JP2954364B2 - Purification method of nitrogen trifluoride gas - Google Patents
Purification method of nitrogen trifluoride gasInfo
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- JP2954364B2 JP2954364B2 JP40829390A JP40829390A JP2954364B2 JP 2954364 B2 JP2954364 B2 JP 2954364B2 JP 40829390 A JP40829390 A JP 40829390A JP 40829390 A JP40829390 A JP 40829390A JP 2954364 B2 JP2954364 B2 JP 2954364B2
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- gas
- temperature
- natural zeolite
- adsorption
- metal plate
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Description
【０００１】[0001]
【産業上の利用分野】本発明は三弗化窒素ガスの精製方
法に関する。更に詳しくは、三弗化窒素ガス中に含まれ
る亜酸化窒素（N2O)、二酸化炭素(CO2)及び二弗化二窒
素 (N2F2)を除去する方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for purifying nitrogen trifluoride gas. More specifically, the present invention relates to a method for removing nitrous oxide (N 2 O), carbon dioxide (CO 2 ), and dinitrogen difluoride (N 2 F 2 ) contained in nitrogen trifluoride gas.
【０００２】[0002]
【従来の技術】三弗化窒素（NF3)ガスは、半導体のドラ
イエッチング剤やCVD 装置のクリーニングガスとして近
年注目されているが、これらの用途に使用されるNF3 ガ
スは、高純度のものが要求されている。2. Description of the Related Art Nitrogen trifluoride (NF 3 ) gas has recently attracted attention as a dry etching agent for semiconductors and a cleaning gas for CVD equipment. However, NF 3 gas used in these applications has a high purity. Things are required.
【０００３】NF3 ガスは、種々の方法で製造されるが何
れの方法で得られたガスも殆どの場合、N2O 、CO2 、N2
F2などの不純物を比較的多量に含んでいるので、上記用
途としての高純度のNF3 ガスを得るためには精製が必要
である。NF3 ガス中のこれらの不純物を除去する精製方
法としては、天然ゼオライト、合成ゼオライト、活性
炭、活性アルミナ等の吸着剤を使用して、これらの不純
物を吸着除去する方法がよく知られている。[0003] NF 3 gas is produced by various methods, and the gas obtained by any of the methods is almost always N 2 O, CO 2 , N 2
Since it contains a relatively large amount of impurities such as F 2, purification is required to obtain high-purity NF 3 gas for the above-mentioned applications. As a purification method for removing these impurities in the NF 3 gas, a method of adsorbing and removing these impurities using an adsorbent such as natural zeolite, synthetic zeolite, activated carbon, and activated alumina is well known.
【０００４】特に天然ゼオライトは、上記不純物を効率
よく吸着するので、この点では一応好ましい吸着剤では
ある。天然ゼオライトは、通常円筒形の容器に充填 (吸
着塔) し、これにN2ガスなどの不活性ガスを通気しなが
ら外部より加熱し、脱水処理したものを使用し、これに
常温以下で不純物を含むNF3 ガスを通気する。通気後脱
水処理と同様に外部より加熱し、再生を行うことによっ
て繰り返し、該天然ゼオライトを使用することができ
る。[0004] In particular, natural zeolite is a preferable adsorbent in this respect, because it adsorbs the impurities efficiently. Natural zeolites are packed in containers usually cylindrical and (adsorption column), this was heated from the outside while passing an inert gas such as N 2 gas, using those dehydrated, this impurity at room temperature or less Vent NF 3 gas containing. The natural zeolite can be used repeatedly by external heating and regeneration as in the case of dehydration after aeration.
【０００５】 しかし、これらを工業的に行う場
合、多量の天然ゼオライトを必要とし円筒形の吸着塔の
径が大きくなり、脱水及び再生時に外部から加熱しても
天然ゼオライト層内が均一な温度とならず、最適な温度
条件で脱水及び再生を行うことが困難である。また、Ｎ
Ｆ３ガス通気時に吸着熱が発生するが、これも吸着塔の
径が大きくなると除熱が不充分となり不純物を吸着しな
いばかりか、ＮＦ３ガスと天然ゼオライトが反応する恐
れがある。However, when these are industrially performed, a large amount of natural zeolite is required, and a cylindrical adsorption tower is required.
