JPH0463993B2 - - Google Patents
Info
- Publication number
- JPH0463993B2 JPH0463993B2 JP60063534A JP6353485A JPH0463993B2 JP H0463993 B2 JPH0463993 B2 JP H0463993B2 JP 60063534 A JP60063534 A JP 60063534A JP 6353485 A JP6353485 A JP 6353485A JP H0463993 B2 JPH0463993 B2 JP H0463993B2
- Authority
- JP
- Japan
- Prior art keywords
- air
- temperature
- nitrogen
- raw air
- hydrogen
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
Classifications
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/044—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air using a single pressure main column system only
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
- F25J3/04163—Hot end purification of the feed air
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J3/00—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification
- F25J3/02—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream
- F25J3/04—Processes or apparatus for separating the constituents of gaseous or liquefied gaseous mixtures involving the use of liquefaction or solidification by rectification, i.e. by continuous interchange of heat and material between a vapour stream and a liquid stream for air
- F25J3/04151—Purification and (pre-)cooling of the feed air; recuperative heat-exchange with product streams
- F25J3/04163—Hot end purification of the feed air
- F25J3/04169—Hot end purification of the feed air by adsorption of the impurities
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2200/00—Processes or apparatus using separation by rectification
- F25J2200/72—Refluxing the column with at least a part of the totally condensed overhead gas
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2205/00—Processes or apparatus using other separation and/or other processing means
- F25J2205/82—Processes or apparatus using other separation and/or other processing means using a reactor with combustion or catalytic reaction
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F25—REFRIGERATION OR COOLING; COMBINED HEATING AND REFRIGERATION SYSTEMS; HEAT PUMP SYSTEMS; MANUFACTURE OR STORAGE OF ICE; LIQUEFACTION SOLIDIFICATION OF GASES
- F25J—LIQUEFACTION, SOLIDIFICATION OR SEPARATION OF GASES OR GASEOUS OR LIQUEFIED GASEOUS MIXTURES BY PRESSURE AND COLD TREATMENT OR BY BRINGING THEM INTO THE SUPERCRITICAL STATE
- F25J2215/00—Processes characterised by the type or other details of the product stream
- F25J2215/42—Nitrogen or special cases, e.g. multiple or low purity N2
- F25J2215/44—Ultra high purity nitrogen, i.e. generally less than 1 ppb impurities
Landscapes
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- Mechanical Engineering (AREA)
- Thermal Sciences (AREA)
- General Engineering & Computer Science (AREA)
- Separation By Low-Temperature Treatments (AREA)
- Separation Of Gases By Adsorption (AREA)
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、空気から窒素等の製品ガスを分離す
る空気分離装置に係り、特に高純度窒素を製造す
るのに好適な方法および装置に関する。DETAILED DESCRIPTION OF THE INVENTION [Field of Industrial Application] The present invention relates to an air separation device for separating a product gas such as nitrogen from air, and particularly to a method and device suitable for producing high-purity nitrogen.
一般に、空気分離装置は、原料空気を圧縮機に
て圧縮昇圧させ、この圧縮熱により高温となつた
原料空気をアフタークーラーにて冷却し、次いで
原料空気中の水分（H2O）および二酸化炭素
（CO2）を吸着塔によつて吸着除去し、H2Oおよ
びCO2除去後の原料空気を熱交換器を介して精留
塔に供給して製品ガス（窒素あるいは酸素）を精
留分離している。このような空気分離装置は、例
えば特開昭56−97772号、特開昭55−49681号、特
開昭55−38423号、特開昭54−52667号、特開昭54
−84888号に開示される。
Generally, air separation equipment compresses and pressurizes feed air using a compressor, cools the feed air that has become high temperature due to the heat of compression using an aftercooler, and then removes moisture (H 2 O) and carbon dioxide from the feed air. (CO 2 ) is adsorbed and removed by an adsorption tower, and the raw air after removing H 2 O and CO 2 is supplied to a rectification tower via a heat exchanger to separate product gas (nitrogen or oxygen) by rectification. are doing. Such air separation devices are disclosed in, for example, JP-A-56-97772, JP-A-55-49681, JP-A-55-38423, JP-A-54-52667, and JP-A-54.
