JPH02150686A - Manufacture of super-high purity oxygen - Google Patents
Manufacture of super-high purity oxygenInfo
- Publication number
- JPH02150686A JPH02150686A JP63306274A JP30627488A JPH02150686A JP H02150686 A JPH02150686 A JP H02150686A JP 63306274 A JP63306274 A JP 63306274A JP 30627488 A JP30627488 A JP 30627488A JP H02150686 A JPH02150686 A JP H02150686A
- Authority
- JP
- Japan
- Prior art keywords
- oxygen
- high purity
- column
- tower
- rectification
- 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
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000001301 oxygen Substances 0.000 title claims abstract description 58
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 58
- 238000004519 manufacturing process Methods 0.000 title claims description 7
- 239000007788 liquid Substances 0.000 claims abstract description 25
- 239000012535 impurity Substances 0.000 claims abstract description 21
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims abstract description 15
- 238000001179 sorption measurement Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 abstract description 14
- 239000007789 gas Substances 0.000 abstract description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 21
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 12
- 229910052757 nitrogen Inorganic materials 0.000 description 8
- 229910002092 carbon dioxide Inorganic materials 0.000 description 5
- 239000001569 carbon dioxide Substances 0.000 description 5
- 229910001873 dinitrogen Inorganic materials 0.000 description 5
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 description 4
- 229930195733 hydrocarbon Natural products 0.000 description 4
- 150000002430 hydrocarbons Chemical class 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- 238000010992 reflux Methods 0.000 description 4
- 239000003990 capacitor Substances 0.000 description 3
- -1 moisture Natural products 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- 229910052786 argon Inorganic materials 0.000 description 2
- 229910002090 carbon oxide Inorganic materials 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 229910052743 krypton Inorganic materials 0.000 description 2
- DNNSSWSSYDEUBZ-UHFFFAOYSA-N krypton atom Chemical compound [Kr] DNNSSWSSYDEUBZ-UHFFFAOYSA-N 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 229910052724 xenon Inorganic materials 0.000 description 2
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 2
- 238000011109 contamination Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 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
- F25J3/08—Separating gaseous impurities from gases or gaseous mixtures or from liquefied gases or liquefied gaseous mixtures
-
- 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
- F25J2200/02—Processes or apparatus using separation by rectification in a single pressure main column system
-
- 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
- F25J2200/30—Processes or apparatus using separation by rectification using a side column in a single pressure column system
-
- 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
- F25J2205/00—Processes or apparatus using other separation and/or other processing means
- F25J2205/60—Processes or apparatus using other separation and/or other processing means using adsorption on solid adsorbents, e.g. by temperature-swing adsorption [TSA] at the hot or cold end
-
- 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
- F25J2215/50—Oxygen or special cases, e.g. isotope-mixtures or low purity O2
- F25J2215/56—Ultra high purity oxygen, i.e. generally more than 99,9% O2
-
- 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
- F25J2220/00—Processes or apparatus involving steps for the removal of impurities
- F25J2220/50—Separating low boiling, i.e. more volatile components from oxygen, e.g. N2, Ar
-
- 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
- F25J2220/00—Processes or apparatus involving steps for the removal of impurities
- F25J2220/52—Separating high boiling, i.e. less volatile components from oxygen, e.g. Kr, Xe, Hydrocarbons, Nitrous oxides, O3
-
- 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
- F25J2270/00—Refrigeration techniques used
- F25J2270/42—Quasi-closed internal or closed external nitrogen refrigeration cycle
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、微量不純物を含む酸素を精製して超高純度の
酸素を製造する方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial Application Field] The present invention relates to a method for producing ultra-high purity oxygen by purifying oxygen containing trace impurities.
高純度の酸素を精製する場合は、一般に、通常の空気分
離装置で得られる酸素を吸着塔等の精製装置によって処
理し、炭化水素、水分、二酸化炭素等の微量不純物を除
去する方法が用いられている。In order to purify high-purity oxygen, a method is generally used in which the oxygen obtained with a normal air separation device is treated with a purification device such as an adsorption tower to remove trace impurities such as hydrocarbons, moisture, and carbon dioxide. ing.