Since the diameter becomes large and the temperature inside the natural zeolite layer does not become uniform even when externally heated during dehydration and regeneration, it is difficult to perform dehydration and regeneration under optimal temperature conditions. Also, N
The heat of adsorption is generated when the F 3 gas is ventilated.
When the diameter is large, heat removal becomes insufficient and not only impurities are not adsorbed, but also NF 3 gas may react with natural zeolite.
【０００６】[0006]
【課題を解決するための手段】本発明はかかる状況に鑑
み工業的に使用される吸着塔において天然ゼオライトが
均一な温度で脱水及び再生ができ、また、NF3 ガス通気
時に発生する吸着熱を速やかに除熱する方法について鋭
意検討を重ねた結果、該天然ゼオライトを充填する吸着
塔内部に、NF3 ガスの通気時に妨げない方法で伝熱のよ
い金属板を挿入する。その後N2ガス等の不活性ガスを通
気しながら吸着塔外部より加熱すれば均一な温度で脱
水、再生を行うことができ、かつNF3 ガス通気に発生す
る吸着熱も容易に除熱できることを見出し、本発明を完
成するに至った。SUMMARY OF THE INVENTION In view of the above circumstances, the present invention enables natural zeolite to be dehydrated and regenerated at a uniform temperature in an industrially used adsorption tower, and to reduce the heat of adsorption generated during the passage of NF 3 gas. As a result of intensive studies on a method of quickly removing heat, a metal plate having good heat transfer is inserted into the adsorption tower filled with the natural zeolite by a method that does not hinder the passage of NF 3 gas. Thereafter, if heating is performed from the outside of the adsorption tower while passing an inert gas such as N 2 gas, dehydration and regeneration can be performed at a uniform temperature, and the heat of adsorption generated in the NF 3 gas ventilation can be easily removed. As a result, the present invention has been completed.
【０００７】 即ち、本発明は三弗化窒素ガス中に含
まれる亜酸化窒素、二酸化炭素及び二弗化二窒素を除去
するに際し、天然ゼオライト層に金属板を挿入し、天然
ゼオライトの脱水及び再生時の温度を２５０〜７００℃
とし、該三弗化窒素ガス通気時の温度を０〜３０℃とす
ることを特徴とする三弗化窒素ガスの精製方法に関す
る。That is, according to the present invention , a metal plate is inserted into a natural zeolite layer to remove nitrous oxide, carbon dioxide and dinitrogen difluoride contained in nitrogen trifluoride gas ,
The temperature at the time of dehydration and regeneration of zeolite is 250-700 ° C
And a method for purifying nitrogen trifluoride gas, characterized in that the temperature at the time of nitrogen trifluoride gas ventilation is 0 to 30 ° C.
【０００８】発明の詳細な開示以下、本発明を更に詳細
に説明する。天然ゼオライトには鉱物学的には種々の種
類のものがあるが、本発明において使用する天然ゼオラ
イトは特にその種類に限定はない。しかしながら埋蔵量
が豊富であることと採掘費用が低廉であることから、ホ
ウフッ石（analcine)、シャバサイト (chabazite)、ク
リノプチロライト (clinoptilolite) 、エリオナイト(e
rionite)、モルデナイト (mordenite)等が好ましい。DETAILED DESCRIPTION OF THE INVENTION The present invention will be described below in more detail. There are various types of natural zeolites in mineralogy, but the types of natural zeolites used in the present invention are not particularly limited. However, due to the abundant reserves and low mining costs, fluorite (analcine), chabazite, clinoptilolite, erionite (e
rionite), mordenite and the like.