-Disclosed in No. 84888.
ところで、半導体製造プロセス等では、大量の
窒素が使用されているが、ここで使用される窒素
は、非常に高純度のものが要求される。特に、窒
素中に一酸化炭素、水素が含まれることは、半導
体の性能劣化、品質不良の原因となり好ましくな
い。深冷分離により製造された窒素ガス中には、
窒素と同程度の沸点を有するか、それより低い沸
点を有する物質が混入している。この様な物質と
しては、ヘリウム、ネオン、水素、アルゴン、一
酸化炭素が挙げられる。一方、炭素水素、塩素、
二酸化炭素、水分等は、窒素より沸点が高いた
め、窒素中にはほとんど含まれない。従つて、半
導体製造プロセスに使用する窒素を深冷分離によ
る空気分離法で製造する場合には、水素および一
酸化炭素を如何にする除去するかが問題となる。
この様な背景のもとで、従来は、窒素ガス中に含
まれる水素、一酸化炭素を除去する精製装置が使
用されていた。以下、従来の精製装置の構成につ
いて概略説明する。第３図に従来の水素および一
酸化炭素の除去装置の系統図を示す。 Incidentally, large amounts of nitrogen are used in semiconductor manufacturing processes and the like, and the nitrogen used here is required to be of extremely high purity. In particular, the inclusion of carbon monoxide and hydrogen in nitrogen is undesirable because it causes performance deterioration and quality defects of semiconductors. Nitrogen gas produced by cryogenic separation contains
Contains a substance with a boiling point similar to or lower than that of nitrogen. Such substances include helium, neon, hydrogen, argon, and carbon monoxide. On the other hand, carbon hydrogen, chlorine,
Carbon dioxide, water, etc. have higher boiling points than nitrogen, so they are hardly included in nitrogen. Therefore, when nitrogen used in a semiconductor manufacturing process is produced by an air separation method using cryogenic separation, the problem is how to remove hydrogen and carbon monoxide.
Against this background, purification equipment for removing hydrogen and carbon monoxide contained in nitrogen gas has conventionally been used. The configuration of a conventional purification device will be briefly described below. FIG. 3 shows a system diagram of a conventional hydrogen and carbon monoxide removal device.
導管４１から供給される水素、一酸化炭素を含
む窒素ガスに対して、導管４２を通して、燃焼用
の酸素ガスが添加される。添加する酸素ガスの量
は、水素と一酸化炭素を燃焼するに必要な量よ
り、多少多目とし、未燃の水素、一酸化炭素が残
存しない様にする。次に、この混合ガスは、電気
ヒータ５１により、90〜120℃程度まで昇温した
後、燃焼触媒を充填した触媒槽５２に供給され
る。これは、水素は室温でも酸素と反応燃焼する
が、一酸化炭素の燃焼開始には前記の温度まで昇
温する必要があるためである。触媒槽５２の中
で、水素は酸素と反応して水分に、一酸化炭素は
酸素と反応して二酸化炭素となる。未反応の加剰
に加えられた酸素は、次に設けられた酸素吸収触
媒（例えばCu）を充填した触媒槽５３により反
応吸収され、窒素ガス中から除去される。次い
で、導管４６を介して冷却器５４に導かれ、ここ
で室温まで冷却される。冷却された窒素ガスは導
管４７を介して吸着塔５５に供給され、ここに充
填されている吸着剤により、水分と炭酸ガスが除
去される。通常、酸素吸収触媒槽５３と吸着塔５
５は、夫々２基設置され、切替使用される。すな
わち、一方が吸収または吸着動作中に他方はその
機能を再生させ、これらを切替えることによつて
連続して吸収または吸着動作を行わせる。 Oxygen gas for combustion is added through a conduit 42 to nitrogen gas containing hydrogen and carbon monoxide supplied from a conduit 41 . The amount of oxygen gas added is slightly larger than the amount required to burn hydrogen and carbon monoxide, so that unburned hydrogen and carbon monoxide do not remain. Next, this mixed gas is heated to about 90 to 120° C. by an electric heater 51 and then supplied to a catalyst tank 52 filled with a combustion catalyst. This is because hydrogen reacts and burns with oxygen even at room temperature, but it is necessary to raise the temperature to the above temperature in order to start burning carbon monoxide. In the catalyst tank 52, hydrogen reacts with oxygen to become water, and carbon monoxide reacts with oxygen to become carbon dioxide. The unreacted excess oxygen is then reacted and absorbed by a catalyst tank 53 filled with an oxygen absorption catalyst (for example, Cu), and is removed from the nitrogen gas. It is then led via conduit 46 to cooler 54 where it is cooled to room temperature. The cooled nitrogen gas is supplied to the adsorption tower 55 via the conduit 47, and water and carbon dioxide are removed by the adsorbent filled therein. Usually, the oxygen absorption catalyst tank 53 and the adsorption tower 5
Two units of 5 are installed and used in a switched manner. That is, while one is performing absorption or adsorption operation, the other regenerates its function, and by switching between these, the absorption or adsorption operation is performed continuously.
