JPH0716581A - Method for sterilizing ultrapure water with ozone and device therefor - Google Patents
Method for sterilizing ultrapure water with ozone and device thereforInfo
- Publication number
- JPH0716581A JPH0716581A JP18925193A JP18925193A JPH0716581A JP H0716581 A JPH0716581 A JP H0716581A JP 18925193 A JP18925193 A JP 18925193A JP 18925193 A JP18925193 A JP 18925193A JP H0716581 A JPH0716581 A JP H0716581A
- Authority
- JP
- Japan
- Prior art keywords
- pure water
- ozone
- ultrapure water
- water
- primary pure
- 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.)
- Pending
Links
Landscapes
- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
Description
【０００１】[0001]
【産業上の利用分野】本発明は、電子工業、医薬品製造
等の技術分野で要求される超純水を多量に製造供給する
システムを高度の無菌状態に維持するための方法及び装
置に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method and an apparatus for maintaining a highly sterile state of a system for producing and supplying a large amount of ultrapure water required in the technical fields such as electronic industry and pharmaceutical manufacturing.
【０００２】[0002]
【従来技術とその問題点】電子工業における部品洗浄や
医薬品製造等の技術分野で要求される超純水を製造する
際には蒸留やイオン交換等の一次精製で製造した純水を
ポリシャー等を含む超純水製造装置に供給して更にパー
ティクル等の不純物を除去し純度を向上させるようにし
ている。このようにして製造された超純水は供給ライン
を通してユースポイントに供給され洗浄等に使用された
後、未使用あるいは使用済の超純水あるいは純水を前記
一次精製工程に循環して再使用するようにしている。2. Description of the Related Art When producing ultrapure water required in the technical fields of electronic parts washing and pharmaceutical manufacturing, pure water produced by primary purification such as distillation or ion exchange is passed through a polisher or the like. It is supplied to an ultrapure water producing apparatus containing the same to further remove impurities such as particles and improve the purity. The ultrapure water produced in this way is supplied to the point of use through the supply line and used for cleaning, etc., and then unused or used ultrapure water or pure water is circulated to the primary purification step for reuse. I am trying to do it.
【０００３】つまり図２に示すように、純水製造装置１
で製造され一次純水タンク２に貯留された純水をポンプ
３を使用して超純水製造装置４に送水する。該超純水製
造装置４は少なくとも純水中の無機物を除去するポリシ
ャー５と微粒子や高分子有機物を除去するミクロンフィ
ルターや限外濾過膜等の精密濾過器６から成り、供給さ
れた前記純水中の純度を向上させ、生ずる不純物を濾過
して除去する。なお前記超純水製造装置４は生菌を殺菌
するための紫外線殺菌灯を含んでいてもよい。該超純水
製造装置４により製造された超純水は供給ライン７を通
して図示の例では２ヵ所のユースポイント８に供給さ
れ、該ユースポイント８において電子部品の洗浄等の操
作を行い被処理体の処理を行う。この処理操作で使用さ
れあるいは過剰に供給されて使用されなかった使用済純
水又は未使用超純水は集められリターンライン９を通っ
て前記一次純水タンク２に循環され、再度超純水製造装
置４へ送水されて洗浄等に利用される。That is, as shown in FIG. 2, a pure water producing apparatus 1
The pure water produced in step 1 and stored in the primary pure water tank 2 is sent to the ultrapure water producing apparatus 4 using the pump 3. The ultrapure water producing device 4 comprises at least a polisher 5 for removing inorganic substances in pure water and a microfilter 6 for removing fine particles and high molecular weight organic substances, and a microfilter 6 such as an ultrafiltration membrane. The purity of the inside is improved and the resulting impurities are removed by filtration. The ultrapure water production system 4 may include an ultraviolet germicidal lamp for sterilizing live bacteria. In the illustrated example, the ultrapure water produced by the ultrapure water producing apparatus 4 is supplied to two use points 8 in the illustrated example, and at the use points 8, an operation such as cleaning of electronic parts is performed and an object to be treated is processed. Process. Used pure water or unused ultrapure water which has been used in this treatment operation or supplied excessively and which has not been used is collected and circulated through the return line 9 to the primary pure water tank 2 to produce ultrapure water again. Water is sent to the device 4 and used for cleaning and the like.