【０００９】更にまた、これらの中でもクリノプチロラ
イト〔Na6(AlO2)8(SiO2)3O・24H2O及びモルデナイト〔N
a8(AlO2)8(SiO2)4O・24H2O〕はNa型であり、吸着性単位
当たりのNF3 ガス中の不純物の吸着量が大きいので好ま
しい。天然ゼオライトは堆積岩中に産出する鉱物である
ので、本発明においては吸着剤として使用するために
は、岩石状として採取された天然ゼオライトを適当な粒
度、例えば４〜100 メッシュ、好ましくは８〜60メッシ
ュ程度に粉砕する必要がある。Furthermore, among these, clinoptilolite [Na 6 (AlO 2 ) 8 (SiO 2 ) 3 O.24H 2 O and mordenite [N
a 8 (AlO 2 ) 8 (SiO 2 ) 4 O · 24H 2 O] is a Na type, and is preferable because the amount of impurities adsorbed in the NF 3 gas per unit of adsorptivity is large. Since natural zeolite is a mineral produced in sedimentary rocks, in order to use it as an adsorbent in the present invention, natural zeolite collected as a rock must have a suitable particle size, for example, 4 to 100 mesh, preferably 8 to 60 mesh. It is necessary to pulverize to a mesh size.
【００１０】粉砕された天然ゼオライトは、次に加熱し
て脱水処理しなければならない。該天然ゼオライトは結
晶水を含有しているので、該天然ゼオライトを本発明の
吸着剤として使用する場合には、上記結晶水 (以下、水
分と記す) が残存し、該天然ゼオライト層へNF3 ガスを
通気した際にN2O 、CO2 、N2F2の除去能力が低下するの
で、本発明では天然ゼオライト中の水分を実質的に完全
に除去するための脱水処理が必要である。[0010] The ground natural zeolite must then be heated and dewatered. Since the natural zeolite contains water of crystallization, when the natural zeolite is used as the adsorbent of the present invention, the water of crystallization (hereinafter referred to as water) remains and NF 3 is added to the natural zeolite layer. Since the ability to remove N 2 O, CO 2 , and N 2 F 2 is reduced when gas is ventilated, the present invention requires a dehydration treatment to substantially completely remove moisture in natural zeolite.
【００１１】脱水処理は、処理した後大気との接触を避
けるため、あらかじめ吸着塔内に入れ、吸着塔外部より
ヒーターで加熱する。その際、N2ガス等の不活性なキャ
リヤーガスを通気し天然ゼオライトの吸着、活性効果を
高める。脱水温度は、250 〜700 ℃、好ましくは300 〜
600 ℃の温度に加熱することで実施される。[0011] In the dehydration treatment, in order to avoid contact with the atmosphere after the treatment, the dehydration treatment is carried out in advance in an adsorption tower and heated by a heater from the outside of the adsorption tower. At this time, an inert carrier gas such as N 2 gas is passed to enhance the adsorption and activation effect of natural zeolite. The dehydration temperature is from 250 to 700 ° C, preferably from 300 to 700 ° C.
It is carried out by heating to a temperature of 600 ° C.
【００１２】また、加熱時間は10〜20時間が好ましく、
20時間以上連続して加熱するとN2O 、CO2 、N2F2の除去
能力が低下する。再生処理は、吸着破過した天然ゼオラ
イトを脱水処理と同様に吸着塔内に入れた状態で、外部
加熱によって吸着した不純物を離脱させる。再生温度は
脱水温度と同じ条件で実施される。再生時間も脱水時間
と同じ条件で実施可能である。The heating time is preferably 10 to 20 hours,
Heating continuously for 20 hours or more decreases the ability to remove N 2 O, CO 2 , and N 2 F 2 . The regeneration treatment removes the adsorbed impurities by external heating in a state where the natural zeolite that has passed through the adsorption is placed in the adsorption tower in the same manner as the dehydration treatment. The regeneration temperature is performed under the same conditions as the dehydration temperature. The regeneration time can be performed under the same conditions as the dehydration time.