このような精製装置を付加することによつて、
空気分離装置で製造された窒素を精製し、窒素中
から一酸化炭素、水素を除去することができる。
しかし、これでは装置全体が複雑化すると共に、
高純度の酸素の使用、電力エネルギーの消費等に
よる運転費のコストアツプとなる。 By adding such a purification device,
Nitrogen produced by an air separation device can be purified to remove carbon monoxide and hydrogen from the nitrogen.
However, this makes the entire device complicated, and
Operating costs will increase due to the use of high-purity oxygen and the consumption of electrical energy.
本発明の目的は、圧縮機の昇圧熱により原料空
気を昇温して触媒反応させ、水素及び一酸化炭素
を含まない高純度の窒素ガスを製造する窒素製造
方法及び装置を提供することにある。
An object of the present invention is to provide a nitrogen production method and apparatus for producing high-purity nitrogen gas that does not contain hydrogen and carbon monoxide by raising the temperature of raw air using the heat of pressurization of a compressor and causing a catalytic reaction. .
本発明は、原料空気を空気圧縮機で圧縮し、圧
縮により原料空気の温度を触媒反応に適した90℃
〜120℃温度まで昇温し、該昇温された原料空気
を触媒槽に導入し該触媒槽で原料空気中の可燃成
分である水素及び精留によつて窒素と分離が困難
な一酸化炭素と酸素とを反応・燃焼させ、該反
応・燃焼で昇温した圧縮された原料空気を常温ま
で冷却後原料空気中の不純物である反応生成物
（水分および二酸化炭素）を除去し、該不純物の
除去された原料空気から深冷分離により高純度の
窒素ガスを製造することを特徴とする。
The present invention compresses raw air using an air compressor, and the temperature of the raw air is reduced to 90°C, which is suitable for catalytic reactions.
The heated feed air is heated to ~120°C and introduced into a catalyst tank where hydrogen, which is a combustible component in the feed air, and carbon monoxide, which is difficult to separate from nitrogen through rectification, are removed. and oxygen are reacted and combusted, and the compressed raw material air that has been heated through the reaction and combustion is cooled down to room temperature, and the reaction products (moisture and carbon dioxide) that are impurities in the raw material air are removed, and the impurities are removed. It is characterized by producing high-purity nitrogen gas from the removed raw material air by cryogenic separation.