ところで、最近の半導体工業等の分野においては、超高
純度の酸素、具体的には９９．９９９９％程度の酸素の
需要が増大しているが、上述の一般的な酸素精製方法で
は、９９．９％程度の酸素しか得られず、前記需要に応
じ得るような超高純度の酸素は得られない。なぜなら、
上述の一般的な酸素精製方法では、酸素中の微量不純物
の一部しか除去されず、十分に高純度な酸素が得られる
ものではないからである。Incidentally, in recent fields such as the semiconductor industry, there has been an increasing demand for ultra-high purity oxygen, specifically about 99.9999% oxygen, but the above-mentioned general oxygen purification method can only produce 99.9999% oxygen. Only about 9% oxygen can be obtained, and ultra-high purity oxygen that can meet the above demand cannot be obtained. because,
This is because the above-mentioned general oxygen purification method only removes a portion of trace impurities in oxygen, and oxygen of sufficiently high purity cannot be obtained.
そこで、前記超高純度の酸素が必要な場合は、コスト高
になるにも拘らず電解等を用いた不経済な方法を利用せ
ざるを得なかった。Therefore, when the ultra-high purity oxygen is required, an uneconomical method using electrolysis or the like has to be used despite the high cost.
本発明は、かかる事情に鑑みてなされたものであり、そ
の目的は、超高純度の酸素を低コストにて有効に得る方
法を提供する点にある。The present invention has been made in view of such circumstances, and its purpose is to provide a method for effectively obtaining ultra-high purity oxygen at low cost.
本発明に係る超高純度酸素製造方法は、微量不純物を含
む液体酸素を第１精溜塔へ導き、該第１精溜塔にて精溜
を行って、該第１精溜塔における精溜部よりもリボイラ
側から高純度の酸素を液体状態で製出した後、該高純度
の酸素を第２精溜塔の精溜部へ導き、該第２精溜塔にて
精溜を行って、該第２精溜塔における精溜部頂部又はそ
れよりもコンデンサ側から超高純度の酸素を製出する点
に特徴を有している。The method for producing ultra-high purity oxygen according to the present invention includes guiding liquid oxygen containing trace impurities to a first rectification column, performing rectification in the first rectification column, and performing rectification in the first rectification column. After producing high-purity oxygen in a liquid state from the reboiler side than the part, the high-purity oxygen is led to the rectification part of a second rectification column, and rectified in the second rectification column. , is characterized in that ultra-high purity oxygen is produced from the top of the rectification section in the second rectification column or from the side closer to the condenser.
なお、前記第１精溜塔のリボイラ側から液体状態で製出
した高純度の酸素は、前記第２精溜塔へ導く前に、低温
吸着塔を経由させるようにするのが好ましい。Note that it is preferable that the high-purity oxygen produced in a liquid state from the reboiler side of the first rectification column be passed through a low-temperature adsorption tower before being led to the second rectification column.
かかる本発明方法による場合、微量不純物を含む液体酸
素を先ず前記第１精溜塔で精溜し、その精溜部よりもリ
ボイラ側から高純度の酸素を液体状態で製出するので、
そのコンデンサ側から、窒素、−酸化炭素、アルゴン等
の酸素に比して蒸発し易いｍｌ不純物が除去できる。そ
して前記高純度の酸素を前記第２精溜塔で精溜し、その
精溜部頂部又はそれよりもコンデンサ側から超高純度の
酸素を液体状態で製出するので、該第２精溜塔では、そ
のリポイラ側からクリプトン、キセノン等の酸素に比し
て凝縮し易い微量不純物が除去できる。In the case of the method of the present invention, liquid oxygen containing trace impurities is first rectified in the first rectification column, and high-purity oxygen is produced in a liquid state from the reboiler side than the rectification section.
From the condenser side, impurities that evaporate more easily than oxygen, such as nitrogen, carbon oxide, and argon, can be removed. Then, the high-purity oxygen is rectified in the second rectification column, and ultra-high purity oxygen is produced in a liquid state from the top of the rectification section or from the side of the condenser, so the second rectification column Then, trace impurities such as krypton and xenon, which are more easily condensed than oxygen, can be removed from the lipoiler side.