【００１３】次に天然ゼオライト層に挿入する金属板に
ついて説明する。使用する金属板の種類は、鉄、ステン
レス、銅、ニッケル、モネル等が使用できるが比較的錆
びにくく、加工しやすいステンレスを使用するのが慣用
である。Next, the metal plate to be inserted into the natural zeolite layer will be described. As the type of metal plate to be used, iron, stainless steel, copper, nickel, monel, etc. can be used, but it is customary to use stainless steel which is relatively hard to rust and is easy to process.
【００１４】 金属板の枚数、形状及び挿入において
は種々の方法があり、特に、限定するものではなく、吸
着塔の形状によって最も好ましい方法で挿入することが
できる。例えば、第１図に示すように穴の開いた目皿を
縦長の吸着塔に対して平行に数枚、該天然ゼオライト層
内に挿入する方法がある。また、第２図に示すように、
羽根型をした金属板を該天然ゼオライト層内に挿入する
方法もある。There are various methods for the number, shape, and insertion of the metal plates, and there is no particular limitation, and the metal plate can be inserted by the most preferable method depending on the shape of the adsorption tower. For example, as shown in FIG. 1, there is a method of inserting several perforated plates parallel to the vertically long adsorption tower into the natural zeolite layer. Also, as shown in FIG.
There is also a method of inserting a metal plate in which the vane to the natural zeolite layer.
【００１５】第２図においては、更に、金属板と吸着塔
内壁とを密着するか溶接することも可能である。このよ
うに金属板を挿入することにより、脱水処理及び再生処
理時に外部より加熱するので吸着塔内壁近くで温められ
た熱を、挿入した金属で中心部に伝熱せしめ中心部の天
然ゼオライトも充分に加熱することができ、該天然ゼオ
ライト層内の温度が均一となる。In FIG. 2, the metal plate and the inner wall of the adsorption tower can be closely adhered or welded. By inserting a metal plate in this way, heat is heated from the outside near the inner wall of the adsorption tower during dehydration treatment and regeneration treatment, so that the inserted metal transfers heat to the center and the natural zeolite in the center is sufficient. And the temperature in the natural zeolite layer becomes uniform.
【００１６】天然ゼオライトをはじめ、合成ゼオライト
やシリカゲル及び活性炭等の吸着剤は比較的伝熱が悪い
ため、大きな吸着塔を使用すると中心部まで最適温度に
達しにくくなる。Adsorbents such as natural zeolites, synthetic zeolites, silica gel, and activated carbon have relatively poor heat transfer, so that if a large adsorption tower is used, it is difficult to reach the optimum temperature up to the center.
【００１７】 従って、金属板の挿入方法は、ガス通
気に際して通気を妨げない方法で、かつ塔内壁から中心
部に至る間を１枚の連なる金属板を挿入する必要があ
る。ＮＦ3ガス通気時の天然ゼオライト層の温度は、０
〜３０℃で実施されるが、通気の初期においては吸着熱
が出る。吸着塔の径が大きくなると吸着熱が内部にこも
り内部の温度が上昇する。このように吸着熱によって温
度が上昇すると不純物の除去能力を低下させることにな
る。更には２００℃以上に上昇するとＮＦ3ガスと天然
ゼオライトが反応し、この反応熱で一気に暴走反応して
しまう危険がある。従って、この吸着熱を速やかに塔外
に除去する必要があるが、金属板を挿入することは、こ
の吸着熱の除去効果も兼ね備えている。[0017] Therefore, it is necessary to insert a metal plate in a manner that does not hinder the ventilation during gas ventilation, and to insert one continuous metal plate from the inner wall of the tower to the center. The temperature of the natural zeolite layer during NF 3 gas ventilation is 0
It is carried out at ３０30 ° C., but heat of adsorption is generated at the beginning of the aeration. As the diameter of the adsorption tower increases, the heat of adsorption is trapped inside and the temperature inside rises. When the temperature rises due to the heat of adsorption, the ability to remove impurities is reduced. Further, when the temperature rises to 200 ° C. or higher, the NF 3 gas reacts with the natural zeolite, and there is a risk that a runaway reaction may be caused at once by the reaction heat. Therefore, it is necessary to quickly remove the heat of adsorption to the outside of the tower, but inserting a metal plate also has the effect of removing the heat of adsorption.
