JPH03230079A - Preparation of nitrogen gas - Google Patents
Preparation of nitrogen gasInfo
- Publication number
- JPH03230079A JPH03230079A JP32021390A JP32021390A JPH03230079A JP H03230079 A JPH03230079 A JP H03230079A JP 32021390 A JP32021390 A JP 32021390A JP 32021390 A JP32021390 A JP 32021390A JP H03230079 A JPH03230079 A JP H03230079A
- Authority
- JP
- Japan
- Prior art keywords
- nitrogen gas
- tower
- heat exchanger
- main heat
- supplied
- 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.)
- Granted
Links
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 title claims abstract description 247
- 229910001873 dinitrogen Inorganic materials 0.000 title claims abstract description 121
- 239000007788 liquid Substances 0.000 claims abstract description 61
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims abstract description 50
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 50
- 238000010992 reflux Methods 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims description 31
- 238000004519 manufacturing process Methods 0.000 claims description 31
- 239000007789 gas Substances 0.000 claims description 13
- 229910001882 dioxygen Inorganic materials 0.000 claims description 10
- 239000002994 raw material Substances 0.000 claims description 9
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 8
- 239000002912 waste gas Substances 0.000 claims description 7
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 4
- 239000001569 carbon dioxide Substances 0.000 claims description 4
- 239000012535 impurity Substances 0.000 claims description 4
- 238000005057 refrigeration Methods 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims 2
- 238000001816 cooling Methods 0.000 abstract description 12
- 238000004781 supercooling Methods 0.000 abstract description 7
- 238000010438 heat treatment Methods 0.000 abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 7
- 230000000694 effects Effects 0.000 description 7
- 229910052760 oxygen Inorganic materials 0.000 description 7
- 239000001301 oxygen Substances 0.000 description 7
- 230000006835 compression Effects 0.000 description 6
- 238000007906 compression Methods 0.000 description 6
- 239000000428 dust Substances 0.000 description 6
- 238000001035 drying Methods 0.000 description 5
- 238000003860 storage Methods 0.000 description 5
- 239000003990 capacitor Substances 0.000 description 4
- 239000000356 contaminant Substances 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 238000007796 conventional method Methods 0.000 description 3
- 230000008929 regeneration Effects 0.000 description 3
- 238000011069 regeneration method Methods 0.000 description 3
- 230000000630 rising effect Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 230000003749 cleanliness Effects 0.000 description 2
- 239000003245 coal Substances 0.000 description 2
- -1 moisture Substances 0.000 description 2
- 239000002808 molecular sieve Substances 0.000 description 2
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000011144 upstream manufacturing Methods 0.000 description 1
- 238000010792 warming Methods 0.000 description 1
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
- F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
- F25J3/04254—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using the cold stored in external cryogenic fluids
-
- 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
- F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
- F25J3/04284—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams
- F25J3/0429—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using internal refrigeration by open-loop gas work expansion, e.g. of intermediate or oxygen enriched (waste-)streams of feed air, e.g. used as waste or product air or expanded into an auxiliary column
-
- 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
- F25J3/04248—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion
- F25J3/04333—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams
- F25J3/04351—Generation of cold for compensating heat leaks or liquid production, e.g. by Joule-Thompson expansion using quasi-closed loop internal vapor compression refrigeration cycles, e.g. of intermediate or oxygen enriched (waste-)streams of nitrogen
-
- 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
- F25J3/04406—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 dual pressure main column system
- F25J3/0443—A main column system not otherwise provided, e.g. a modified double column flowsheet
-
- 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
- F25J2200/50—Processes or apparatus using separation by rectification using multiple (re-)boiler-condensers at different heights of the column
-
- 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
- F25J2210/00—Processes characterised by the type or other details of the feed stream
- F25J2210/42—Nitrogen
-
- 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
- F25J2245/00—Processes or apparatus involving steps for recycling of process streams
- F25J2245/40—Processes or apparatus involving steps for recycling of process streams the recycled stream being 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
- F25J2245/00—Processes or apparatus involving steps for recycling of process streams
- F25J2245/42—Processes or apparatus involving steps for recycling of process streams the recycled stream being nitrogen
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)
Abstract
Description
【発明の詳細な説明】
〔産業上の利用分野〕
本発明は、圧縮空気を原料とし、単式清潔塔により製品
窒素ガスを製造する窒素方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a nitrogen method for producing nitrogen product using a single clean tower using compressed air as a raw material.
この種の単式清潔塔利用の窒素ガス製造方法としては、
清潔塔の塔頂から取出した窒素ガスを主熱交換器の寒冷
源として使用したのち、この常温まで加温された窒素ガ
スを原料空気とほぼ同圧の低圧製品窒素ガスとして取出
す方法か知られている（例えば、特公昭５４−３９８３
０号公報）。This type of nitrogen gas production method using a single clean tower is as follows:
There is a known method in which the nitrogen gas taken out from the top of the clean tower is used as a cold source for the main heat exchanger, and then this nitrogen gas heated to room temperature is taken out as a low-pressure product nitrogen gas with almost the same pressure as the feed air. (For example, Special Publication No. 54-3983
Publication No. 0).
この従来方法による場合は、清潔塔の下部から供給され
る原料空気と清潔塔の上部から下降する還流液との接触
による分縮作用により、原料空気から窒素ガスを清潔分
離することができるのであるが、まだ、原料空気量に対
する窒素ガスの回収率は低く、現行の窒素ガス製造設備
における収率を見てみると、下記の表で示すように３７
％〜４８％程度の収率である。In the case of this conventional method, nitrogen gas can be cleanly separated from the feed air by the decomposition effect caused by the contact between the feed air supplied from the bottom of the clean tower and the reflux liquid descending from the top of the clean tower. However, the recovery rate of nitrogen gas relative to the amount of raw material air is still low, and looking at the yield in current nitrogen gas production equipment, it is 37% as shown in the table below.
The yield is about % to 48%.
収率表
そのため、窒素成分を多く含んだ不純液体酸素か清潔塔
底部の不純液体酸素溜部に下降して溜められるのである
が、この溜部内に不純液体酸素はそのまま外部に取出さ
れ、清潔塔の上部に設けられたコンデンサや主熱交換器
等の寒冷源として用いられた後、廃ガスとして放出され
ているのが現状である。Yield table For this reason, impure liquid oxygen containing a large amount of nitrogen components descends to the impure liquid oxygen reservoir at the bottom of the clean tower and is stored there.The impure liquid oxygen in this reservoir is directly taken out to the outside and is stored in the clean tower. Currently, after being used as a cold source for condensers and main heat exchangers installed at the top of the refrigerator, it is released as waste gas.
その上、この種の窒素ガス製造方法においては、エレク
トロニクス産業等で使用される中圧の窒素ガスを製造す
る場合、清潔塔の塔頂から取り出され、かつ、常温まで
加温された製品窒素ガスを中圧に圧縮する方法が採られ
ることがあるが、この圧縮時にゴミ粒子やその他の汚染
物質が混入する問題があった。Furthermore, in this type of nitrogen gas production method, when producing medium-pressure nitrogen gas used in the electronics industry, etc., the product nitrogen gas is taken out from the top of the clean tower and heated to room temperature. However, there is a problem in that dust particles and other contaminants get mixed in during this compression.