以下、本発明を実施例により説明する。第１図
は本発明の一実施例を示すフローシート図であ
る。第１図において、フイルター１は原料となる
空気中のちり等を除去する。空気圧縮機２はフイ
ルター１通過後の原料空気を圧縮（昇圧）する。
触媒槽３には、白金やパラジウム等の触媒が充填
されており、ここで空気中の可燃成分が燃焼され
る。冷却器４は原料空気を冷却する。吸着塔５に
は、水分および二酸化炭素等の不純物を吸着する
吸着剤が充填されており、ここで原料空気中の水
分および二酸化炭素等の不純物を吸着除去する。
100は深冷分離部であり、熱交換器６、精留塔７
等で構成される。熱交換器６は、原料空気を精留
塔７からの戻りのガスの寒冷によつて深冷温度ま
で低下させる。精留塔７は、熱交換器６によつて
低温となつた原料空気の供給を受け、製品ガス
（この例では、窒素のみ）を精留分離する。ここ
での廃ガスおよび製品ガスは、熱交換器６の戻り
ガスとなる。８は精留塔上部の凝縮器、１１〜２
３は導管、３１は膨張弁、３２〜３９は吸着塔５
の切替弁である。
The present invention will be explained below using examples. FIG. 1 is a flow sheet diagram showing one embodiment of the present invention. In FIG. 1, a filter 1 removes dust and the like from the air, which is a raw material. The air compressor 2 compresses (boosts the pressure) the raw air that has passed through the filter 1.
The catalyst tank 3 is filled with a catalyst such as platinum or palladium, and combustible components in the air are burned here. The cooler 4 cools the raw air. The adsorption tower 5 is filled with an adsorbent that adsorbs impurities such as moisture and carbon dioxide, and adsorbs and removes impurities such as moisture and carbon dioxide from the raw air.
100 is a cryogenic separation section, which includes a heat exchanger 6 and a rectification column 7.
Consists of etc. The heat exchanger 6 lowers the feed air to a cryogenic temperature by cooling the gas returned from the rectification column 7. The rectifying column 7 is supplied with the raw material air that has been made low temperature by the heat exchanger 6, and rectifies and separates the product gas (in this example, only nitrogen). The waste gas and product gas here become the return gas of the heat exchanger 6. 8 is a condenser at the top of the rectification column, 11-2
3 is a conduit, 31 is an expansion valve, and 32 to 39 are adsorption towers 5
This is a switching valve.
水素、一酸化炭素等を燃焼させる燃焼触媒を充
填した触媒槽３は、空気圧縮機２の出口と、冷却
器４の中間に設けられている。これは、圧縮熱に
より空気の温度が90〜120℃に上昇していること
を利用して触媒槽３における反応を起こさせるた
めである。空気中の水素、一酸化炭素は空気中に
大過剰に存在する酸素と燃焼触媒のもとで反応す
る。反応生成物は、水分および二酸化炭素であ
る。酸素21％に対して、水素、一酸化炭素の濃度
は高々数十ppm程度であり、未反応の水素、一酸
化炭素が残存する可能性は非常に希である。反応
による生成熟もわずかであり、温度上昇は高々数
度Ｃなので、加熱防止等の考慮は必要でない。水
素、一酸化炭素等が燃焼除去された空気は、導管
１３を通つて冷却器４に導かれる。冷却器で水に
より室温まで冷却された後、導管１４により、吸
着塔５に導かれる。吸着塔は通常２基からそれ以
上設けられ、一方を再生しながら、交互に切替え
られて使用される。吸着塔５には水分、炭酸ガス
を吸着除去する吸着剤が充填されているので、吸
着塔出口の空気中には水分、二酸化炭素等の不純
物はほとんど含まれない。吸着塔５を出た空気
は、熱交換器６、精留塔７塔で構成される深冷分
離部１００に導かれる。まず、導管１５により原
料空気は熱交換器６に導入される。原料空気は、
ここで窒素ガス、廃ガスと熱交換し冷却される。
更にこの空気は、精留塔７の底部に導管１６を通
して供給される。ここで、原料空気は塔内に多数
設けられている精留皿上の液体と気液接触し、精
留分離される。この結果、精留塔７の底部には酸
素濃度の高い液体空気が溜まる。一方窒素ガス
は、精留塔上部の導管１７を通して精留塔より抜
出され、空気熱交換器６の内部で温度回復して、
製品窒素ガスとして導管１８を通して送出され
る。この場合、精留操作前でCO、H2を除去して
おり、製品窒素ガス中に一酸化炭素、水素（可燃
成分）は含まれない。なお、この例では、精留塔
７は、窒素のみを製造する単式精留塔としたが、
これは酸素ガスを同時に採取する複式精留塔であ
つてもかまわない。一方液体空気は導管１９を通
して精留塔から抜出され、途中膨張弁３１で脱圧
され、所謂ジユール・トムソン効果により、温度
降下した後、凝縮器８の冷熱源として凝縮器に供
給され、ここで蒸発した後、導管２１、空気熱交
換器６を通して常温まで温度回復し、吸着塔５の
再生ガスとして使用され、大気中に導管２３を通
して放出される。 A catalyst tank 3 filled with a combustion catalyst for burning hydrogen, carbon monoxide, etc. is provided between the outlet of the air compressor 2 and the cooler 4. This is because the reaction in the catalyst tank 3 is caused by utilizing the fact that the temperature of the air is increased to 90 to 120°C due to the heat of compression. Hydrogen and carbon monoxide in the air react with oxygen, which is present in large excess in the air, under a combustion catalyst. The reaction products are moisture and carbon dioxide. Compared to 21% oxygen, the concentration of hydrogen and carbon monoxide is at most a few tens of ppm, and the