【００１８】[0018]
【実施例】実施例１ 第１図に示すように、長さ１ｍ、塔径0.2 ｍのステンレ
ス（SUS310) の吸着塔（１）の天然ゼオライト（２）層
内に10cm毎にステンレス（SUS304) の円盤状の目皿型金
属板(3)(穴径２cm、穴 100個) を挿入し、モルデナイト
型天然ゼオライトを、高さ ０．８ｍのところまで充填
した。脱水処理のためN2ガスを10L/minで通気しなが
ら、３ kＷの外部ヒーター（５）で塔壁温度450 ℃に設
定し加熱を開始した。その結果、約２時間で天然ゼオラ
イト層内の温度計（６）の部分が 380℃まで昇温し安定
した。EXAMPLE 1 As shown in FIG. 1, stainless steel (SUS304) was introduced at every 10 cm in a natural zeolite (2) layer of a stainless steel (SUS310) adsorption tower (1) having a length of 1 m and a tower diameter of 0.2 m. And a mordenite-type natural zeolite was filled to a height of 0.8 m. The tower wall temperature was set to 450 ° C. with an external heater (5) of 3 kW while passing N 2 gas at 10 L / min for dehydration treatment, and heating was started. As a result, the temperature of the thermometer (6) in the natural zeolite layer rose to 380 ° C. in about 2 hours and was stabilized.
【００１９】上記条件で20時間加熱後、吸着塔を室温
(20℃)まで冷却し、N2O 0.3 ％を含むNF3 ガスをNF3 ガ
ス入口（８） より 15 Ｌ/minで通気した。NF3 ガス出
口（９）をガスクロマトグラフィーで検知したところ、
約84時間でN2O が検出され吸着破過した。通気時の吸着
熱測定ではNF3 ガス通気開始から、30分後天然ゼオライ
ト層内の中心部の温度計（７）の部分が28℃と最高値を
示したが２時間後22℃で安定した。再度、N2ガスを10Ｌ
/minで通気しながら、同ヒーター（５）で400 ℃に設定
し、加熱再生を開始した。その結果、約２時間で温度計
（６）の温度が320℃まで昇温し、安定した。After heating under the above conditions for 20 hours, the adsorption tower is brought to room temperature.
(20 ° C.), and NF 3 gas containing 0.3% of N 2 O was passed through the NF 3 gas inlet (8) at 15 L / min. When gas chromatography detected the NF 3 gas outlet (9),
At about 84 hours, N 2 O was detected and adsorption breakthrough occurred. In the measurement of adsorption heat during aeration, the thermometer (7) at the center of the natural zeolite layer showed a maximum value of 28 ° C. 30 minutes after the start of NF 3 gas aeration, but stabilized at 22 ° C. after 2 hours. . Again, 10 L of N 2 gas
While aerating at / min, the temperature was set to 400 ° C. by the same heater (5) and heating and regeneration were started. As a result, the temperature of the thermometer (6) rose to 320 ° C. in about 2 hours, and was stabilized.
【００２０】通気、再生を５回繰り返したところで６回
目の通気を行ったところ、N2O 0.3 ％を含むNF3 ガスの
吸着破過時間は、80時間であった。When aeration and regeneration were repeated five times and aeration was performed a sixth time, the adsorption breakthrough time of NF 3 gas containing 0.3% of N 2 O was 80 hours.
【００２１】ここでいう破過時間とは、不純物を含有す
るガスを吸着剤層に通気して不純物を吸着除去する場
合、ガスの通気開始直後は得られるガス中の不純物含有
量は少なく、かつ一定含有量かまたは漸増する状態で推
移する。しかし吸着剤が吸着能力を喪失するころになる
と、不純物含有量が急激に増加し始める。この急激に増
加し始めるまでの通気時間を破過時間という。The term "breakthrough time" as used herein means that when a gas containing impurities is passed through the adsorbent layer to adsorb and remove the impurities, the content of impurities in the gas obtained immediately after the start of gas ventilation is small, and It changes in a state where the content is constant or gradually increases. However, when the adsorbent is about to lose its adsorption capacity, the impurity content starts to increase sharply. The ventilation time until the rapid increase starts is called breakthrough time.