本発明の第１目的は、製品として取出される低圧の窒素
ガスを有効利用して、窒素ガスの収率を向上させ、単位
量当たりの製造コストの低廉化とを図ることのできる製
造方法を提供する点にあり、第２目的は、上述の第１目
的を達成しつつ清浄な中圧の製品窒素ガスを連続製造す
ることかできる製造方法を提供する点にある。The first object of the present invention is to provide a manufacturing method that can effectively utilize low-pressure nitrogen gas taken out as a product, improve the yield of nitrogen gas, and reduce the manufacturing cost per unit amount. The second object is to provide a production method that can continuously produce clean, medium-pressure product nitrogen gas while achieving the above-mentioned first object.
本第１発明による窒素ガス製造方法は、清潔塔の塔頂か
ら取出した窒素ガスを過冷却器、主熱交換器の寒冷源と
して使用して常温まで加温した後に、この窒素ガスの少
なくとも一部を圧縮した後、少なくともその一部を主熱
交換器に戻して液化点付近まで冷却し、清潔塔の底部の
不純液体酸素溜部に設けられたりボイラーの頂部に供給
して、不純液体酸素溜部内の不純液体酸素との熱交換に
より完全に液化した液体窒素をリボイラーの底部から取
出し、前記過冷却器で過冷却後、膨張させて清潔塔の上
部に還流液として供給すると共に、全工程中において別
途に寒冷を補給する点に特徴を有し、それによる作用・
効果は次の通りである。The method for producing nitrogen gas according to the first invention uses nitrogen gas taken out from the top of a clean tower as a cold source for a supercooler and a main heat exchanger to warm it to room temperature, and then at least part of the nitrogen gas is heated to room temperature. After compressing the part, at least a part of it is returned to the main heat exchanger to cool it to near the liquefaction point, and then it is placed in the impure liquid oxygen storage part at the bottom of the clean tower or supplied to the top of the boiler to make impure liquid oxygen. Liquid nitrogen, which has been completely liquefied by heat exchange with impure liquid oxygen in the reservoir, is taken out from the bottom of the reboiler, supercooled in the supercooler, expanded, and supplied to the top of the clean tower as a reflux liquid, and the entire process It is characterized by the fact that cold is supplied separately inside, and the effect and
The effects are as follows.
清潔塔の塔頂から取出される窒素ガスの寒冷エネルギー
を過冷却器及び主熱交換器での寒冷源として使用し、窒
素ガスを設定温度にまで加温する。この窒素ガスの少な
くとも一部を圧縮し、更に、その圧縮窒素ガスの少なく
とも一部を主熱交換で冷却したのち清潔塔底部のリポイ
ラーに供給する。このリボイラーでの窒素ガスと不純液
体酸素との熱交換により、不純液体酸素は加熱されると
共に、窒素ガスは完全に液化される。不純液体酸素の加
熱に伴って蒸発したガスは、清潔塔内を下降する液体窒
素（還流液）と向流状態で接触しなから上昇し、酸素は
液化して下降し、窒素に富むガスか上昇して清潔が行わ
れる。他方、液化された液体窒素はりボイラーの底部か
ら取出され、過冷却器で過冷却された後膨張され、原料
空気から窒素成分を分離する上で必要となる還流液とし
て清潔塔の上部に供給され、窒素ガス収率の一層の向上
に役立っている。The cold energy of the nitrogen gas taken out from the top of the clean tower is used as a cold source in the supercooler and main heat exchanger to heat the nitrogen gas to a set temperature. At least a portion of this nitrogen gas is compressed, and after being cooled by main heat exchange, at least a portion of the compressed nitrogen gas is supplied to a repoiler at the bottom of the clean tower. By heat exchange between the nitrogen gas and the impure liquid oxygen in this reboiler, the impure liquid oxygen is heated and the nitrogen gas is completely liquefied. The gas that evaporates as the impure liquid oxygen is heated rises without contacting the liquid nitrogen (reflux liquid) descending in the clean tower in a countercurrent state, and the oxygen liquefies and descends, forming a nitrogen-rich gas. Ascend and cleanse. On the other hand, liquefied liquid nitrogen is taken out from the bottom of the boiler, subcooled in a subcooler, expanded, and then supplied to the top of the clean tower as a reflux liquid necessary for separating nitrogen components from the feed air. , which helps further improve nitrogen gas yield.
従って、清潔塔の塔頂から取出される窒素ガスを過冷却
器及び主熱交換器での寒冷源として利用した後に窒素ガ
スを圧縮し、かつ、冷却してリボイラーに供給し、清潔
塔底部の不純液体酸素に対する加熱源として利用するこ
と、並びに、このリボイラーで液化した液体窒素を還流
液として利用することとの相乗により、従来の製造方法
に比して窒素ガスの収率向上、すなわち単位量当たりの
製造コストの低廉化とを図ることができるのである。Therefore, the nitrogen gas taken out from the top of the clean tower is used as a cold source in the subcooler and the main heat exchanger, and then the nitrogen gas is compressed, cooled, and supplied to the reboiler, and the nitrogen gas at the bottom of the clean tower is By combining the use of impure liquid oxygen as a heating source and the use of liquid nitrogen liquefied in this reboiler as a reflux liquid, the yield of nitrogen gas is improved compared to conventional production methods, i.e., the unit amount is increased. This makes it possible to reduce the per unit manufacturing cost.
尚、後述実施例で示すように、清潔塔の不純液体酸素溜
部と原料空気供給部との間に補助精溜部が設けられてい
る場合には、従来法に比べて清潔効率か向上し、製品窒
素ガスの収率を高めることができるから、単位量当たり
の製造コストの低廉化を一層促進することかできる。As shown in the examples below, if an auxiliary rectifying section is provided between the impure liquid oxygen storage section of the clean tower and the raw air supply section, the cleanliness efficiency will be improved compared to the conventional method. Since the yield of the product nitrogen gas can be increased, it is possible to further reduce the manufacturing cost per unit amount.
本第２発明による窒素ガス製造方法は、清潔塔の塔頂か
ら取出した窒素ガスを過冷却器、主熱交換器の寒冷源と
して使用して常温まで加温した後に、この窒素ガスの少
なくとも一部を圧縮した後、主熱交換器に戻して液化点
付近まで冷却し、清潔塔の底部に設けられた液体窒素洗
浄塔の下部に供給して塔の洗浄部内を上昇させ、洗浄塔
頂部に設けられたコンデンサで清潔塔底部の不純液体酸
素により冷却液化されて下降する液体窒素と向流状態で
接触させて不純物を洗浄除去した後、洗浄塔の塔頂から
取出し、再び主熱交換器で常温まで加温して清浄な製品
中圧窒素ガスとして取出し、洗浄塔の底部から取出され
た液体窒素は前記過冷却器で過冷却後、膨張させて清潔
塔の上部に還流液として供給すると共に、全工程中にお
いて別途に寒冷を補給する点に特徴を有し、それによる
作用・効果は次の通りである。In the method for producing nitrogen gas according to the second invention, at least part of the nitrogen gas is heated to room temperature using the nitrogen gas taken out from the top of the clean tower as a cold source for the supercooler and the main heat exchanger. After compressing the liquid nitrogen, it is returned to the main heat exchanger and cooled to near the liquefaction point, and then supplied to the lower part of the liquid nitrogen cleaning tower installed at the bottom of the clean tower, rising inside the cleaning section of the tower, and reaching the top of the cleaning tower. It is cooled and liquefied by the impure liquid oxygen at the bottom of the clean tower in the provided condenser and brought into contact with the descending liquid nitrogen in a countercurrent state to wash and remove impurities, and then taken out from the top of the cleaning tower and returned to the main heat exchanger. The liquid nitrogen taken out from the bottom of the cleaning tower is subcooled in the supercooler, expanded, and supplied to the top of the clean tower as a reflux liquid. , is characterized in that cold is separately supplied during the entire process, and the effects and effects thereof are as follows.