possibility that unreacted hydrogen and carbon monoxide remain is extremely rare. Since biomaturation due to the reaction is slight and the temperature rise is only a few degrees Celsius at most, there is no need to take measures to prevent heating. The air from which hydrogen, carbon monoxide, etc. have been burned and removed is led to the cooler 4 through the conduit 13. After being cooled down to room temperature with water in a cooler, it is led to an adsorption tower 5 through a conduit 14. Usually, two or more adsorption towers are provided, and one of them is regenerated while being switched to use alternately. Since the adsorption tower 5 is filled with an adsorbent that adsorbs and removes moisture and carbon dioxide, the air at the outlet of the adsorption tower contains almost no impurities such as moisture and carbon dioxide. The air leaving the adsorption tower 5 is guided to a cryogenic separation section 100 that includes a heat exchanger 6 and seven rectification towers. First, raw air is introduced into the heat exchanger 6 through the conduit 15 . The raw air is
Here, it is cooled by exchanging heat with nitrogen gas and waste gas.
Furthermore, this air is fed to the bottom of the rectification column 7 through a conduit 16. Here, the raw air comes into gas-liquid contact with the liquid on a large number of rectification plates provided in the column, and is separated by rectification. As a result, liquid air with a high oxygen concentration accumulates at the bottom of the rectification column 7. On the other hand, nitrogen gas is extracted from the rectification column through the conduit 17 at the top of the rectification column, and its temperature is recovered inside the air heat exchanger 6.
It is delivered through conduit 18 as product nitrogen gas. In this case, CO and H 2 are removed before the rectification operation, and the product nitrogen gas does not contain carbon monoxide or hydrogen (combustible components). In this example, the rectification column 7 is a single type rectification column that only produces nitrogen, but
This may be a double rectification column that simultaneously extracts oxygen gas. On the other hand, liquid air is extracted from the rectification column through the conduit 19, depressurized by the expansion valve 31 midway through, and after its temperature drops due to the so-called Juul-Thomson effect, it is supplied to the condenser 8 as a cold heat source. After being evaporated, the temperature is restored to room temperature through a conduit 21 and an air heat exchanger 6, used as regeneration gas in the adsorption tower 5, and discharged into the atmosphere through a conduit 23.
上述した実施例では、圧縮熱を利用しているの
で、水素、一酸化炭素を燃焼温度まで昇温するヒ
ーターが不用となつている。又、深冷方式の空気
分離装置と組合せてあるので、窒素ガスより沸点
の低い炭化水素類も除去できる等の効果を同時に
得ることが出来る。さらに、本実施例では原料空
気中の不純物（水分および二酸化炭素）の除去手
段に吸着等を用いているが、これは可逆式熱交換
器による除去装置を用いても同様の効果を得るこ
とが出来る。 In the embodiment described above, since the heat of compression is utilized, a heater for raising the temperature of hydrogen and carbon monoxide to the combustion temperature is unnecessary. Furthermore, since it is combined with a deep-cooling type air separation device, it is possible to obtain effects such as being able to remove hydrocarbons having a boiling point lower than that of nitrogen gas at the same time. Furthermore, in this example, adsorption or the like is used as a means for removing impurities (moisture and carbon dioxide) in the feed air, but the same effect can also be obtained by using a removal device using a reversible heat exchanger. I can do it.