【００２２】実施例２ 第２図に示すように、実施例１と同じ吸着塔（１）を用
い羽根型金属板（４）（８枚羽根）に加工したステンレ
ス（SUS304) を挿入し、これにモルデナイト型天然ゼオ
ライト（２）を高さ、０．８ｍまで充填した。Example 2 As shown in FIG. 2, stainless steel (SUS304) processed into a blade-shaped metal plate (4) (eight blades) was inserted using the same adsorption tower (1) as in Example 1, and Was filled with a natural mordenite zeolite (2) to a height of 0.8 m.
【００２３】実施例１と同様に脱水処理を行ったとこ
ろ、1.5 時間で塔内の温度計（６）部分が、400 ℃まで
昇温し安定した。20時間加熱後、室温 (20℃) まで冷却
し、実施例１と同等のNF3 ガスをNF3 ガス入口（８）よ
り通気したところ、約85時間で吸着破過した。When the dehydration treatment was carried out in the same manner as in Example 1, the temperature of the thermometer (6) in the column was raised to 400 ° C. in 1.5 hours and stabilized. After heating for 20 hours, the system was cooled to room temperature (20 ° C.), and the same NF 3 gas as in Example 1 was passed through the NF 3 gas inlet (8).
【００２４】通気時の吸着熱測定では、NF3 ガス通気開
始から30分後天然ゼオライト（２）層内のはぼ中心部の
温度計（７）部分が27℃と最高値を示したが1.5 時間後
22℃で安定した。実施例１と同様に、通気、再生を５回
繰り返したところで６回目の通気を行ったところ、N2O
0.3 ％を含むNF3 ガスの吸着破過時間は、80時間であっ
た。In the measurement of heat of adsorption during aeration, the thermometer (7) at the center of the warp in the natural zeolite (2) layer showed a maximum value of 27 ° C. 30 minutes after the start of the aeration of the NF 3 gas. After hours
Stable at 22 ° C. As in Example 1, the vent was subjected to a sixth aeration was repeated 5 times playback, N 2 O
The adsorption breakthrough time of NF 3 gas containing 0.3% was 80 hours.
【００２５】比較例１ 第３図に示すように、実施例１と同じ吸着塔（１）を用
い金属板を使用せず、モルデナイト型天然ゼオライト
（２）を高さ、０．８ｍまで充填した。実施例１と同様
に脱水処理し、塔壁温度450 ℃に設定し加熱を開始した
ところ塔内の温度計(６）の部分は、５時間で250 ℃し
か昇温せずに安定した。Comparative Example 1 As shown in FIG. 3, a mordenite type natural zeolite (2) was packed to a height of 0.8 m using the same adsorption tower (1) as in Example 1 without using a metal plate. . Dehydration treatment was performed in the same manner as in Example 1, and the column wall temperature was set to 450 ° C., and heating was started. When the temperature of the thermometer (6) in the column was raised to 250 ° C. in 5 hours, the temperature was stabilized and stabilized.
【００２６】20時間加熱した後、室温 (20℃) まで冷却
し、実施例１と同等のNF3 ガスをNF 3 ガス入口（８）よ
り通気したところ、約２時間で破過した。通気時の吸着
熱測定では、天然ゼオライト（２）層内のほぼ中心部の
温度計（７）の部分が、NF3 ガス通気開始から25分後、
40℃、更に40分後最高温度の73℃まで昇温した。After heating for 20 hours, cool to room temperature (20 ° C.)
NF equivalent to that of the first embodimentThree NF gas Three Gas inlet (8)
After aeration, it broke through in about 2 hours. Adsorption during ventilation
In the heat measurement, the center of the natural zeolite (2) layer
The part of the thermometer (7) is NFThree 25 minutes after the start of gas ventilation,
The temperature was raised to 40 ° C., and after a further 40 minutes, to the maximum temperature of 73 ° C.