なお、前記第１精溜塔のリボイラ側から液体状態で製出
した高純度の酸素を、前記第２精溜塔へ導く前に、低温
吸着塔を経由させるようにすれば、該低温吸着塔によっ
て炭化水素、水分。Note that if the high-purity oxygen produced in a liquid state from the reboiler side of the first rectification column is passed through a low-temperature adsorption column before being led to the second rectification column, the low-temperature adsorption column By hydrocarbons, moisture.
二酸化炭素等が吸着除去され、もってこれらの不純物が
、第２精溜塔のコンデンサ側へ製出される超高純度の酸
素へ混入するのが回避される。Carbon dioxide and the like are adsorbed and removed, thereby preventing these impurities from being mixed into the ultra-high purity oxygen produced to the condenser side of the second rectification column.
従って、本発明方法によれば、最近の半導体工業等の分
野においても利用し得るような超高純度の酸素を、コス
ト高となる電解等を用いた方法によらずに有効に得るこ
とができるようになる。Therefore, according to the method of the present invention, it is possible to effectively obtain ultra-high purity oxygen, which can be used in recent fields such as the semiconductor industry, without using expensive methods such as electrolysis. It becomes like this.
以下、本発明方法をその実施に使用する装置を示す図面
に基づいて説明する。DESCRIPTION OF THE PREFERRED EMBODIMENTS The method of the present invention will be described below with reference to the drawings showing an apparatus used for carrying out the method.
図中、（１）は塔底部にリボイラ（１ａ）を塔頂部にコ
ンデンサ（１ｂ）を夫々備える第１精溜塔を示しており
、該第１精溜塔（１）には、その精溜部へ空気から分離
して得られた微量不純物を含む液体酸素（純度： ９９
．６〜９９．９％）がポンプ（２）で約０ 、５ ｋｇ
／ ｃ＋ａ ［Ｈの圧力に圧縮された上で配管（ｐ＋
）を通して導入されるようになっている。なお、該液体
酸素の圧力が元々０ 、５ ｋｇ ／ ｃｄｌ Ｇ以上
ある場合には、該液体酸素は前記ポンプ（２）を経由す
ることなく、直接的に前記第１精溜塔（１）へ導入され
るようになっている。In the figure, (1) shows a first rectification column that is equipped with a reboiler (1a) at the bottom of the column and a condenser (1b) at the top of the column. Liquid oxygen containing trace impurities obtained by separating it from air (purity: 99%)
．． 6-99.9%) is approximately 0.5 kg at pump (2)
/ c+a [Piping (p+
). Note that if the pressure of the liquid oxygen is originally 0.5 kg/cdl G or more, the liquid oxygen is directly sent to the first rectification column (1) without passing through the pump (2). It is about to be introduced.
前記第１精溜塔（１）では、上述の如く導入され前記リ
ボイラ（１ａ）に貯留される微量不純物を含む液体酸素
からりボイルガスが発生し、該リボイルガスと塔頂部の
コンデンサ（１ｂ）からの還流液とが向流接触すること
によって精溜が行われ、前記塔頂部から配管（Ｐ２）、
熱交換器（３）及び配管（Ｐ３）を通し、蒸気のまま廃
ガスとして排出される少量の酸素中に、酸素に比して凝
縮し難い窒素、−酸化炭素、アルゴン等の不純物を含有
させてこれを分離する一方、大部分の酸素は凝縮し、高
純度な状態となって前記塔底部から液体の状態で製出さ
れるようになっている。In the first rectification column (1), a boil gas containing trace impurities is generated, which is introduced as described above and stored in the reboiler (1a), and the reboil gas and the condenser (1b) at the top of the column are Rectification is performed by countercurrent contact with the reflux liquid, and from the top of the column there are pipes (P2),
Impurities such as nitrogen, carbon oxide, and argon, which are difficult to condense compared to oxygen, are contained in a small amount of oxygen that is discharged as waste gas in the form of vapor through the heat exchanger (3) and piping (P3). Most of the oxygen is condensed and produced in a liquid state from the bottom of the column in a highly pure state.
