JPH04292403A - Purification of ozone - Google Patents
Purification of ozoneInfo
- Publication number
- JPH04292403A JPH04292403A JP5292291A JP5292291A JPH04292403A JP H04292403 A JPH04292403 A JP H04292403A JP 5292291 A JP5292291 A JP 5292291A JP 5292291 A JP5292291 A JP 5292291A JP H04292403 A JPH04292403 A JP H04292403A
- Authority
- JP
- Japan
- Prior art keywords
- ozone
- distiller
- oxygen
- liquid
- pressure
- 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.)
- Withdrawn
Links
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 title claims abstract description 72
- 238000000746 purification Methods 0.000 title claims description 18
- 239000007789 gas Substances 0.000 claims abstract description 43
- 239000007788 liquid Substances 0.000 claims abstract description 41
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 20
- 239000001301 oxygen Substances 0.000 claims abstract description 20
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 20
- 229920006395 saturated elastomer Polymers 0.000 claims abstract description 18
- 239000002994 raw material Substances 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 abstract description 20
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 abstract description 17
- 229910001882 dioxygen Inorganic materials 0.000 abstract description 10
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 10
- 238000001179 sorption measurement Methods 0.000 abstract description 5
- 238000007670 refining Methods 0.000 abstract description 2
- 239000012808 vapor phase Substances 0.000 abstract description 2
- 230000000694 effects Effects 0.000 abstract 1
- 230000001105 regulatory effect Effects 0.000 abstract 1
- 239000012071 phase Substances 0.000 description 8
- 239000003507 refrigerant Substances 0.000 description 8
- 238000001816 cooling Methods 0.000 description 7
- 238000010521 absorption reaction Methods 0.000 description 3
- 238000004880 explosion Methods 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004821 distillation Methods 0.000 description 2
- 239000011261 inert gas Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 1
- 238000004904 shortening Methods 0.000 description 1
Landscapes
- Separation By Low-Temperature Treatments (AREA)
- Oxygen, Ozone, And Oxides In General (AREA)
Abstract
Description
【０００１】0001
【産業上の利用分野】この発明は、液体オゾンの精製方
法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention This invention relates to a method for purifying liquid ozone.
【０００２】0002
【従来の技術】従来より、酸化物超電導膜の形成に用い
る液体オゾンを生成するための方法として、例えば文献
１：Ｒｅｖｉｅｗ ｏｆ ＳｃｉｅｎｔｉｆｉｃＩ
ｎｓｔｒｕｍｅｎｔｓ（レビュー オブ サイエン
ティフィック インストルメンツ）Ｖｏｌ．６０
Ｎｏ．１２ １９８９年 ｐ．３７６９〜３７７０
に提案されている方法がある。[Prior Art] Conventionally, as a method for producing liquid ozone used for forming an oxide superconducting film, for example, Document 1: Review of Scientific I
nstruments (Review of Scientific Instruments) Vol. 60
No. 12 1989 p. 3769-3770
There is a method proposed.
【０００３】この方法では、原料ガス例えばオゾン及び
酸素の混合ガスを、液体窒素により冷却された蒸留器内
へ導入して液化し、液体原料例えば液体オゾン及び液体
酸素の混合液を蒸留器内に貯留する。所定量の液体原料
が蒸留器内に貯まったら、原料ガスを蒸留器内に導入す
るのをやめるとともにソープションポンプによる蒸留器
内の排気を開始する。液体窒素温度７７Ｋにおけるオゾ
ンの蒸気圧（約３ｍｍＴｏｒｒ）は酸素の蒸気圧（約１
５０Ｔｏｒｒ）に比して非常に小さいので、蒸留器内の
排気により液体オゾンを精製することができる。In this method, a raw material gas, such as a mixture of ozone and oxygen, is introduced into a distiller cooled with liquid nitrogen and liquefied, and the liquid raw material, such as a mixture of liquid ozone and liquid oxygen, is introduced into the distiller. Store. When a predetermined amount of liquid raw material is stored in the distiller, the introduction of the raw material gas into the distiller is stopped, and at the same time, the sorption pump starts exhausting the interior of the distiller. The vapor pressure of ozone (approximately 3 mm Torr) at a liquid nitrogen temperature of 77 K is the vapor pressure of oxygen (approximately 1