清潔塔の塔頂から取出される低圧窒素ガスの寒冷エネル
ギーを過冷却器及び主熱交換器での寒冷源として使用し
、窒素ガスを常温にまで加温する。この窒素ガスの少な
くとも一部を圧縮し、主熱交換器で冷却した後、清潔塔
の底部に設けられた液体窒素洗浄塔の下部に供給する。The cold energy of the low-pressure nitrogen gas taken out from the top of the clean tower is used as a cold source in the supercooler and main heat exchanger to warm the nitrogen gas to room temperature. At least a portion of this nitrogen gas is compressed, cooled in a main heat exchanger, and then supplied to the lower part of a liquid nitrogen cleaning tower provided at the bottom of the clean tower.
この洗浄塔内に供給された窒素ガスは上昇して洗浄塔頂
部のコンデンサ内て清潔塔底部の不純液体酸素と熱交換
され、窒素ガスの一部は凝縮して液体窒素として下降す
る。この液体窒素と洗浄塔の下部に供給される窒素ガス
とか向流状態で接触し、圧縮時に混入した窒素ガス中の
ゴミ粒子やその他の汚染物質が液体窒素にて洗浄除去さ
れる。他方、不純液体酸素は加熱され、この加熱に伴っ
て蒸発したガスは、清潔塔内を下降する液体窒素（還流
液）と向流状態で接触しなから上昇し、酸素は液化して
下降し、窒素に富むガスが上昇して清潔が行われる。The nitrogen gas supplied into the cleaning tower rises and exchanges heat with impure liquid oxygen at the bottom of the clean tower in a condenser at the top of the cleaning tower, and a portion of the nitrogen gas condenses and descends as liquid nitrogen. This liquid nitrogen and nitrogen gas supplied to the lower part of the cleaning tower come into contact with each other in a countercurrent state, and dust particles and other contaminants in the nitrogen gas mixed in during compression are washed and removed by the liquid nitrogen. On the other hand, the impure liquid oxygen is heated, and the gas that evaporates as a result of this heating comes into contact with the liquid nitrogen (reflux liquid) descending in the clean tower in a countercurrent state and rises, and the oxygen liquefies and descends. , nitrogen-rich gas rises and cleansing takes place.
前記洗浄塔の頂部から取出される洗浄後の中圧窒素ガス
は主熱交換器での寒冷源として使用されたのち、清浄な
製品中圧窒素ガスとして取出される。The washed medium pressure nitrogen gas taken out from the top of the washing tower is used as a cooling source in the main heat exchanger and then taken out as a clean product medium pressure nitrogen gas.
又、洗浄塔の底部から取出された液体窒素は、過冷却器
で過冷却された後膨張され、原料空気から窒素成分を清
潔分離する上で必要となる還流液として清潔塔の上部に
供給されるので、窒素ガス収率の一層の向上に役立って
いる。In addition, the liquid nitrogen taken out from the bottom of the cleaning tower is supercooled in a supercooler, expanded, and then supplied to the top of the cleaning tower as a reflux liquid that is necessary for cleanly separating nitrogen components from the raw air. This helps further improve nitrogen gas yield.
従って、清潔塔の塔頂から取出される低圧窒素ガスを過
冷却器及び主熱交換器での寒冷源として利用した後に圧
縮し、かつ、冷却して洗浄塔の下部からその頂部のコン
デンサに供給し、清潔塔底部の不純液体酸素に対する加
熱源として利用することと、洗浄塔の塔頂から取出され
る中圧窒素ガスを主熱交換器での寒冷源としてそれぞれ
利用すること、並びに、この洗浄塔で液化した液体窒素
を清潔塔での還流液として利用することとの相乗により
、従来の製造方法に比して窒素ガスの収率向上と単位量
当たりの製造コストの低廉化とを図ることかできる。し
かも、洗浄塔内での液体窒素と窒素ガスとの向流状態で
の接触により、圧縮時に混入した窒素ガス中のゴミ粒子
やその他の汚染物質を洗浄除去することができるから、
清浄な中圧の製品窒素ガスを連続製造することができる
のである。Therefore, the low-pressure nitrogen gas taken out from the top of the cleaning tower is used as a cold source in the supercooler and main heat exchanger, and then compressed, cooled, and supplied from the bottom of the cleaning tower to the condenser at the top. In addition, the cleaning tower uses medium-pressure nitrogen gas taken out from the top of the cleaning tower as a cooling source for the main heat exchanger. By synergistically using the liquid nitrogen liquefied in the tower as the reflux liquid in the clean tower, we aim to improve the yield of nitrogen gas and lower the manufacturing cost per unit amount compared to conventional production methods. I can do it. Moreover, the countercurrent contact between liquid nitrogen and nitrogen gas in the cleaning tower makes it possible to wash and remove dust particles and other contaminants from the nitrogen gas mixed in during compression.
It is possible to continuously produce clean, medium-pressure product nitrogen gas.
尚、後述実施例で示すように、清潔塔の不純液体酸素溜
部と原料空気供給部との間に補助精溜部が設けられてい
る場合には、従来法に比べて清潔効率か向上し、製品窒
素ガスの収率を高めることができるから、単位量当たり
の製造コストの低廉化を一層促進することかできる。As shown in the examples below, if an auxiliary rectifying section is provided between the impure liquid oxygen storage section of the clean tower and the raw air supply section, the cleanliness efficiency will be improved compared to the conventional method. Since the yield of the product nitrogen gas can be increased, it is possible to further reduce the manufacturing cost per unit amount.
先ず、本第１発明による窒素ガス製造方法を第１図に基
づいて説明する。First, the method for producing nitrogen gas according to the first invention will be explained based on FIG.
空気濾過器（図示せず）て除塵された原料空気（ＧＡ）
を圧縮機（１）で空気分離運転に必要な圧力（例エバ、
４．７ｋｇ／ａＩｒＧ） マで圧縮シタ後、コノ圧縮原
料空気（ＧＡ）を配管（Ｐｌ）を通して冷却・除炭・乾
燥ユニット（２）に供給する。この冷却・除炭・乾燥ユ
ニット（２）では、圧縮原料空気（ＧＡ）をアフターク
ーラで常温まで冷却したのち、冷凍設備により約５℃ま
で冷却し、さらに、二基よりなるモレキュラーシーブ塔
のうちの一方に供給し、原料空気（ＧＡ）中の炭酸ガス
及び水分を吸着除去する。その間、他方のモレキュラー
シーブ塔には後述の主熱交換器（３）を通過した廃ガス
（不純酸素ガス）を供給して再生する。Raw air (GA) from which dust has been removed using an air filter (not shown)
The pressure required for air separation operation in the compressor (1) (e.g. Eva,
4.7kg/aIrG) After being compressed by a machine, the compressed raw air (GA) is supplied to the cooling/carburization/drying unit (2) through the piping (Pl). In this cooling/carburization/drying unit (2), compressed feed air (GA) is cooled to room temperature in an aftercooler, then cooled to approximately 5°C in a refrigeration equipment, and then is supplied to one side of the feed air (GA) to adsorb and remove carbon dioxide and moisture in the raw air (GA). Meanwhile, waste gas (impure oxygen gas) that has passed through the main heat exchanger (3), which will be described later, is supplied to the other molecular sieve column for regeneration.