【０００４】このように図示の超純水循環による処理シ
ステムでは超純水が有効に使用され効率的に被処理体の
処理を行うことができるが、前記紫外線殺菌灯を使用し
た場合でも該殺菌灯の殺菌力が弱く、水流の停滞が生じ
ないように前記循環ポンプ３を常時稼働させて循環流が
途切れないようにしてもバクテリアの発生が観察され
る。このバクテリアは超純水の水質を悪化させ、この水
質が悪化した超純水により被処理体を前記ユースポイン
トで処理して得られる製品の品質悪化及び歩留りや生産
性の低下を招くことになる。このバクテリア数の増加に
伴ってシステム内の超純水中のパーティクル数やＴＯＣ
も増加する傾向にある。As described above, in the treatment system using the ultrapure water circulation shown in the figure, the ultrapure water is effectively used and the object to be treated can be efficiently treated. However, even when the ultraviolet sterilizing lamp is used, the sterilization is performed. Even if the circulation pump 3 is constantly operated so that the sterilizing power of the lamp is weak and the water flow does not become stagnant so that the circulation flow is not interrupted, the generation of bacteria is observed. This bacterium deteriorates the water quality of the ultrapure water, and the ultrapure water with the deteriorated water quality causes a deterioration in the quality of the product obtained by treating the object at the point of use and a decrease in the yield and productivity. . As the number of bacteria increases, the number of particles in the ultrapure water in the system and the TOC
Also tends to increase.
【０００５】従来は前記超純水循環システムで不可避的
に発生するバクテリア数を極力低レベルに維持するため
に、定期的に運転を停止して次亜塩素酸ソーダ、過酸化
水素及びオゾン等の殺菌剤や熱水をシステム内に保持す
ることにより該システム内の殺菌及び洗浄を行うことが
一般的であった。この方法によるとバクテリアの繁殖は
抑制できるものの、超純水循環システムの運転が数時間
〜１日程度停止することを余儀なくされ、従って超純水
の製造及び該超純水を使用する生産活動もこの間操業を
停止又はスローダウンしなければならず、特に年間連続
操業を目指す電子工業では生産性の低下を招く前記方法
を採用することは望ましくない。Conventionally, in order to keep the number of bacteria inevitably generated in the ultrapure water circulation system at a low level as much as possible, the operation is periodically stopped to remove sodium hypochlorite, hydrogen peroxide, ozone, etc. It has been common to sterilize and clean the system by holding a bactericide and hot water in the system. According to this method, although the growth of bacteria can be suppressed, the operation of the ultrapure water circulation system must be stopped for several hours to 1 day, and therefore, the production of ultrapure water and the production activities using the ultrapure water are also required. During this time, the operation must be stopped or slowed down, and it is not desirable to adopt the above method which causes a decrease in productivity, especially in the electronic industry aiming at continuous operation for a year.
【０００６】更に前記殺菌剤添加法ではそれに伴って副
次的問題が生ずる。例えば殺菌剤使用後に該殺菌剤がシ
ステム内に残存しないように超純水による徹底したシス
テム内の後洗浄が必要となり、かつ洗浄排水の処理の問
題となる。又熱水を使用した場合にも、昇降温に要する
熱エネルギー消費、有機材料等の装置配管の耐熱性等の
問題があり、これらは未解決である。Further, in the above-mentioned bactericidal agent addition method, a secondary problem occurs accordingly. For example, thorough post-cleaning of the system with ultrapure water is necessary so that the sterilizing agent does not remain in the system after the sterilizing agent is used, and there is a problem of treatment of cleaning waste water. Further, even when hot water is used, there are problems such as heat energy consumption required for raising and lowering temperature, heat resistance of apparatus piping for organic materials and the like, and these are unsolved.
【０００７】[0007]
【発明の目的】本発明は、前述の従来技術の問題点を解
消し、超純水製造及び供給システムの運転を実質的に停
止することなく継続的に運転しながらシステム内の超純
水中のバクテリア数を最低レベルに維持し高純度の超純
水で被処理体の処理を行い得るようにした超純水オゾン
殺菌方法及び装置を提供することを目的とする。It is an object of the present invention to solve the above-mentioned problems of the prior art by continuously operating the ultrapure water production and supply system without substantially stopping the operation of the ultrapure water production and supply system. It is an object of the present invention to provide an ultrapure water ozone sterilization method and apparatus capable of treating an object to be treated with high-purity ultrapure water while keeping the number of bacteria at the minimum level.