50 Torr), liquid ozone can be purified by exhausting the distiller.
【０００４】0004
【発明が解決しようとする課題】上述の液体オゾンの精
製において蒸留器内に残存する液体酸素が実質的に無く
なるまで液体オゾンを精製するためには、蒸留器内の気
相の圧力が液体窒素温度７７Ｋにおけるオゾンの飽和蒸
気圧（約３ｍｍＴｏｒｒ）と等しくなるまで、蒸留器内
の排気を継続して行なえばよい。しかし単純に蒸留器内
の排気を継続するだけでは、蒸留器内に残存する液体酸
素を無くして１００％液体オゾンを得るまでに非常に長
い時間が掛かるという問題点があった。また液体オゾン
と液体酸素の分離には突沸による爆発の危険性が大きい
という問題点があった。[Problems to be Solved by the Invention] In order to purify liquid ozone until the liquid oxygen remaining in the distiller is substantially eliminated, the pressure of the gas phase in the distiller must be lower than that of liquid nitrogen. The distiller may be continuously evacuated until the pressure becomes equal to the saturated vapor pressure of ozone (approximately 3 mmTorr) at a temperature of 77K. However, simply continuing to exhaust the inside of the distiller has the problem that it takes a very long time to eliminate the liquid oxygen remaining in the distiller and obtain 100% liquid ozone. Separation of liquid ozone and liquid oxygen also has the problem of a high risk of explosion due to bumping.
【０００５】しかしながら上述の文献１には、液体オゾ
ンの精製時間短縮に関して詳細な説明がなされていない
。[0005] However, the above-mentioned document 1 does not provide a detailed explanation regarding shortening the purification time of liquid ozone.
【０００６】この発明の目的は、上述した従来の問題点
を解決し、液体オゾンの精製時間の短縮を図れるオゾン
精製方法を提供することにある。[0006] An object of the present invention is to provide an ozone purification method that solves the above-mentioned conventional problems and shortens the time required to purify liquid ozone.
【０００７】[0007]
【課題を解決するための手段】この目的の達成を図るた
め、この発明のオゾン精製方法は、オゾン及び酸素を含
む原料ガスを冷却された蒸留器内へ導入することにより
液化して蒸留器内で液体オゾンを精製するに当り、該蒸
留器内の気相圧力を、該蒸留器内の温度における酸素の
飽和蒸気圧より低く、かつ該温度におけるオゾンの飽和
蒸気圧より高い圧力にまで、減圧することにより、液体
オゾンを該蒸留器内に貯留することを特徴とする。[Means for Solving the Problems] In order to achieve this object, the ozone purification method of the present invention involves introducing a raw material gas containing ozone and oxygen into a cooled distillation vessel to liquefy it into the distillation vessel. When purifying liquid ozone, the gas phase pressure in the distiller is reduced to a pressure that is lower than the saturated vapor pressure of oxygen at the temperature inside the distiller and higher than the saturated vapor pressure of ozone at the temperature. By doing so, liquid ozone is stored in the distiller.