この冷却・除炭・乾燥ユニット（２）で炭酸ガス、水分
、その他不純物を除去された原料空気（ＧＡ）を配管（
Ｐ２）を通して主熱交換器（３）に供給し、液化点付近
まで冷却した後、配管（Ｐ３）を通して清潔塔（４）下
部の原料空気供給部（４ａ）に供給する。又、この清潔
塔（４）の上部に、寒冷源の一例である液体窒素（ＬＮ
２）を配管（Ｐ４）を通して供給し、清潔塔（４）内の
主精溜部（４ｂ）において、下部から上昇する原料空気
（ＧＡ）と清潔塔（４）内の上部から下降する液体窒素
（還流液）とを向流状態で接触させ、原料空気（ＧＡ）
から酸素を液化させて窒素ガス（ＧＮ２）を清潔分離す
る。The raw air (GA) from which carbon dioxide, moisture, and other impurities have been removed by this cooling/carburization/drying unit (2) is piped (
After being supplied to the main heat exchanger (3) through P2) and cooled to near the liquefaction point, it is supplied to the raw air supply section (4a) at the bottom of the clean tower (4) through piping (P3). In addition, liquid nitrogen (LN), which is an example of a cold source, is installed at the top of the clean tower (4).
2) is supplied through the pipe (P4), and in the main rectification section (4b) in the clean tower (4), raw air (GA) rising from the bottom and liquid nitrogen descending from the top in the clean tower (4) are mixed. (reflux liquid) in a countercurrent state, and feed air (GA)
Oxygen is liquefied and nitrogen gas (GN2) is cleanly separated.
前記清潔塔（４）の塔頂から取出した窒素ガス（ＧＮ２
）を配管（Ｐ、）を通して過冷却器（５）に、さらに、
配管（Ｐ、）を通して主熱交換器（３）に供給し、窒素
ガス（ＧＮ２）の寒冷エネルギーを過冷却器（５）及び
主熱交換器（３）での寒冷源として使用すると共に、窒
素ガス（ＧＮ２）を常温にまで加温する。この主熱交換
器（３）から低圧製品窒素ガス用配管（Ｐ７）を通して
取出される常温窒素ガス（ＧＮ２）の少なくとも一部を
配管（Ｐ、）を通して圧縮機（６）に供給し、原料空気
（ＧＡ）とほぼ同圧の低圧製品窒素ガス（ＧＮ２Ｘ例え
ば、４．０ｋｇ／ｃｎｌ’Ｇ）を中圧（例えば、９．Ｏ
ｋｇ／ｃｎｒＧ）にまで圧縮する。Nitrogen gas (GN2) taken out from the top of the clean tower (4)
) to the supercooler (5) through the pipe (P, ), and
Nitrogen gas (GN2) is supplied to the main heat exchanger (3) through the pipe (P,), and the cold energy of the nitrogen gas (GN2) is used as a cold source in the supercooler (5) and the main heat exchanger (3). Heat the gas (GN2) to room temperature. At least a part of the normal temperature nitrogen gas (GN2) taken out from the main heat exchanger (3) through the low-pressure product nitrogen gas pipe (P7) is supplied to the compressor (6) through the pipe (P,), and the raw material (GA) and a low pressure product nitrogen gas (GN2
kg/cnrG).
前記圧縮機（６）から中圧製品窒素ガス用配管（Ｐ９）
を通して取出される圧縮窒素ガスの少なくとも一部を配
管（ｈ。）を通して主熱交換器（３）に戻し、液化点付
近にまで冷却した後、配管（ＰＩ、）を通して清潔塔（
４）底部の不純液体酸素溜部（４ｃ）内に設けられたり
ボイラー（７）の頂部に供給する。このリボイラー（７
）での窒素ガス（ＧＮ２）と不純液体酸素（ＬＯ□）と
の熱交換により、不純液酸素（１，０２）は加熱される
と共に、窒素ガス（ＧＮ２）は完全に液化される。Medium pressure product nitrogen gas pipe (P9) from the compressor (6)
At least a part of the compressed nitrogen gas taken out through the pipe (h.) is returned to the main heat exchanger (3) through the pipe (h.), and after being cooled to near the liquefaction point, it is passed through the pipe (PI,) to the clean tower (
4) Provided in the impure liquid oxygen reservoir (4c) at the bottom or supplied to the top of the boiler (7). This reboiler (7
), the impure liquid oxygen (1,02) is heated and the nitrogen gas (GN2) is completely liquefied by the heat exchange between the nitrogen gas (GN2) and the impure liquid oxygen (LO□).
この不純液体酸素（ＬＯ□）の加熱に伴って蒸発したガ
スは、清潔塔（４）の、原料空気供給部（４ａ）と不純
液体酸素溜部（４Ｃ）との間に介在された補助精溜部（
４ｄ）を通して清潔塔（４）の上部に上昇し、清潔塔（
４）内を下降する液体窒素（還流液）と向流状態で接触
して、酸素は液化して下降し、窒素に富むガスが上流し
て清潔か行われる。このような補助精溜部（４ｄ）及び
主精溜部（４ｂ）での２段清潔作用により、窒素ガス（
ＧＮ２）の収率を向上することかできる。The gas evaporated with the heating of this impure liquid oxygen (LO Tamabe (
4d) to the top of the clean tower (4), and go up to the top of the clean tower (4).
4) In countercurrent contact with liquid nitrogen (reflux liquid) descending inside, the oxygen liquefies and descends, and the nitrogen-rich gas flows upstream for cleaning. Due to the two-stage cleaning action in the auxiliary rectifying section (4d) and the main rectifying section (4b), nitrogen gas (
The yield of GN2) can be improved.
前記リボイラー（７）の底部から配管（Ｐ、２）を通し
て取出された液体窒素（ＬＮ２）を過冷却器（５）に供
給し、液体窒素（ＬＮ２）を過冷却した後、膨張弁（８
）を有する配管（Ｐ、３）に導き、膨張させて清潔塔（
４）の上部に還流液として供給する。Liquid nitrogen (LN2) taken out from the bottom of the reboiler (7) through the pipe (P, 2) is supplied to the supercooler (5), and after supercooling the liquid nitrogen (LN2), the expansion valve (8
) into the pipe (P, 3), which is expanded to form a clean tower (
4) is supplied as a reflux liquid to the upper part of step 4).
又、前記清潔塔（４）の不純液体酸素溜部（４ｃ）の下
部から取出された不純液体酸素（ｌＯ２）を配管（Ｐ、
、）を通して過冷却器（５）に供給し、不純液体酸素（
ｌＯ２）を過冷却した後、膨張弁（９）を有する配管（
Ｐ、５）に導き、膨張させて清潔塔（４）の上部に設け
られたコンデンサ（１０）に供給する。In addition, impure liquid oxygen (lO2) taken out from the lower part of the impure liquid oxygen storage section (4c) of the clean tower (4) is transferred to a pipe (P,
, ) to the supercooler (5) and impure liquid oxygen (
After supercooling the lO2), the pipe with the expansion valve (9)
P, 5), expanded and supplied to the condenser (10) provided at the top of the clean tower (4).