【０００８】[0008]
【問題点を解決するための手段】本発明は、一次純水タ
ンク中の一次純水を少なくともポリシャーを含む超純水
製造装置に供給して超純水とし、該超純水を供給ライン
を経由してユースポイントに送水し該ユースポイントで
前記超純水を使用して被処理体を処理し、使用済純水を
リターンラインを経由して前記一次純水タンクに循環す
る超純水オゾン殺菌方法において、前記ユースポイント
と前記一次純水タンク間で前記使用済純水中にオゾンを
注入し、かつ前記一次純水タンクと前記超純水製造装置
間で水素含有ガスを供給して残留オゾン除去及び脱酸素
を行うことを特徴とする超純水オゾン殺菌方法及び該方
法に使用する装置である。According to the present invention, primary pure water in a primary pure water tank is supplied to an ultrapure water producing apparatus containing at least a polisher to form ultrapure water, and the ultrapure water is supplied to a supply line. Ultrapure water ozone that is supplied to the point of use through which water is sent to the point of use to treat the object using the ultrapure water and the used pure water is circulated to the primary pure water tank via a return line. In the sterilization method, ozone is injected into the used pure water between the point of use and the primary pure water tank, and a hydrogen-containing gas is supplied between the primary pure water tank and the ultrapure water producing apparatus to remain. It is an ultrapure water ozone sterilization method characterized by performing ozone removal and deoxidation, and an apparatus used for the method.
【０００９】以下本発明を詳細に説明する。オゾンは塩
素より酸化力が強く、殺菌、脱臭、脱色等に効果を有
し、かつ酸化作用後に酸素に分解し二次公害の問題も生
じないため、近年オゾンの利用範囲が拡大されつつあ
り、半導体洗浄水等の水処理、医療、食品関係等の多方
面でオゾンが使用されている。The present invention will be described in detail below. Ozone has a stronger oxidizing power than chlorine, has an effect on sterilization, deodorization, decolorization, and the like, and since it does not cause the problem of secondary pollution by decomposing into oxygen after the oxidation action, the range of use of ozone is being expanded in recent years, Ozone is used in various fields such as water treatment for semiconductor cleaning water, medical treatment, and food.
【００１０】本発明でもオゾンの有する殺菌力を利用し
て超純水製造及び供給システムの殺菌を行う。本発明に
おける超純水循環システムの適所つまり前記ユースポイ
ントと前記一次純水タンク間で循環する超純水又は純水
（超純水と純水を含めて単に純水と称することがある）
中にオゾン含有ガスを連続的又は間欠的に注入する。こ
れにより前記超純水又は純水がオゾンを含有し従ってこ
の注入地点より下流側のシステム内は実質的に無菌状態
に維持されバクテリア等の発生及び繁殖が抑制される。
しかし本発明のシステムにはオゾンに対する耐性が劣る
超純水製造装置が含まれ、オゾンを含有する前記超純水
又は純水をそのまま供給すると該装置により製造される
超純水の純度が低下して該超純水により処理される被処
理体の品質も低下する。従って本発明では前記一次純水
タンクと前記超純水製造装置間のラインに水素含有ガス
を供給して残留オゾンの除去を行い、実質的にオゾンを
含有しない純水を前記超純水製造装置に供給する。Also in the present invention, the sterilizing power of ozone is utilized to sterilize the ultrapure water production and supply system. Ultrapure water or pure water that circulates between the use point and the primary pure water tank in the proper place of the ultrapure water circulation system of the present invention (the ultrapure water and pure water may be simply referred to as pure water)
Ozone-containing gas is continuously or intermittently injected therein. As a result, the ultrapure water or pure water contains ozone. Therefore, the inside of the system downstream from the injection point is kept substantially sterile, and the generation and propagation of bacteria and the like is suppressed.