【０００８】[0008]
【作用】このような精製方法によれば、蒸留器の気相圧
力は冷媒による冷却温度における酸素の飽和蒸気圧より
低く、かつオゾンの飽和蒸気圧より高いので、蒸留器内
には液化オゾンのみを貯留でき、酸素ガスは排気される
。従って、所定量の液化オゾンが貯留した後、原料ガス
の供給を停止すると、蒸留器内の気相圧力はオゾンの飽
和蒸気圧まですみやかに下り、オゾン精製の時間が短縮
できる。また、酸素は液化していないので、液体オゾン
と液体酸素の分離における突沸による爆発の危険性がほ
とんどなくせる。[Operation] According to this purification method, the vapor phase pressure of the distiller is lower than the saturated vapor pressure of oxygen at the cooling temperature of the refrigerant and higher than the saturated vapor pressure of ozone, so only liquefied ozone is present in the distiller. can be stored, and oxygen gas can be exhausted. Therefore, when the supply of raw material gas is stopped after a predetermined amount of liquefied ozone has been stored, the gas phase pressure in the distiller quickly drops to the saturated vapor pressure of ozone, and the time for ozone purification can be shortened. Furthermore, since oxygen is not liquefied, the risk of explosion due to bumping during separation of liquid ozone and liquid oxygen can be almost eliminated.
【０００９】[0009]
【実施例】以下、図面を参照しこの発明の実施例につき
説明する。尚、図面はこの発明が理解できる程度に概略
的に示してあるにすぎず、従ってこの発明を図示例に限
定するものではない。Embodiments Hereinafter, embodiments of the present invention will be described with reference to the drawings. Note that the drawings are merely shown schematically to the extent that the invention can be understood, and therefore the invention is not limited to the illustrated examples.
【００１０】図１はこの発明の実施例において用いるオ
ゾン精製装置の説明図であり、オゾン精製装置を成膜室
に接続した状態を示す。FIG. 1 is an explanatory diagram of an ozone purification apparatus used in an embodiment of the present invention, and shows the ozone purification apparatus connected to a film forming chamber.
【００１１】まず、この発明の実施例で用いたオゾン精
製装置の構成につき説明する。図１に示すオゾン精製装
置は、原料ガス供給部１０、蒸留器１２、冷却部１４、
バルブ１６、ソープションポンプ１８、及び分解器３０
を具える。First, the structure of the ozone purification apparatus used in the embodiment of the present invention will be explained. The ozone purification apparatus shown in FIG. 1 includes a raw material gas supply section 10, a distiller 12, a cooling section 14,
Valve 16, sorption pump 18, and decomposer 30
Equipped with.
【００１２】原料ガス供給部１０は酸素ガス源２０とオ
ゾナイザー２２とを有する。オゾナイザー２２は酸素ガ
ス源２０から導入した酸素ガスをオゾン化し、オゾンガ
ス及び酸素を含む原料ガスを生成する。そしてオゾナイ
ザー２２は原料ガスの一部をバルブ１６を通して蒸留器
１２内へ供給する。原料ガスの残りは分解器３０を通し
オゾンを酸素に分解して外部へ放出する。The source gas supply section 10 has an oxygen gas source 20 and an ozonizer 22. The ozonizer 22 ozonizes the oxygen gas introduced from the oxygen gas source 20 to generate a source gas containing ozone gas and oxygen. The ozonizer 22 then supplies a portion of the raw material gas into the distiller 12 through the valve 16. The remainder of the raw material gas passes through the decomposer 30, decomposes ozone into oxygen, and releases it to the outside.
【００１３】冷却部１４は第一の容器２４とこの容器２
４内に配置した第二の容器２６とこれら容器２４、２６
の間に貯留された冷媒２８例えば液体窒素とを有してい
る。冷媒２８により蒸留器１２を冷却し、かつソープシ
ョンポンプ１８で蒸留器１２内を排気し減圧することに
よって酸素ガスを液化させずオゾンガスのみを液化し、
これにより得られる液体オゾンを蒸留器１２内に貯留す
る。尚、酸素ガスは酸素ガスの生成プロセス上不可避的
に混入する微量の不純物を含み、従ってこの不純物が液
化することも考えられる。従ってここでオゾンガスのみ
を液化するというのは実質的には不純物が液化される場
合も含む。The cooling section 14 includes a first container 24 and this container 2.