第２図は、空気の圧縮熱が十分でない場合の本
発明の他の実施例である。圧縮機２と触媒槽３の
間に加熱器９を設けて、水素および一酸化炭素等
の可燃成分の燃焼に適当な90℃〜120℃の温度ま
で、加熱器で昇温している。加熱器の熱源として
は、電気、蒸気、燃焼ガスなどが挙げられる。水
素、一酸化炭素等の可燃成分を除去した後の系統
は第１図の場合と同様であり、説明は省略する。 FIG. 2 shows another embodiment of the present invention when the heat of compression of air is insufficient. A heater 9 is provided between the compressor 2 and the catalyst tank 3, and the temperature is raised to a temperature of 90°C to 120°C, which is suitable for combustion of combustible components such as hydrogen and carbon monoxide. Examples of the heat source for the heater include electricity, steam, and combustion gas. The system after removing combustible components such as hydrogen and carbon monoxide is the same as that shown in FIG. 1, and its explanation will be omitted.
以上説明したように、本発明によれば、圧縮機
の昇圧熱により原料空気を昇温して触媒反応さ
せ、水素及び一酸化炭素を含まない高純度の窒素
ガス製造方法および装置を提供することが出来
る。
As explained above, according to the present invention, there is provided a method and apparatus for producing high-purity nitrogen gas that does not contain hydrogen and carbon monoxide by raising the temperature of raw air using the heat of pressurization of a compressor and causing a catalytic reaction. I can do it.
第１図及び第２図は、夫々本発明の一実施例を
示す窒素製造装置の系統図であり、第３図は従来
の窒素精製装置の一例を示す系統図である。
１……フイルター、２……空気圧縮機、３……
触媒槽、４……冷却器、５……吸着塔、６……燃
交換器、７……精留塔、８……凝縮器、１１〜２
３……導管、３１……膨張弁。
FIGS. 1 and 2 are system diagrams of a nitrogen production apparatus showing one embodiment of the present invention, and FIG. 3 is a system diagram showing an example of a conventional nitrogen purification apparatus. 1... Filter, 2... Air compressor, 3...
Catalyst tank, 4... Cooler, 5... Adsorption tower, 6... Fuel exchanger, 7... Rectification column, 8... Condenser, 11-2
3... Conduit, 31... Expansion valve.
Claims (1)
原料空気の温度を触媒反応に適した90℃〜120℃
の温度まで昇温し、該昇温された原料空気を触媒
槽に導入し該触媒槽で原料空気中の水素及び精留
によつて窒素と分離が困難な一酸化炭素と酸素と
を反応・燃焼させ、該反応・燃焼で昇温した圧縮
された原料空気を常温まで冷却後原料空気中の不
純物である反応生成物を除去し、該不純物の除去
された原料空気から深冷分離により高純度の窒素
ガスを製造することを特徴とする窒素製造方法。 ２ 原料空気を圧縮する圧縮機と、該圧縮機で圧
縮されて触媒反応に適した90℃〜120℃の温度ま
で原料空気を昇温後導入し原料空気中の水素及び
精留によつて窒素と分離が困難な一酸化炭素と酸
素とを反応・燃焼させる触媒槽と、該触媒槽で反
応・燃焼後の圧縮された原料空気を冷却する冷却
器と、該冷却器で冷却された原料空気中の不純物
である反応生成物を除去する除去装置と、該除去
装置を経た原料空気から深冷分離により、高純度
の窒素ガスを製造する深冷分離装置とを具備した
ことを特徴とする窒素製造装置。 ３ 前記触媒反応に適した90℃〜120℃の温度ま
での原料空気の昇温は、圧縮機と触媒槽との間に
設けた過熱器で昇温させるように構成したことを
特徴とする特許請求の範囲第２記載の窒素製造装
置。[Scope of Claims] 1. Compress the raw air with an air compressor and adjust the temperature of the raw air to 90°C to 120°C, which is suitable for the catalytic reaction.