このコンデンサ（ｌＯ）内で減圧蒸発される不純液体酸
素（ＬＯ□）と清潔塔（４）内の上部に存在する低温窒
素ガス（ＧＮ２）とが熱交換され、低温窒素ガス（ＧＮ
２）の一部が液化されて還流液として下降する。The impure liquid oxygen (LO□) evaporated under reduced pressure in this condenser (1O) and the low temperature nitrogen gas (GN2) present in the upper part of the clean tower (4) exchange heat, and the low temperature nitrogen gas (GN2) is heated.
A part of 2) is liquefied and descends as a reflux liquid.
前記コンデンサ（１０）で蒸発した不純酸素ガス（ＧＯ
２）を配管（Ｐ、６）を通して過冷却器（５）に、さら
に、配管（Ｐ＋７）を通して主熱交換器（３）に供給し
、不純酸素ガス（ＧＯ□）の寒冷エネルギーを過冷却器
（５）及び主熱交換器（３）での寒冷源として使用する
。この寒冷放出に伴って常温まで加温された不純酸素ガ
スの廃ガス（ＧＯ□）は配管（Ｐ、、）を通して冷却・
給炭・乾燥ユニット（２）の非使用のモレキュラーシー
ブ塔に供給され、再生ガスとして使用された後外部に放
出される。Impure oxygen gas (GO) evaporated in the condenser (10)
2) is supplied to the supercooler (5) through the pipe (P, 6), and then to the main heat exchanger (3) through the pipe (P+7), and the cold energy of the impure oxygen gas (GO□) is transferred to the supercooler. (5) and as a cold source in the main heat exchanger (3). The impure oxygen gas waste gas (GO
The gas is supplied to an unused molecular sieve tower in the coal supply/drying unit (2), used as regeneration gas, and then discharged to the outside.
製品窒素ガス（ＧＮ２）としての取出し方には、バルブ
制御により次の３通りがある。There are three ways to take out the product nitrogen gas (GN2) using valve control:
（イ）前記主熱交換器（３）で常温まで加温された窒素
ガス（ＧＮ２）の所要量を原料空気（ＧＡ）とほぼ同圧
の低圧製品窒素ガス（ＧＮ２）として取出し、残部を圧
縮後に主熱交換器（３）へ戻す方法。(b) The required amount of nitrogen gas (GN2) heated to room temperature in the main heat exchanger (3) is taken out as a low-pressure product nitrogen gas (GN2) with approximately the same pressure as the raw material air (GA), and the remainder is compressed. How to return it to the main heat exchanger (3) later.
（０）前記主熱交換器（３）で常温まで加温された窒素
ガス（ＧＮ２）を圧縮し、その所要量を中圧製品窒素ガ
ス（ＧＮ２）として取出し、残部を主熱交換器（３）へ
戻す方法。(0) The nitrogen gas (GN2) heated to room temperature in the main heat exchanger (3) is compressed, the required amount is taken out as medium pressure product nitrogen gas (GN2), and the remainder is transferred to the main heat exchanger (3). ).
（ハ）前記主熱交換器（３）で常温まで加温された窒素
ガス（ＧＮ２）の所要量を原料空気（ＧＡ）とほぼ同圧
の低圧製品窒素ガス（ＧＮ２）として取出し、残部を圧
縮後さらにその所要量を中圧製品窒素ガス（ＧＮ２）と
して取出し、その残部を主熱交換器（３）へ戻す方法。(c) The required amount of nitrogen gas (GN2) heated to room temperature in the main heat exchanger (3) is taken out as a low-pressure product nitrogen gas (GN2) with approximately the same pressure as the feed air (GA), and the remainder is compressed. Then, the required amount is taken out as intermediate pressure product nitrogen gas (GN2), and the remainder is returned to the main heat exchanger (3).
尚、上記実施例では、全工程中において別途に寒冷を補
給する方法として、外部から清潔塔（４）の上部に液体
窒素（ＬＮ２）を供給したが、この補給方法に限定され
るものではなく、例えば、第２図に示すように、前記主
熱交換器（３）の原料空気供給系の中間から配管（Ｐ、
）を通して取出された一部の原料空気（ＧＡ）を膨張タ
ービン（１１）で断熱膨張した後、この膨張タービン（
１１）から配管（Ｐ２゜）を通して取出される寒冷の原
料空気（ＧＡ）を過冷却器（５）を通過した廃ガス（不
純酸素ガス）系の配管（Ｐ、７）に合流させ、もって、
この原料空気（ＧＡ）の一部を主熱交換器（３）の寒冷
源として補給してもよい。In the above example, liquid nitrogen (LN2) was supplied from the outside to the top of the clean tower (4) as a method of separately replenishing cold during the entire process, but the method is not limited to this replenishment method. For example, as shown in FIG. 2, a pipe (P,
) A part of the raw air (GA) taken out through the expansion turbine (11) is adiabatically expanded, and then the expansion turbine (
The cold raw material air (GA) taken out from 11) through the pipe (P2°) is joined to the waste gas (impure oxygen gas) system pipe (P, 7) that has passed through the supercooler (5), and thereby,
A part of this raw air (GA) may be supplied as a cooling source for the main heat exchanger (3).
次に、本第２発明による窒素ガス製造方法を第３図に基
づいて説明する。Next, a method for producing nitrogen gas according to the second invention will be explained based on FIG. 3.
空気濾過器（図示せず）で除塵された原料空気（ＧＡ）
を圧縮機（１）で空気分離運転に必要な圧力（例えば、
４．７ ｋｇ／ａｌＧ）まで圧縮した後、この圧縮原料
空気（ＧＡ”）を配管（Ｐ＋）を通して冷却・給炭・乾
燥ユニット（２）に供給する。Raw air (GA) from which dust has been removed by an air filter (not shown)
The pressure required for air separation operation in the compressor (1) (for example,
After being compressed to 4.7 kg/alG), this compressed raw air (GA'') is supplied to the cooling/coal feeding/drying unit (2) through the pipe (P+).
この冷却・給炭・乾燥ユニット（２）で炭酸ガス、水分
、その他不純物を除去された原料空気（ＧＡ）を配管（
Ｐ２）を通して主熱交換器（３）に供給し、液化点付近
まで冷却した後、配管（Ｐ３）を通して清潔塔（４）下
部の原料空気供給部（４ａ）に供給する。又、この清潔
塔（４）の上部に、寒冷源の一例である液体窒素（ＬＮ
２）を配管（Ｐ４）を通して供給し、清潔塔（４）内の
主精溜部（４ｂ）において、下部から上昇する原料空気
と清潔塔（４）内の上部から下降する液体窒素（還流液
）とを向流状態で接触させ、原料空気（ＧＡ）から酸素
を液化させて窒素ガスを積属分離する。The raw air (GA) from which carbon dioxide, moisture, and other impurities have been removed is piped (
After being supplied to the main heat exchanger (3) through P2) and cooled to near the liquefaction point, it is supplied to the raw air supply section (4a) at the bottom of the clean tower (4) through piping (P3). In addition, liquid nitrogen (LN), which is an example of a cold source, is installed at the top of this clean tower (4).
2) is supplied through the pipe (P4), and in the main rectification section (4b) in the clean tower (4), raw air rising from the bottom and liquid nitrogen (reflux liquid) descending from the top in the clean tower (4) ) in a countercurrent state to liquefy oxygen from raw air (GA) and separate nitrogen gas.
