02-07 | Messer Griesheim Gmbh | METHOD FOR THE FINE PURIFICATION OF GASES |
-
2000
- 2000-08-10 KR KR1020000046417A patent/KR100356611B1/en active IP Right Grant
- 2000-11-24 TW TW089125007A patent/TW539644B/en not_active IP Right Cessation
- 2000-12-05 JP JP2000370234A patent/JP2002060209A/en active Pending
- 2000-12-06 FR FR0015786A patent/FR2812823A1/en not_active Withdrawn
Also Published As
| Publication number | Publication date |
|---|---|
| KR20020013059A (en) | 2002-02-20 |
| TW539644B (en) | 2003-07-01 |
| JP2002060209A (en) | 2002-02-26 |
| FR2812823A1 (en) | 2002-02-15 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| US7862645B2 (en) | Removal of gaseous contaminants from argon | |
| Ichikawa et al. | Disproportionation of CO on small particles of silica-supported palladium | |
| Sircar et al. | Activated carbon for gas separation and storage | |
| US6361750B2 (en) | Systems for purification of boron trichloride | |
| US5685172A (en) | Process and device for the preparation of a flow which is substantially purified with respect to at least one of the impurities oxygen and carbon monoxide | |
| Ertl et al. | Interactions of nitrogen and hydrogen on iron surfaces | |
| US5492682A (en) | Hydrogen purification | |
| KR930006690B1 (en) | Superpurifier for nitrogen and process for purifying same | |
| JPH10507735A (en) | Method for removing oxygen from ammonia at room temperature | |
| JPH08332375A (en) | Adsorbent and method for removing trace of oxygen from inertgas | |
| US7666379B2 (en) | Process and apparatus for removing Bronsted acid impurities in binary halides | |
| Li et al. | Zeolite monoliths for air separation: Part 2: Oxygen enrichment, pressure drop and pressurization | |
| TW445170B (en) | Process for the removal of water from evacuated chambers or from gases | |
| KR20000062311A (en) | Method for purifying a cryogenic fluid by filtration and adsorption | |
| KR100356611B1 (en) | Purification Method and Apparatus for Nitrogen | |
| WO1997014648A1 (en) | Hydrogen purification using metal hydride getter material | |
| CN112569912A (en) | Flexible metal organic framework material and preparation method and application thereof | |
| US4859435A (en) | Deoxygenation of inert gas streams with methanol | |
| US6047561A (en) | Process and device for the production of ultra-pure inert gas | |
| US5737941A (en) | Method and apparatus for removing trace quantities of impurities from liquified bulk gases | |
| US5913893A (en) | Process for the purification of a cryogenic fluid by filtration and/or adsorption | |
| Golden et al. | Activated carbon adsorbent for PSA driers | |
| US6436352B1 (en) | Hydrogen purification | |
| JPS60241931A (en) | Adsorbent for pressure-variable separation by adsorption | |
| WO2022075351A1 (en) | Method for removing oxygen molecule and method for purifying carbon monoxide |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| A201 | Request for examination | ||
| E701 | Decision to grant or registration of patent right | ||
| GRNT | Written decision to grant | ||
| FPAY | Annual fee payment |
Payment date: 20120914 Year of fee payment: 11 |
|
| FPAY | Annual fee payment |
Payment date: 20130904 Year of fee payment: 12 |
|
| FPAY | Annual fee payment |
Payment date: 20140917 Year of fee payment: 13 |
|
| FPAY | Annual fee payment |
Payment date: 20150909 Year of fee payment: 14 |
|
| FPAY | Annual fee payment |
Payment date: 20160907 Year of fee payment: 15 |
|
| FPAY | Annual fee payment |
Payment date: 20170907 Year of fee payment: 16 |
|
| FPAY | Annual fee payment |
Payment date: 20190909 Year of fee payment: 18 |