なお、図中の（４）は窒素ガスのリサイクル圧縮機であ
り、該リサイクル圧縮機（４）に・て約６．５ｋｇ ／
ａｌｌ Ｇに圧縮された窒素ガスは、配管（Ｐ４）を
通して熱交換器（３）へ導かれてそこで熱交換された上
で配管（Ｐ５）を通して前記塔底部のリボイラ（１ａ）
へ導かれ、該リボイラ（１ａ）にて前記リボイルガスを
発生させる一方、自らは液化して液体窒素となった後、
配管（Ｐ６）を通して前記塔頂部のコンデンサ（１ｂ）
へ導かれる。そして該液体窒素は、前記コンデンサ（１
ｂ）にて約２ 、５ ｋｇ ／ ｃｉ Ｇの圧力で蒸発
すると共に第１精溜塔（１）内を下降する還流液を製出
するようになっている。そして上述の如く蒸発した窒素
は、前記塔頂部のコンデンサ（１ｂ）から第１精溜塔（
１）外へ排出されるが、該窒素ガスは、配管（Ｐ７）、
熱交換器（３）及び配管（ｐａ）を通して前記リサイク
ル圧縮機（４）へ返戻されるようになっている。In addition, (4) in the figure is a nitrogen gas recycling compressor, and the recycling compressor (4) is approximately 6.5 kg /
The nitrogen gas compressed to all G is led to the heat exchanger (3) through the pipe (P4), where it undergoes heat exchange, and then passes through the pipe (P5) to the reboiler (1a) at the bottom of the tower.
and generates the reboiling gas in the reboiler (1a), while liquefying itself to become liquid nitrogen,
The condenser (1b) at the top of the tower through the pipe (P6)
be led to. Then, the liquid nitrogen is supplied to the condenser (1).
In b), the reflux liquid is evaporated at a pressure of about 2.5 kg/ci G and descends in the first rectification column (1). The nitrogen vaporized as described above is then transferred from the condenser (1b) at the top of the column to the first rectification column (
1) The nitrogen gas is discharged to the outside through the pipe (P7),
It is returned to the recycling compressor (4) through a heat exchanger (3) and piping (pa).
前記第１精溜塔（１）の塔底部から製出される高純度の
液体酸素は、配管（Ｐ、）を通して低温吸着塔（５）へ
導かれ、該吸着塔（５）内にて不純物としての炭化水素
、水分、炭酸ガス等が吸着除去され、然る後に配管（ｐ
ｒｏ）を通して第２精溜塔（６）の精溜部へ導入される
ようになっている。High-purity liquid oxygen produced from the bottom of the first rectification column (1) is led to a low-temperature adsorption column (5) through a pipe (P,), and is removed as impurities in the adsorption column (5). Hydrocarbons, water, carbon dioxide, etc. are adsorbed and removed, and then the pipes (p
ro) to the rectification section of the second rectification column (6).
前記第２精溜塔（６）は、前記第１精溜塔（１）と同様
、塔頂部にコンデンサ（６ｂ）を塔底部にリボイラ（６
ａ）を夫々備えてなっている。そして該第２精溜塔（６
）では、上述の如く導入され塔底部のリボイラ（６ａ）
に貯留される液体からりボイルガスが発生し、該リボイ
ルガスと塔頂部のコンデンサ（６ｂ）からの還流液とが
向流接触することによって精溜が行われ、前記塔底部か
らクリプトン、キセノン等の酸素に比して凝縮し易い不
純物を含有する少量の液体酸素を、配管（ｐ＋＋）、蒸
発器（７）及び配管（ｐ、□）を通して排出する一方、
前記塔頂部のコンデンサ（６ｂ）からは超高純度の酸素
を液体状態で製出し、該超高純度の酸素を、配管（ＰＩ
３）を通して液体状態のまま取り出すか、或いはポンプ
（９）及び蒸発器（８）を通して蒸発させた上で取り出
すようになっている。The second rectification column (6), like the first rectification column (1), has a condenser (6b) at the top of the column and a reboiler (6b) at the bottom of the column.
a). And the second rectification column (6
), the reboiler (6a) at the bottom of the column was introduced as described above.