【００２７】[0027]
【発明の効果】以上、詳細に説明したように本発明は、
NF3 ガス中のN2O 、CO2 、N2F2を工業に安全に、かつ効
率よく除去する方法である。天然ゼオライト層内に金属
板を挿入することによって、脱水処理や再生処理におい
て最適温度で均一に加熱することができ、天然ゼオライ
トの活性化能力を充分に生かすことが出来るようになっ
た。また、本発明はNF3 ガス通気時の吸着熱の除去効果
を兼ね備えているので安全面でも改善され、工業的な操
業が可能となった。As described above, the present invention provides:
This is a method for industrially safely and efficiently removing N 2 O, CO 2 , and N 2 F 2 in NF 3 gas. By inserting a metal plate into the natural zeolite layer, it is possible to uniformly heat at an optimum temperature in the dehydration treatment and the regeneration treatment, and to fully utilize the activation ability of the natural zeolite. In addition, the present invention also has an effect of removing heat of adsorption at the time of aeration of NF 3 gas, so that safety is improved and industrial operation is possible.
【００２８】[0028]
【図１】目皿型金属板を使用した場合の吸着塔FIG. 1 shows an adsorption tower using a perforated metal plate.
【図２】羽根型金属板を使用した場合の吸着塔Fig. 2 Adsorption tower using blade-shaped metal plate
【図３】本発明を使用しない従来の方法による吸着塔FIG. 3 shows a conventional adsorption tower without using the present invention.
【００２９】[0029]
１ 吸着塔 ２ 天然ゼオライト ３ 目皿型金属板 ４ 羽根型金属板 ５ ヒーター ６ 温度計 7 温度計 8 NF3 ガス入口 9 NF3 ガス出口DESCRIPTION OF SYMBOLS 1 Adsorption tower 2 Natural zeolite 3 Plate-shaped metal plate 4 Blade-shaped metal plate 5 Heater 6 Thermometer 7 Thermometer 8 NF 3 Gas inlet 9 NF 3 Gas outlet
Claims (1)
素、二酸化炭素及び二弗化二窒素を除去するに際し、天
然ゼオライト層に金属板を挿入し、天然ゼオライトの脱
水及び再生時の温度を２５０〜７００℃とし、該三弗化
窒素ガス通気時の温度を０〜３０℃とすることを特徴と
する三弗化窒素ガスの精製方法。1. A nitrous oxide contained in nitrogen trifluoride gas, upon the removal of carbon dioxide and difluoride dinitrogen heaven
Naturally, insert a metal plate into the zeolite layer to remove the natural zeolite.
The temperature at the time of water and regeneration is 250 to 700 ° C.
A method for purifying nitrogen trifluoride gas, wherein the temperature at the time of passing nitrogen gas is 0 to 30 ° C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP40829390A JP2954364B2 (en) | 1990-12-27 | 1990-12-27 | Purification method of nitrogen trifluoride gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP40829390A JP2954364B2 (en) | 1990-12-27 | 1990-12-27 | Purification method of nitrogen trifluoride gas |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH04228408A JPH04228408A (en) | 1992-08-18 |
| JP2954364B2 true JP2954364B2 (en) | 1999-09-27 |
Family
ID=18517765
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP40829390A Expired - Lifetime JP2954364B2 (en) | 1990-12-27 | 1990-12-27 | Purification method of nitrogen trifluoride gas |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JP2954364B2 (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| KR100841183B1 (en) * | 2003-09-23 | 2008-06-24 | 주식회사 효성 | Method for NF3 Purification using Zeolite absorbent impregnated with Nickel and Copper |
| US8404024B2 (en) * | 2010-04-15 | 2013-03-26 | Air Products And Chemicals, Inc. | Recovery of NF3 from adsorption operation |
-
1990
- 1990-12-27 JP JP40829390A patent/JP2954364B2/en not_active Expired - Lifetime
Also Published As
| Publication number | Publication date |
|---|---|
| JPH04228408A (en) | 1992-08-18 |
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