A second container 26 arranged in 4 and these containers 24, 26
A refrigerant 28, such as liquid nitrogen, is stored between the two. By cooling the distiller 12 with the refrigerant 28 and exhausting the inside of the distiller 12 with the sorption pump 18 to reduce the pressure, only the ozone gas is liquefied without liquefying the oxygen gas,
The liquid ozone obtained thereby is stored in the distiller 12. Note that oxygen gas contains a small amount of impurities that are inevitably mixed in during the oxygen gas production process, and it is therefore possible that this impurity may be liquefied. Therefore, here, liquefying only ozone gas also includes the case where impurities are liquefied.
【００１４】ソープションポンプ１８は蒸留器１２内の
気体を吸着及び又は吸収する物質を有し、この物質の作
用により蒸留器１２内を排気する。The absorption pump 18 has a substance that adsorbs and/or absorbs gas within the distiller 12, and the inside of the distiller 12 is evacuated by the action of this substance.
【００１５】尚、図１において３８及び４０は基板及び
ヒーターをそれぞれ示す。In FIG. 1, 38 and 40 indicate a substrate and a heater, respectively.
【００１６】オゾン精製に当ってはまず、蒸留器１２及
び第二の容器２６の間に不活性ガス３２を封入しておき
、冷媒２８例えば液体窒素により蒸留器１２を冷却して
おく。そして原料ガス供給部１０により原料ガスを生成
し、ほぼ大気圧の原料ガスの一部をバルブ１６で流量を
調整して蒸留器１２内に供給する。残りの原料ガスは分
解器３０を通して外部へ放出する。原料ガスのほぼ５重
量％がオゾンガスであり残りのほぼ全部が酸素ガスであ
る。In ozone purification, first, an inert gas 32 is sealed between the distiller 12 and the second container 26, and the distiller 12 is cooled with a refrigerant 28, such as liquid nitrogen. Then, a raw material gas is generated by the raw material gas supply section 10, and a portion of the raw material gas at approximately atmospheric pressure is supplied into the distiller 12 with the flow rate adjusted by a valve 16. The remaining raw material gas is discharged to the outside through the decomposer 30. Approximately 5% by weight of the raw material gas is ozone gas, and almost all of the remainder is oxygen gas.
【００１７】原料ガスからの液体オゾンの生成は、原料
ガスの蒸留器１２内への流量をバルブ１６で調整して、
例えば、約１Ｋｇ／ｃｍ２の圧力で約０．６ｌ／ｍｉｎ
の流量とし、同時に、ソープションポンプ１８により蒸
留器１２内の排気を行い、蒸留器１２内の気相圧力を約
１００Ｔｏｒｒに保持して行う。Liquid ozone is produced from the raw material gas by adjusting the flow rate of the raw material gas into the distiller 12 with the valve 16.
For example, about 0.6 l/min at a pressure of about 1 Kg/cm2
At the same time, the distiller 12 is evacuated by the absorption pump 18, and the gas phase pressure in the distiller 12 is maintained at about 100 Torr.
【００１８】蒸留器１２内は、液体窒素温度での酸素の
飽和蒸気圧（約１５０Ｔｏｒｒ）より低く、オゾンの飽
和蒸気圧約３ｍＴｏｒｒより高く常に保持されているの
で、オゾンのみが液化され、酸素は液化しないで排気さ
れる。蒸留器１２内に所定量例えば０．５ｃｃの液体オ
ゾンを貯留したのち、バルブ１６を閉じ、原料ガスの供
給を停止し、蒸留器１２内をソープションポンプで排気
する。The inside of the distiller 12 is always maintained lower than the saturated vapor pressure of oxygen (approximately 150 Torr) at liquid nitrogen temperature and higher than the saturated vapor pressure of ozone (approximately 3 mTorr), so that only ozone is liquefied and oxygen is liquefied. It is exhausted without doing so. After a predetermined amount, for example, 0.5 cc of liquid ozone is stored in the distiller 12, the valve 16 is closed, the supply of raw material gas is stopped, and the inside of the distiller 12 is evacuated by a absorption pump.