Boil gas is generated from the liquid stored in the column, and rectification is performed by countercurrent contact between the reboil gas and the reflux liquid from the condenser (6b) at the top of the column, and oxygen such as krypton and xenon is released from the bottom of the column. While discharging a small amount of liquid oxygen containing impurities that are easily condensed compared to the pipe (p++), the evaporator (7) and the pipe (p, □),
Ultra-high purity oxygen is produced in a liquid state from the condenser (6b) at the top of the column, and the ultra-high purity oxygen is transferred to a pipe (PI
3), it can be taken out in a liquid state, or it can be taken out after being evaporated through a pump (9) and an evaporator (8).
また、前記リサイクル圧縮機（４）にて約６ 、５ ｋ
ｇ ／ｃ＋ＩＩＧに圧縮された窒素ガスは、配管（Ｐ＋
４）を通して蒸発器（７）へ導かれてそこで熱交換され
た上で配管（Ｐ ＋ ｓ）を通して前記塔底部のボイラ
（６ａ）へ導かれ、該リボイラ（６ａ）にて前記リボイ
ルガスを発生させる一方、自らは液化した液体窒素とな
った後、配管（Ｐ＋６）を通して前記塔頂部のコンデン
サ（６ｂ）へ導かれる。そして該液体窒素は、前記コン
デンサ（６ｂ）にて約２．５ｋｇ／ｃ艷Ｇの圧力で蒸発
すると共に第２精溜塔（６）内を下降する還流液を製出
するようになっている。そして上述の如く蒸発した窒素
は、前記塔頂部から排出されるが、該窒素ガスは、配管
（Ｐ、）、熱交換器（３）及び配管（Ｐ８）を通して前
記リサイクル圧縮器（４）へ返戻されるようになってい
る。In addition, the recycling compressor (4) generates approximately 6.5 k
Nitrogen gas compressed to g/c+IIG is transferred to the pipe (P+
4) to the evaporator (7), where it undergoes heat exchange, and is then led to the boiler (6a) at the bottom of the tower through the piping (P + s), where the reboiler (6a) generates the reboil gas. On the other hand, after it becomes liquid nitrogen, it is led to the condenser (6b) at the top of the column through the pipe (P+6). The liquid nitrogen is evaporated in the condenser (6b) at a pressure of about 2.5 kg/cmG and produces a reflux liquid that descends in the second rectification column (6). . The nitrogen vaporized as described above is discharged from the top of the column, but the nitrogen gas is returned to the recycle compressor (4) through the pipe (P,), the heat exchanger (3), and the pipe (P8). It is now possible to do so.
なお、図中の（１１）はコールドボックスであり、該コ
ールドボックス（１１）内には、前記第１精溜塔（１）
、第２精溜塔（６）、熱交換器（３）、低温吸着塔（５
）等、上述の装置の主要部分が一括して収められている
。Note that (11) in the figure is a cold box, and inside the cold box (11) is the first rectification column (1).
, second rectification column (6), heat exchanger (3), low temperature adsorption column (5
), etc., the main parts of the above-mentioned devices are all housed together.
かかる装置を用いて本発明方法を実施する場合、微量不
純物を含む液体酸素を先ず第１精溜塔（１）で精溜して
高純度の酸素を塔底部から製出した後、更に該高純度の
酸素を第２精溜塔（６）で精溜することにより、不純物
を塔底部から分離して超高純度の酸素を塔頂部から製出
することができる。なお、第１精溜塔（１）の塔底部か
ら製出した高純度の酸素は、第２精溜塔（６）へ導かれ
る前に低温吸着塔（５）を経由せしめられるので、そこ
で炭化水素、水分、二酸化炭素等の微量不純物が有効に
吸着除去され、もってこれらの不純物が、第２精溜塔（
６）の塔頂部にて液体状体として製出される超高純度の
酸素へ混入するのが回避される。When carrying out the method of the present invention using such an apparatus, liquid oxygen containing trace impurities is first rectified in the first rectification column (1) to produce high-purity oxygen from the bottom of the column, and then the high-purity oxygen is further purified. By rectifying pure oxygen in the second rectification column (6), impurities can be separated from the bottom of the column and ultra-high purity oxygen can be produced from the top of the column. Note that the high-purity oxygen produced from the bottom of the first rectifying column (1) is passed through a low-temperature adsorption column (5) before being led to the second rectifying column (6), where it is carbonized. Trace impurities such as hydrogen, moisture, and carbon dioxide are effectively adsorbed and removed, and these impurities are then transferred to the second rectification column (
6) Contamination with the ultra-high purity oxygen produced as a liquid at the top of the column is avoided.