However, the system of the present invention includes an ultrapure water production apparatus having poor resistance to ozone, and if the ultrapure water containing ozone or pure water is supplied as it is, the purity of the ultrapure water produced by the apparatus decreases. The quality of the object to be processed by the ultrapure water is also reduced. Therefore, in the present invention, hydrogen-containing gas is supplied to the line between the primary pure water tank and the ultrapure water producing device to remove residual ozone, and pure water containing substantially no ozone is produced in the ultrapure water producing device. Supply to.
【００１１】前記残留オゾンの除去は水素散気装置等を
使用して行うことができる。オゾンや酸素と水素含有ガ
スの反応で水を生成する反応用の触媒を充填した水素散
気装置にオゾンや酸素を含有する純水を噴霧状態で供給
すると該純水中のオゾンや酸素が水素ガスと反応し水と
なって除去される。この水素ガスを使用する残留オゾン
除去では活性炭処理と異なり不純物が混入しにくい。こ
れらの装置と超純水製造装置との間はオゾンが存在せず
バクテリアの発生を抑制できないため、該装置は前記超
純水製造装置の直前に設置してオゾンが存在しないライ
ンをできるだけ短くすることが望ましい。The residual ozone can be removed by using a hydrogen diffuser or the like. When pure water containing ozone or oxygen is supplied in a spray state to a hydrogen diffuser filled with a catalyst for a reaction that produces water by the reaction of ozone or oxygen with a hydrogen-containing gas, the ozone or oxygen in the pure water becomes hydrogen. It reacts with the gas and becomes water and is removed. Unlike the activated carbon treatment, impurities are unlikely to be mixed in when removing residual ozone using hydrogen gas. Since ozone does not exist between these devices and the ultrapure water producing device and the generation of bacteria cannot be suppressed, the device is installed immediately before the ultrapure water producing device to make the ozone-free line as short as possible. Is desirable.
【００１２】本発明で使用するオゾンは不純物を殆ど含
まない高純度オゾンであることが必要である。該オゾン
は酸素ガスに高電圧を印加して酸素の一部をオゾンに変
換する無声放電方式により製造することもできるが、該
方式により製造されるオゾンはパーティクルや金属の混
入がかなりあり、特に電子工業での洗浄用としては望ま
しくない。本発明では前記無声放電方式で得られるオゾ
ンより高純度のオゾンが得られる電気分解方式による酸
素混合オゾンガスを使用することが望ましい。純水を電
気分解して前記酸素−オゾン混合ガスを得るためには、
固体電解質の一方に陽極として耐オゾン性を有する基材
例えばチタン基材上に酸化鉛や酸化スズを被覆した材料
を、又他方に陰極としてステンレスや炭素等を基材とし
白金等の白金族金属を被覆した材料をそれぞれ用い、陽
極に純水を連続的又は間欠的に供給し、陽極／陰極間に
直流電圧を印加すればよい。又オゾンによる殺菌を効果
的に行うためオゾン含有ガスは超純水又は純水中のオゾ
ン濃度が10×10-3〜500 ×10-3ｍｇ／リットル程度とな
るように注入することが望ましい。The ozone used in the present invention must be high-purity ozone containing almost no impurities. The ozone can be produced by a silent discharge method in which a high voltage is applied to oxygen gas to convert a part of oxygen into ozone, but the ozone produced by the method has a considerable amount of particles and metals mixed therein, Not desirable for cleaning in the electronics industry. In the present invention, it is desirable to use an oxygen-mixed ozone gas by an electrolysis method that can obtain ozone of higher purity than the ozone obtained by the silent discharge method. To electrolyze pure water to obtain the oxygen-ozone mixed gas,
A substrate having ozone resistance as an anode on one side of the solid electrolyte, for example, a material in which lead oxide or tin oxide is coated on a titanium substrate, and on the other side a platinum group metal such as platinum using stainless steel or carbon as a substrate as a cathode. It is sufficient to supply pure water to the anode continuously or intermittently and apply a DC voltage between the anode and the cathode by using each of the materials coated with. Further, in order to effectively sterilize with ozone, it is desirable to inject the ozone-containing gas so that the ozone concentration in ultrapure water or pure water will be about 10 × 10 −3 to 500 × 10 −3 mg / liter.