【００１９】この排気は、好ましくは、蒸留器１２内の
気相圧力が冷媒２８による冷却温度におけるオゾンの飽
和蒸気圧となるまで行なうのがよい。蒸留器１２内の気
相圧力が液体窒素温度７７Ｋにおけるオゾンの飽和蒸気
圧３ｍｍＴｏｒｒとなるまで、液体オゾンを濃縮するの
に要する時間（以下、濃縮時間）は酸素が液化されてい
ないので、ほとんどかからない。Preferably, this evacuation is performed until the gas phase pressure in the distiller 12 reaches the saturated vapor pressure of ozone at the cooling temperature by the refrigerant 28. The time required to condense liquid ozone (hereinafter referred to as concentration time) until the gas phase pressure in the distiller 12 reaches the saturated vapor pressure of ozone of 3 mmTorr at a liquid nitrogen temperature of 77 K is hardly required because oxygen is not liquefied. .
【００２０】液体酸素と液体オゾンとを含む液体原料を
生成したのちに、蒸留器１２内を排気して、液化した酸
素を除去する従来の液体オゾンの濃縮方法では濃縮時間
は数時間かかっていた。しかしながら本実施例では、オ
ゾン精製時間を従来の方法に比べて約１／５に短縮でき
る。また、酸素が液化していないので、液体酸素と液体
オゾンの分離の際の突沸による爆発の危険性も除去でき
る。[0020] In the conventional method of concentrating liquid ozone, in which a liquid raw material containing liquid oxygen and liquid ozone is generated and then the inside of the distiller 12 is evacuated to remove the liquefied oxygen, the concentration time takes several hours. . However, in this embodiment, the ozone purification time can be reduced to about 1/5 compared to the conventional method. Furthermore, since the oxygen is not liquefied, the risk of explosion due to bumping during separation of liquid oxygen and liquid ozone can also be eliminated.
【００２１】液体オゾンを用いて超電導酸化膜を成膜す
る場合には、上述のようにして非常に純度の高い液体オ
ゾンを精製したのち、冷媒２８及び蒸留器１２を断熱し
て蒸留器１２を図示しない加熱手段、例えば電熱線で加
熱し液体オゾンを気化させてオゾンガスを生成する。そ
して成膜室３６内に設置した基板３８をヒーター４０で
加熱しながら、基板３８の成膜面に超電導酸化膜の材料
元素と共にオゾンガスを供給し超電導酸化膜を成膜する
。When forming a superconducting oxide film using liquid ozone, after refining the extremely pure liquid ozone as described above, the refrigerant 28 and the distiller 12 are insulated and the distiller 12 is heated. The liquid ozone is heated by a heating means (not shown), such as a heating wire, to vaporize the liquid ozone to generate ozone gas. Then, while heating the substrate 38 placed in the film forming chamber 36 with the heater 40, ozone gas is supplied together with material elements for the superconducting oxide film onto the film forming surface of the substrate 38 to form a superconducting oxide film.
【００２２】この発明は上述した実施例にのみ限定され
るものではなく、従って装置構成、各構成成分の組成、
温度、圧力、及びそのほかの条件を任意好適に変更する
ことができる。[0022] The present invention is not limited to the above-mentioned embodiments, and therefore the device configuration, the composition of each component,
Temperature, pressure, and other conditions can be changed as desired.
【００２３】例えば上述した実施例では、蒸留器１２の
気相圧力を約１００Ｔｏｒｒになるように原料ガスの流
量を調整したが、冷媒２８による冷却温度における酸素
の飽和蒸気圧より低く、かつオゾンの飽和蒸気圧より高
い気相圧力となるよう原料ガスの流量を調整してよい。For example, in the above embodiment, the flow rate of the raw material gas was adjusted so that the gas phase pressure in the distiller 12 was about 100 Torr, but it was lower than the saturated vapor pressure of oxygen at the cooling temperature by the refrigerant 28, and The flow rate of the raw material gas may be adjusted so that the gas phase pressure is higher than the saturated vapor pressure.