なお、図中の配管（Ｐ＋、）は、前記第２精溜塔（６）
のコンデンサ（６ｂ）内の蒸気分を排出するためのもの
であるが、これを用いることにより、酸素に比して凝縮
し難くて蒸気のまま存在する確率の高い極微量の不純物
は除去されることとなる。In addition, the pipe (P+,) in the figure is the second rectification column (6).
This is to exhaust the vapor in the condenser (6b), but by using this, extremely small amounts of impurities that are difficult to condense compared to oxygen and have a high probability of existing as vapor can be removed. It happens.
上記実施例は、超高純度の酸素を、前記第２精溜塔（６
）の精溜部よりも上方のコンデンサ（６ｂ）において製
出するものであったが、超高純度の酸素は、前記精溜部
の頂部においても製出できる。In the above embodiment, ultra-high purity oxygen is transferred to the second rectification column (6
), but ultra-high purity oxygen can also be produced at the top of the rectification section.
また、上述の実施例においては、超高純度の酸素を、前
記コンデンサ（６ｂ）から液体状態で取り出−すもので
あったが、超高純度の酸素は、前記コンデンサ（６ｂ）
から気体状態で取り出すこともできる。具体的には、前
記コンデンサ（６ｂ）における前記配管（ＰＩ３）連結
位置よりも上方に連結した配管（Ｐ＋ｅ）より気体状態
で超高純度の酸素を取り出し、該酸素を前記熱交換器（
３）を経由させて寒冷を回収した後、製品ガスとするこ
とができる。なお、図においては、前記配管（ｐｕｓ）
の熱交換器（３）以後の下流域配管系は省略しである。Further, in the above-described embodiment, ultra-high purity oxygen was extracted from the capacitor (6b) in a liquid state, but the ultra-high purity oxygen was extracted from the capacitor (6b).
It can also be extracted in gaseous form. Specifically, ultra-high purity oxygen is taken out in a gaseous state from a pipe (P+e) connected above the connection position of the pipe (PI3) in the condenser (6b), and the oxygen is transferred to the heat exchanger (
After recovering the cold through 3), it can be used as a product gas. In addition, in the figure, the piping (pus)
The downstream piping system after the heat exchanger (3) is omitted.
また、上述した装置を用いて精製する原料中に、炭化水
素、水分、二酸化炭素等が実質的に含まれていない場合
は、上述の装置の中から低温吸着塔（５）を除いても差
支えがないこともあり得る。In addition, if the raw material to be purified using the above-mentioned equipment does not substantially contain hydrocarbons, moisture, carbon dioxide, etc., the low-temperature adsorption tower (5) may be omitted from the above-mentioned equipment. It is possible that there is no.
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方法
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 method shown in the accompanying drawings.
図面は本発明に係る超高純度酸素製造方法の実施に使用
する装置の配管系統図である。
（１）・・・・・・第１精溜塔、（１ａ）・・・・・・
リボイラ、（１ｂ）・・・・・・コンデンサ、（５）・
・・・・・低温吸着塔、（６）・・・・・・第２精溜塔
、
（６ｂ）・・・・・・コンデンサ。The drawing is a piping system diagram of an apparatus used to carry out the method for producing ultra-high purity oxygen according to the present invention. (1)...First rectification column, (1a)...
Reboiler, (1b)... Capacitor, (5).
...low temperature adsorption tower, (6) ... second rectification tower, (6b) ... condenser.