前記清潔塔（４）の塔頂から取出した窒素ガス（ＧＮ２
）を配管（ｐｇ）を通して過冷却器（５）に、さらに配
管（Ｐ６）を通して主熱交換器（３）に供給し、窒素ガ
ス（ＧＮ２）の寒冷エネルギーを過冷却器（５）及び主
熱交換器（３）での寒冷源として使用すると共に、窒素
ガス（ＧＮ２）を常温にまで加温する。Nitrogen gas (GN2) taken out from the top of the clean tower (4)
) is supplied to the supercooler (5) through the pipe (pg), and further to the main heat exchanger (3) through the pipe (P6), and the cold energy of nitrogen gas (GN2) is supplied to the supercooler (5) and the main heat exchanger (3) through the pipe (P6). It is used as a cold source in the exchanger (3) and also heats nitrogen gas (GN2) to room temperature.
この主熱交換器（３）から配管（Ｐ２． ）を通して取
出される常温窒素ガスを圧縮機（６）に供給し、原料空
気（ＧＡ）とほぼ同圧の窒素ガス（ＧＮ２Ｘ例えば、４
．０ｋｇ／ＣｄＧ）を中圧（例えば、９．０ｋｇ／ｃｎ
ｒＧ）にまで圧縮する。Room-temperature nitrogen gas taken out from this main heat exchanger (3) through piping (P2.) is supplied to the compressor (6), and the nitrogen gas (GN2X, for example, 4
．． 0kg/CdG) to medium pressure (for example, 9.0kg/cn
rG).
前記圧縮機（６）から取出される圧縮窒素ガスを配管（
Ｐ２２）を通して主熱交換器（３）に戻し、液化点付近
まで冷却した後、配管（Ｐ２３）を通して清潔塔（４）
の底部に設けられた液体窒素洗浄塔（１２）の下部に供
給する。この洗浄塔（１２）内に供給された窒素ガス（
ＧＮ２）は、洗浄部（１２ａ）を上昇して、洗浄塔（１
２）の頂部の、清潔塔（４）底部の不純液体酸素溜部（
４ｃ）内に位置する状態で設けられたコンデンサ（１２
ｂ）で不純液体酸素（ＬＯ□）と熱交換され、窒素ガス
（ＧＮ２）の一部は凝縮して液体窒素（ＬＮ２）として
下降する。この液体窒素（ＬＮ２）と洗浄塔（１２）の
下部に供給される窒素ガス（ＧＮ２）とか洗浄部（１２
ａ）において向流状態で接触し、圧縮時に混入した窒素
ガス（ＧＮ２）中のゴミ粒子やその他の汚染物質か液体
窒素（ＬＮ２）にて洗浄除去される。The compressed nitrogen gas taken out from the compressor (6) is piped (
After returning to the main heat exchanger (3) through the pipe (P22) and cooling it to near the liquefaction point, it is returned to the clean tower (4) through the pipe (P23).
The liquid nitrogen is supplied to the lower part of the liquid nitrogen cleaning tower (12) provided at the bottom of the tank. Nitrogen gas (
GN2) ascends through the cleaning section (12a) and enters the cleaning tower (1
2), the impure liquid oxygen reservoir (4) at the bottom of the clean tower (4)
capacitor (12) located within the capacitor (12)
In b), heat is exchanged with impure liquid oxygen (LO□), and a portion of the nitrogen gas (GN2) condenses and descends as liquid nitrogen (LN2). This liquid nitrogen (LN2) and nitrogen gas (GN2) supplied to the lower part of the cleaning tower (12) and the cleaning section (12)
In a), they are brought into contact in a countercurrent state, and dust particles and other contaminants in the nitrogen gas (GN2) mixed during compression are washed away with liquid nitrogen (LN2).
他方、不純液体酸素（ＬＯ□）は加熱され、この加熱に
伴って蒸発したガスは、清潔塔（４）の、原料空気供給
部（４ａ）と不純液体酸素溜部（４ｃ）との間に介在さ
れた補助精溜部（４ｄ）を通して清潔塔（４）の上部に
上昇し、清潔塔（４）内を下降する液体窒素（還流液）
と向流状態で接触して、酸素は液化して下降し、窒素に
富むガスか上昇して清瀬か行われる。このような補助精
溜部（４ｄ）及び主精溜部（４ｂ）での２段清潔分離作
用により、窒素ガスの収率を向上することかできる。On the other hand, the impure liquid oxygen (LO□) is heated, and the gas evaporated due to this heating is transferred between the raw air supply section (4a) and the impure liquid oxygen storage section (4c) of the clean tower (4). Liquid nitrogen (reflux liquid) rises to the top of the clean tower (4) through the interposed auxiliary rectification section (4d) and descends inside the clean tower (4).
In countercurrent contact with the oxygen, the oxygen liquefies and descends, while the nitrogen-rich gas rises and clears. Such two-stage clean separation action in the auxiliary rectifying section (4d) and the main rectifying section (4b) can improve the yield of nitrogen gas.
前記洗浄塔（１２）の頂部から配管（Ｐ２４）を通して
取出される洗浄後の中圧窒素ガス（ＧＮ２）を主熱交換
器（３）に供給し、この中圧窒素ガス（ＧＮ２）の寒冷
エネルギーを主熱交換器（３）での寒冷源として使用す
ると共に、中圧窒素ガス（ＧＮ２）を常温にまで加温し
た後、この主熱交換器（３）から配管（Ｐ２．）を通し
て清浄な製品中圧窒素ガスを取出す。The washed medium pressure nitrogen gas (GN2) taken out from the top of the washing tower (12) through the pipe (P24) is supplied to the main heat exchanger (3), and the cold energy of this medium pressure nitrogen gas (GN2) is is used as a cold source in the main heat exchanger (3), and after warming the medium pressure nitrogen gas (GN2) to room temperature, a clean Take out medium pressure nitrogen gas from the product.
又、洗浄塔（１２）の底部から配管（Ｐ、□）を通して
取出された液体窒素（ＬＮ２）を過冷却器（５）に供給
し、液体窒素（ＬＮ２）を過冷却した後、膨張弁（８）
を存する配管（Ｐ、、）に導き、膨張−させて清潔塔（
４）の上部に還流液として供給する。In addition, liquid nitrogen (LN2) taken out from the bottom of the cleaning tower (12) through the pipe (P, □) is supplied to the supercooler (5), and after supercooling the liquid nitrogen (LN2), the expansion valve ( 8)
is introduced into the existing piping (P, , ) and expanded to form a clean tower (
4) is supplied as a reflux liquid to the upper part of step 4).
前記清潔塔（４）の不純液体酸素溜部（４Ｃ）の下部か
ら取出された不純液体酸素（ＬＯ□）を配管（Ｐ、、）
を通して過冷却器（５）に供給し、不純液体酸素（ＬＯ
２）を過冷却した後、膨張弁（９）を有する配管（Ｐ、
５）に導き、膨張させて清潔塔（４）の上部に設けられ
たコンデンサ（１０）に供給する。The impure liquid oxygen (LO□) taken out from the lower part of the impure liquid oxygen reservoir (4C) of the clean tower (4) is piped (P,,)
Impure liquid oxygen (LO
2), the pipe (P,
5), expanded and supplied to the condenser (10) provided at the top of the clean tower (4).