【００２４】[0024]
【発明の効果】上述した説明からも明らかなように、こ
の発明のオゾン精製方法によれば、原料ガスの流量を調
整して、蒸留器内の排気を行なう。原料ガスの流量を抑
えることにより蒸留器内を酸素の飽和蒸気圧以下に減圧
して液体オゾンのみを生成しているので、原料ガス供給
停止後すみやかにオゾンの飽和蒸気圧まで減圧するので
、液体オゾンの濃縮時間を短縮できる。また酸素を一緒
に液化しないので、安全性が向上する。As is clear from the above description, according to the ozone purification method of the present invention, the flow rate of the raw material gas is adjusted to exhaust the inside of the distiller. By suppressing the flow rate of the raw material gas, the pressure inside the distiller is reduced to below the saturated vapor pressure of oxygen and only liquid ozone is produced. Ozone concentration time can be shortened. Furthermore, since oxygen is not liquefied together, safety is improved.
【図１】この発明の実施例において用いるオゾン精製装
置の説明図である。FIG. 1 is an explanatory diagram of an ozone purification apparatus used in an example of the present invention.
１０：原料ガス供給部 １２：蒸留器 １４：冷却部 １６：バルブ １８：ソープションポンプ ２０：酸素ガス源 ２２：オゾナイザー ２４、２６：容器 ２８：冷媒 ３０：分解器 ３２：不活性ガス ３４：液体原料 10: Raw material gas supply section 12: Distiller 14: Cooling section 16: Valve 18:Sorption pump 20: Oxygen gas source 22: Ozonizer 24, 26: Container 28: Refrigerant 30: Decomposer 32: Inert gas 34: Liquid raw material
Claims (3)
された蒸留器内へ導入することにより液化して、蒸留器
内で液体オゾンを精製するに当り、該蒸留器内の気相圧
力を、該蒸留器内の温度における酸素の飽和蒸気圧より
低く、かつ該温度におけるオゾンの飽和蒸気圧より高い
圧力にまで減圧することにより、液体オゾンを該蒸留器
内に貯留することを特徴とするオゾン精製方法。Claim 1: When a raw material gas containing ozone and oxygen is introduced into a cooled distiller to liquefy it and purify liquid ozone in the distiller, the gas phase pressure in the distiller is Ozone characterized by storing liquid ozone in the distiller by reducing the pressure to a pressure lower than the saturated vapor pressure of oxygen at the temperature in the distiller and higher than the saturated vapor pressure of ozone at the temperature. Purification method.
調整して、前記蒸留器内を前記気相圧力に保持すること
を特徴とする請求項１に記載のオゾン精製方法。2. The ozone purification method according to claim 1, wherein the amount of the raw material gas supplied into the distiller is adjusted to maintain the inside of the distiller at the gas phase pressure.
ｒｒとすることを特徴とする請求項１に記載のオゾン精
製方法。3. The gas phase pressure in the distiller is set to 100 To
The ozone purification method according to claim 1, wherein the ozone purification method is rr.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5292291A JPH04292403A (en) | 1991-03-19 | 1991-03-19 | Purification of ozone |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP5292291A JPH04292403A (en) | 1991-03-19 | 1991-03-19 | Purification of ozone |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH04292403A true JPH04292403A (en) | 1992-10-16 |
Family
ID=12928327
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP5292291A Withdrawn JPH04292403A (en) | 1991-03-19 | 1991-03-19 | Purification of ozone |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH04292403A (en) |
-
1991
- 1991-03-19 JP JP5292291A patent/JPH04292403A/en not_active Withdrawn
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