Claims (1)
き、該第１精溜塔（１）にて精溜を行って、該第１精溜
塔（１）における精溜部よりもリボイラ（１ａ）側から
高純度の酸素を液体状態で製出した後、該高純度の酸素
を第２精溜塔（６）の精溜部へ導き、該第２精溜塔（６
）にて精溜を行って、該第２精溜塔（６）における精溜
部頂部又はそれよりもコンデンサ（６ｂ）側から超高純
度の酸素を製出することを特徴とする超高純度酸素製造
方法。 ２、前記第１精溜塔（１）のリボイラ（１ａ）側から液
体状態で製出した高純度の酸素を、低温吸着塔（５）経
由で第２精溜塔（６）の精溜部へ導く請求項１記載の超
高純度酸素製造方法。[Claims] 1. Liquid oxygen containing trace impurities is led to the first rectification column (1), and rectified in the first rectification column (1). After producing high-purity oxygen in a liquid state from the reboiler (1a) side rather than the rectification part in 1), the high-purity oxygen is led to the rectification part of the second rectification column (6), and then 2 rectification towers (6
) to produce ultra-high purity oxygen from the top of the rectification section in the second rectification column (6) or from the condenser (6b) side thereof. Oxygen production method. 2. High purity oxygen produced in a liquid state from the reboiler (1a) side of the first rectification column (1) is sent to the rectification section of the second rectification column (6) via the low temperature adsorption column (5). The method for producing ultra-high purity oxygen according to claim 1, which leads to.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63306274A JP2680082B2 (en) | 1988-12-02 | 1988-12-02 | Ultra high purity oxygen production method |
| FR898915844A FR2640032B1 (en) | 1988-12-02 | 1989-12-01 | METHOD FOR PRODUCING ULTRA-PUR OXYGEN |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP63306274A JP2680082B2 (en) | 1988-12-02 | 1988-12-02 | Ultra high purity oxygen production method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH02150686A true JPH02150686A (en) | 1990-06-08 |
| JP2680082B2 JP2680082B2 (en) | 1997-11-19 |
Family
ID=17955111
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP63306274A Expired - Lifetime JP2680082B2 (en) | 1988-12-02 | 1988-12-02 | Ultra high purity oxygen production method |
Country Status (2)
| Country | Link |
|---|---|
| JP (1) | JP2680082B2 (en) |
| FR (1) | FR2640032B1 (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2015155083A (en) * | 2014-02-20 | 2015-08-27 | オルガノ株式会社 | Method and apparatus for supply of ozone water |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2966999B2 (en) * | 1992-04-13 | 1999-10-25 | 日本エア・リキード株式会社 | Ultra high purity nitrogen / oxygen production equipment |
| US5682763A (en) * | 1996-10-25 | 1997-11-04 | Air Products And Chemicals, Inc. | Ultra high purity oxygen distillation unit integrated with ultra high purity nitrogen purifier |
| US6178776B1 (en) * | 1999-10-29 | 2001-01-30 | Praxair Technology, Inc. | Cryogenic indirect oxygen compression system |
| WO2023132876A1 (en) * | 2022-01-04 | 2023-07-13 | Praxair Technology, Inc. | System and method for co-producing ultra-high purity oxygen and ultra-high purity hydrogen |
| EP4477980A1 (en) * | 2023-06-15 | 2024-12-18 | Linde GmbH | Method and apparatus for producing air products from an oxygen fraction |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61105088A (en) * | 1984-08-16 | 1986-05-23 | ユニオン・カ−バイド・コ−ポレ−シヨン | Manufacture of ultra-high purity oxygen |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE3322473A1 (en) * | 1983-06-22 | 1985-01-03 | Linde Ag, 6200 Wiesbaden | Method and device for avoiding enrichment of undesired components in a liquid medium |
| US4869741A (en) * | 1988-05-13 | 1989-09-26 | Air Products And Chemicals, Inc. | Ultra pure liquid oxygen cycle |
-
1988
- 1988-12-02 JP JP63306274A patent/JP2680082B2/en not_active Expired - Lifetime
-
1989
- 1989-12-01 FR FR898915844A patent/FR2640032B1/en not_active Expired - Fee Related
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61105088A (en) * | 1984-08-16 | 1986-05-23 | ユニオン・カ−バイド・コ−ポレ−シヨン | Manufacture of ultra-high purity oxygen |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2015155083A (en) * | 2014-02-20 | 2015-08-27 | オルガノ株式会社 | Method and apparatus for supply of ozone water |
Also Published As
| Publication number | Publication date |
|---|---|
| FR2640032B1 (en) | 1992-07-31 |
| FR2640032A1 (en) | 1990-06-08 |
| JP2680082B2 (en) | 1997-11-19 |
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