このコンデンサ（１０）内で減圧蒸発される不純液体酸
素（ＬＯ□）と清潔塔（４）内の上部に存在する低温窒
素ガス（ＧＮ２）とが熱交換され、低温窒素ガス（ＧＮ
２）の一部が液化されて還流液として下降する。The impure liquid oxygen (LO□) evaporated under reduced pressure in the condenser (10) and the low-temperature nitrogen gas (GN2) present in the upper part of the clean tower (4) exchange heat, and the low-temperature nitrogen gas (GN2)
A part of 2) is liquefied and descends as a reflux liquid.
前記コンデンサ（１０）で蒸発した不純酸素ガス（ＧＯ
２）を配管（ｐｅｇ）を通して過冷却器（５）に、さら
に、配管（Ｐ、、）を通して主熱交換器（３）に供給し
、不純酸素ガス（ＧＯ２）の寒冷エネルギーを過冷却器
（５）及び主熱交換器（３）での寒冷源として使用する
。この寒冷放出に伴って常温まで加温された不純酸素ガ
スの廃ガス（ＧＯ□）は、配管（Ｐ＋−）を通して冷却
・給炭・乾燥ユニット（２）の非使用のモレキュラーシ
ーブ塔に供給され、再生ガスとして使用された後、外部
に放出される。Impure oxygen gas (GO) evaporated in the condenser (10)
2) is supplied to the supercooler (5) through the piping (peg), and further to the main heat exchanger (3) through the piping (P, ,), and the cold energy of the impure oxygen gas (GO2) is transferred to the supercooler ( 5) and as a cold source in the main heat exchanger (3). The impure oxygen gas waste gas (GO , used as regeneration gas and then released to the outside.
尚、上述の第２発明の実施例では、前記主熱交換器（３
）で最初に常温まで加温された窒素ガス（ＧＮ２）の全
てを圧縮して主熱交換器（３）に戻し、清浄な中圧窒素
ガスのみを製品として取出したが、この製造方法に限定
されるものではなく、例えば、主熱交換器（３）で最初
に常温まで加温された窒素ガス（ＧＮ２）の一部を原料
空気（ＧＡ）とほぼ同圧の低圧製品窒素ガスとして取出
し、残部を圧縮して主熱交換器（３）へ戻し、清浄な中
圧製品窒素ガスとして取出すようにしてもよい。In addition, in the embodiment of the second invention described above, the main heat exchanger (3
) All of the nitrogen gas (GN2) that was first heated to room temperature was compressed and returned to the main heat exchanger (3), and only clean medium-pressure nitrogen gas was extracted as a product, but this production method was limited. For example, a part of the nitrogen gas (GN2) that is first heated to room temperature in the main heat exchanger (3) is taken out as a low-pressure product nitrogen gas with approximately the same pressure as the raw material air (GA), The remainder may be compressed and returned to the main heat exchanger (3) and removed as a clean intermediate pressure product nitrogen gas.
又、上述の第２発明の実施例では、全工程中において別
途に寒冷を補給する方法として、外部から清潔塔（４）
の上部に液体窒素（ＬＮ２）を供給したが、この補給方
法に限定されるものではなく、例えば、第４図に示すよ
うに、前記主熱交換器（３）の、原料空気供給系の中間
か−ら配管（Ｐ、、）を通して取出された一部の原料空
気（ＧＡ）を膨張タービン（１１）で断熱膨張した後、
この膨張タービン（１１）から配管（Ｐ、ｏ）を通して
取出される寒冷の原料空気を過冷却器（５）を通過した
廃ガス（不純酸素ガス）系の配管（Ｐ、□）に合流させ
、もって、この原料空気（ＧＡ）の一部を主熱交換器（
３）の寒冷源として補給してもよい。In addition, in the above-mentioned embodiment of the second invention, as a method of separately supplying cold during the entire process, the clean tower (4) is supplied from the outside.
Although liquid nitrogen (LN2) is supplied to the upper part of the main heat exchanger (3), it is not limited to this replenishment method. For example, as shown in FIG. A part of the raw air (GA) taken out from the pipe (P, , ) is adiabatically expanded in the expansion turbine (11), and then
The cold raw material air taken out from the expansion turbine (11) through the pipe (P, o) is joined to the pipe (P, □) of the waste gas (impure oxygen gas) system that has passed through the supercooler (5), With this, a part of this raw air (GA) is transferred to the main heat exchanger (
It may be supplied as a cold source in 3).
更に、上述の各実施例では、原料空気を圧縮する圧縮機
（１）と、主熱交換器（３）で最初に常温まで加温され
た窒素ガスを圧縮する圧縮機（６）との二つの圧縮機を
使用した製造方法について説明したが、これに限定され
るものではない。Furthermore, in each of the above-mentioned embodiments, two compressors are used: a compressor (1) that compresses the raw material air, and a compressor (6) that compresses the nitrogen gas that is first heated to room temperature in the main heat exchanger (3). Although the manufacturing method using two compressors has been described, the present invention is not limited to this.
つまり、これら二つの圧縮機（１）、 （６）の圧力レ
ベルを考慮すると、同一の圧縮機の低圧段を原料空気圧
縮用に、そして又高圧段を窒素ガス圧縮用にそれぞれ使
用することにより、一つの圧縮機を用いて兼用すること
もできる。In other words, considering the pressure levels of these two compressors (1) and (6), it is possible to use the same compressor's low pressure stage for raw air compression and the high pressure stage for nitrogen gas compression. , it is also possible to use one compressor for both purposes.
尚、特許請求の範囲の項に図面との対照を便利にする為
に符号を記すが、該記入により本発明は添付図面の構成
に限定されるものではない。Incidentally, although reference numerals are written in the claims section for convenient comparison with the drawings, the present invention is not limited to the structure shown in the accompanying drawings.
第１図乃至第４図は本発明に係る実施例を示し、第１図
は第１発明の窒素ガス製造方法を示す配管系統図、第２
図は第１発明の窒素ガス製造方法の別実施例を示す配管
系統図、第３図は第２発明の窒素ガス製造方法を示す配
管系統図、第４図は第２発明の窒素ガス製造方法の別実
施例を示す配管系統図である。
（３）・・・・・・主熱交換器、（４）・・・・・・清
潔塔、（４ａ）・・・・・・原料空気供給部、（４ｂ）
・・・・・・主精溜部、（４Ｃ）・・・・・・不純液体
酸素溜部、（４ｄ）・・・・・・補助精溜部、（５）・
・・・・・過冷却器、（７）・・・・・・リボイラー、
（１０）・・・・・・コンデンサ、（１１）・・・・・
・膨張タービン、（１２）・・・・・・液体窒素洗浄塔
、（１２ａ）・・・・・・洗浄部、（１２ｂ）・・・・
・・コンデンサ。1 to 4 show examples according to the present invention, FIG. 1 is a piping system diagram showing the nitrogen gas production method of the first invention, and FIG.
Fig. 3 is a piping system diagram showing another embodiment of the nitrogen gas production method of the first invention, Fig. 3 is a piping system diagram showing the nitrogen gas production method of the second invention, and Fig. 4 is a nitrogen gas production method of the second invention. It is a piping system diagram showing another example. (3) Main heat exchanger, (4) Clean tower, (4a) Raw air supply section, (4b)
...Main rectifying section, (4C)... Impure liquid oxygen reservoir section, (4d)... Auxiliary rectifying section, (5)
...Supercooler, (7) ...Reboiler,
(10)... Capacitor, (11)...