The temperature is raised to a temperature of The compressed raw air that has been heated through the reaction and combustion is cooled down to room temperature, then the reaction products that are impurities in the raw air are removed, and the raw air from which the impurities have been removed is purified by cryogenic separation. A method for producing nitrogen, characterized by producing nitrogen gas. 2. A compressor that compresses the feed air, and the feed air is compressed by the compressor and heated to a temperature of 90℃ to 120℃ suitable for catalytic reaction, and then introduced, and the hydrogen in the feed air and nitrogen are removed by rectification. a catalyst tank that reacts and burns carbon monoxide and oxygen, which are difficult to separate; a cooler that cools the compressed raw air after the reaction and combustion in the catalyst tank; and a cooler that cools the raw air cooled by the cooler. Nitrogen, characterized in that it is equipped with a removal device that removes reaction products that are impurities in nitrogen, and a cryogenic separation device that produces high-purity nitrogen gas by cryogenic separation from the raw air that has passed through the removal device. Manufacturing equipment. 3. A patent characterized in that the temperature of the feed air is raised to a temperature of 90°C to 120°C suitable for the catalytic reaction using a superheater installed between the compressor and the catalyst tank. A nitrogen production apparatus according to claim 2.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60063534A JPS61225568A (en) | 1985-03-29 | 1985-03-29 | air separation equipment |
| JP2012587A JPH0711384B2 (en) | 1985-03-29 | 1990-01-24 | Nitrogen production method and device |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP60063534A JPS61225568A (en) | 1985-03-29 | 1985-03-29 | air separation equipment |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP2012587A Division JPH0711384B2 (en) | 1985-03-29 | 1990-01-24 | Nitrogen production method and device |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS61225568A JPS61225568A (en) | 1986-10-07 |
| JPH0463993B2 true JPH0463993B2 (en) | 1992-10-13 |
Family
ID=13231976
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP60063534A Granted JPS61225568A (en) | 1985-03-29 | 1985-03-29 | air separation equipment |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPS61225568A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1137643A (en) * | 1997-07-18 | 1999-02-12 | Osaka Oxygen Ind Ltd | Air separation method and air separation device |
| JPH1190181A (en) * | 1997-09-24 | 1999-04-06 | Osaka Oxygen Ind Ltd | Air purifier |
| JPH1194458A (en) * | 1997-09-24 | 1999-04-09 | Osaka Oxygen Ind Ltd | Air separation equipment |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP3072992B2 (en) * | 1988-09-30 | 2000-08-07 | 株式会社日立製作所 | Method and apparatus for removing carbon monoxide with two-layer filling |
| JP2645137B2 (en) * | 1989-05-22 | 1997-08-25 | テイサン株式会社 | Equipment for purifying raw material air for nitrogen production equipment |
| JP2882917B2 (en) * | 1991-09-20 | 1999-04-19 | 株式会社日立製作所 | Toxic-resistant catalyst for combustible gas combustion, method for producing the same and method of using the catalyst |
| JP3306517B2 (en) * | 1992-05-08 | 2002-07-24 | 日本酸素株式会社 | Air liquefaction separation apparatus and method |
| JP3277340B2 (en) * | 1993-04-22 | 2002-04-22 | 日本酸素株式会社 | Method and apparatus for producing various gases for semiconductor manufacturing plants |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| IE37892B1 (en) * | 1972-07-31 | 1977-11-09 | Lilly Co Eli | Antibiotic a-2315 and process for preparation thereof |
| US3986778A (en) * | 1975-10-01 | 1976-10-19 | International Business Machines Corporation | Spectrophotometer sample holder |
-
1985
- 1985-03-29 JP JP60063534A patent/JPS61225568A/en active Granted
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH1137643A (en) * | 1997-07-18 | 1999-02-12 | Osaka Oxygen Ind Ltd | Air separation method and air separation device |
| JPH1190181A (en) * | 1997-09-24 | 1999-04-06 | Osaka Oxygen Ind Ltd | Air purifier |
| JPH1194458A (en) * | 1997-09-24 | 1999-04-09 | Osaka Oxygen Ind Ltd | Air separation equipment |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS61225568A (en) | 1986-10-07 |
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