- Expansion turbine, (12)...Liquid nitrogen cleaning tower, (12a)...Cleaning section, (12b)...
...Capacitor.
Claims (1)
た後、主熱交換器（３）において液化点付近まで冷却し
て精溜塔（４）の下部に供給し、精溜により塔頂から製
品窒素ガスを取出す窒素ガス製造方法であって、精溜塔
（４）の塔頂から取出した窒素ガスを過冷却器（５）、
主熱交換器（３）の寒冷源として使用して常温まで加温
し、この窒素ガスの少なくとも一部を圧縮した後、主熱
交換器（３）に戻して液化点付近まで冷却し、精溜塔（
４）の底部に設けられた液体窒素洗浄塔（１２）の下部
に供給して塔の洗浄部（１２ａ）内を上昇させ、洗浄塔
（１２）頂部に設けられたコンデンサ（１２ｂ）で精溜
塔（４）底部の不純液体酸素により冷却液化されて下降
する液体窒素と向流状態で接触させて不純物を洗浄除去
した後、洗浄塔（１２）の塔頂から取出し、再び主熱交
換器（３）で常温まで加温して清浄な製品中圧窒素ガス
として取出し、洗浄塔（１２）の底部から取出された液
体窒素は前記過冷却器（５）で過冷却後、膨張させて精
溜塔（４）の上部に還流液として供給すると共に、全工
程中において別途に寒冷を補給することを特徴とする窒
素ガス製造方法。 ２、前記不純液体酸素から蒸発したガスを精溜塔（４）
の、原料空気供給部（４ａ）と不純液体酸素溜部（４ｃ
）との間に介在された補助精溜部（４ｄ）を通して精溜
塔（４）の主精溜部（４ｂ）に上昇させる特許請求の範
囲第１項に記載の窒素ガス製造方法。 ３、前記別途補給される寒冷が、外部から精溜塔（４）
の上部に供給される液体窒素である特許請求の範囲第１
項又は第２項に記載の窒素ガス製造方法。 ４、前記別途補給される寒冷が、主熱交換器（３）の中
間から取出されて膨張タービン（１１）で膨張され、精
溜塔（４）の上部に設けられたコンデンサ（１０）から
取出され、過冷却器（５）で加温された廃ガスである不
純酸素ガスと合流して主熱交換器（３）の寒冷源として
用いられる原料空気の一部である特許請求の範囲第１項
又は第２項に記載の窒素ガス製造方法。 ５、前記主熱交換器（３）で最初に常温まで加温された
窒素ガスの所要量を原料空気とほぼ同圧の低圧製品窒素
ガスとして取出し、残部を圧縮して主熱交換器（３）へ
戻す第３項又は第４項に記載の窒素ガス製造方法。[Claims] 1. Compressed air is used as a raw material, and after removing moisture, carbon dioxide, etc., it is cooled to near the liquefaction point in a main heat exchanger (3) and then supplied to the lower part of a rectification column (4). , a nitrogen gas production method in which product nitrogen gas is extracted from the top of the column by rectification, the nitrogen gas taken out from the top of the rectification column (4) is passed through a supercooler (5),
It is used as a cold source for the main heat exchanger (3) to warm it to room temperature, compress at least a portion of this nitrogen gas, and then return it to the main heat exchanger (3) and cool it to near the liquefaction point. Water tower (
4) is supplied to the lower part of the liquid nitrogen cleaning tower (12) installed at the bottom of the cleaning tower (12), and is raised inside the cleaning section (12a) of the tower, and then rectified in the condenser (12b) installed at the top of the cleaning tower (12). After being cooled and liquefied by the impure liquid oxygen at the bottom of the tower (4) and brought into contact with the descending liquid nitrogen in a countercurrent state to wash and remove impurities, it is taken out from the top of the washing tower (12) and returned to the main heat exchanger ( The liquid nitrogen taken out from the bottom of the cleaning tower (12) is supercooled in the supercooler (5), then expanded and purified. A method for producing nitrogen gas, which is characterized in that it is supplied as a reflux liquid to the upper part of the column (4), and that refrigeration is separately supplied during the entire process. 2. The gas evaporated from the impure liquid oxygen is sent to a rectification column (4)
The raw air supply section (4a) and the impure liquid oxygen reservoir section (4c)
) The method for producing nitrogen gas according to claim 1, wherein the nitrogen gas is raised to the main rectifying section (4b) of the rectifying column (4) through the auxiliary rectifying section (4d) interposed between the nitrogen gas and the rectifying column (4). 3. The separately supplied cold is supplied to the rectification tower (4) from the outside.
Claim 1 which is liquid nitrogen supplied to the upper part of the
The method for producing nitrogen gas according to item 1 or 2. 4. The separately supplied cold water is taken out from the middle of the main heat exchanger (3), expanded in the expansion turbine (11), and taken out from the condenser (10) provided at the top of the rectification column (4). Claim 1, which is part of the feed air that is combined with impure oxygen gas, which is waste gas heated in the supercooler (5), and used as a cold source for the main heat exchanger (3). The method for producing nitrogen gas according to item 1 or 2. 5. The required amount of nitrogen gas that is first heated to room temperature in the main heat exchanger (3) is taken out as a low-pressure product nitrogen gas with approximately the same pressure as the feed air, and the remainder is compressed and transferred to the main heat exchanger (3). ) The method for producing nitrogen gas according to item 3 or 4.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP32021390A JPH03230079A (en) | 1990-11-22 | 1990-11-22 | Preparation of nitrogen gas |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP32021390A JPH03230079A (en) | 1990-11-22 | 1990-11-22 | Preparation of nitrogen gas |
Related Parent Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5095186A Division JPS62206373A (en) | 1986-03-07 | 1986-03-07 | Manufacture of nitrogen gas |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH03230079A true JPH03230079A (en) | 1991-10-14 |
| JPH0427476B2 JPH0427476B2 (en) | 1992-05-11 |
Family
ID=18118983
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP32021390A Granted JPH03230079A (en) | 1990-11-22 | 1990-11-22 | Preparation of nitrogen gas |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH03230079A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0701099B1 (en) * | 1994-09-12 | 2001-09-26 | AIR LIQUIDE PROCESS & CONSTRUCTION, INC. | High purity nitrogen production process |
| EP1314941A3 (en) * | 2001-11-23 | 2003-08-27 | Messer AGS GmbH | Process and device for the production of nitrogen from air |
| JP2007003097A (en) * | 2005-06-23 | 2007-01-11 | Air Water Inc | Nitrogen generation method and apparatus used therefor |
-
1990
- 1990-11-22 JP JP32021390A patent/JPH03230079A/en active Granted
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0701099B1 (en) * | 1994-09-12 | 2001-09-26 | AIR LIQUIDE PROCESS & CONSTRUCTION, INC. | High purity nitrogen production process |
| EP1314941A3 (en) * | 2001-11-23 | 2003-08-27 | Messer AGS GmbH | Process and device for the production of nitrogen from air |
| JP2007003097A (en) * | 2005-06-23 | 2007-01-11 | Air Water Inc | Nitrogen generation method and apparatus used therefor |
Also Published As
| Publication number | Publication date |
|---|---|
| JPH0427476B2 (en) | 1992-05-11 |
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