【００１３】前記水素含有ガスとしてボンベの水素ガス
を使用し供給してもよいが、前記電気分解により陰極で
高濃度水素ガスが得られるためこの水素ガスを前記水素
散気装置等に供給することが望ましい。又前記水素散気
装置に供給される水素ガスとラインに注入されるオゾン
ガスとの比は２：１〜５：１の範囲に維持することが望
ましい。Although hydrogen gas in a cylinder may be used as the hydrogen-containing gas and supplied, the hydrogen gas is supplied to the hydrogen diffuser or the like because a high concentration hydrogen gas is obtained at the cathode by the electrolysis. Is desirable. Further, it is desirable to maintain the ratio of the hydrogen gas supplied to the hydrogen diffuser to the ozone gas injected into the line in the range of 2: 1 to 5: 1.
【００１４】次に添付図面に基づいて本発明に係わる超
純水オゾン殺菌方法の一例を説明する。図１は、本発明
方法に係わる超純水オゾン殺菌方法の一例を示すフロー
シートである。蒸留やイオン交換により純水製造装置11
で製造された一次純水はまず一次純水タンク12に貯留さ
れる。この一次純水はその後該タンク12に接続された循
環ポンプ13により水素散気装置15を経て超純水製造装置
16に供給される。Next, an example of the ultrapure water ozone sterilization method according to the present invention will be described with reference to the accompanying drawings. FIG. 1 is a flow sheet showing an example of the ultrapure water ozone sterilization method according to the method of the present invention. Pure water production equipment by distillation or ion exchange 11
The primary pure water produced in step 1 is first stored in the primary pure water tank 12. This primary pure water is then passed through a hydrogen diffuser 15 by a circulation pump 13 connected to the tank 12 and an ultrapure water producing device.
Supplied to 16.
【００１５】前記超純水製造装置16はポリシャー17と精
密濾過装置18から成り、前記純水中の無機物質を前記ポ
リシャー17で除去し、既に存在する有機物粒子等ととも
に前記濾過装置18で除去して超純水を製造する。該超純
水は供給ライン19を通り、図示の例では２ヵ所のユース
ポイント21に並列的に供給され、該ユースポイント21に
おいて電子部品の洗浄等の操作を行い被処理体の処理を
行う。この処理操作で使用されあるいは過剰に供給され
て使用されなかった使用済純水又は未使用超純水は集め
られリターンライン22を通って前記一次純水タンク12に
循環されるが、前記リターンライン22中の使用済純水又
は未使用超純水にはオゾナイザー23で製造されたオゾン
含有ガスが注入される。The ultrapure water producing device 16 comprises a polisher 17 and a microfiltration device 18. The inorganic substance in the pure water is removed by the polisher 17 and removed by the filtration device 18 together with already existing organic particles. To produce ultrapure water. The ultrapure water is supplied to the two use points 21 in parallel in the illustrated example through the supply line 19, and at the use points 21, operations such as cleaning of electronic parts are performed to process the object. Spent pure water or unused ultrapure water used or excessively supplied in this treatment operation is collected and circulated to the primary pure water tank 12 through a return line 22. The ozone-containing gas produced by the ozonizer 23 is injected into the used pure water or unused ultrapure water in 22.
【００１６】一次純水タンク12に循環した純水は同様に
して循環ポンプ13により前述の水素散気装置15に供給さ
れる。この水素散気装置15にはオゾンや酸素の分解触媒
が充填され、該水素散気装置15に供給されるオゾンや酸
素が水素と反応して水を生成して前記オゾンや酸素が純
水中から除去されて前記超純水製造装置16に供給され
る。The pure water circulated in the primary pure water tank 12 is similarly supplied to the hydrogen diffuser 15 by the circulation pump 13. The hydrogen diffuser 15 is filled with a decomposition catalyst for ozone and oxygen, and the ozone and oxygen supplied to the hydrogen diffuser 15 react with hydrogen to generate water, so that the ozone and oxygen are in pure water. And is supplied to the ultrapure water production system 16.
【００１７】このような操作により各ユースポイント21
において被処理体が超純水で処理されるが、供給ライン
19及びリターンライン22中でオゾナイザー23によりオゾ
ン含有ガスが超純水中に注入されるため、システム内を
循環する純水あるいは超純水は水素散気装置15まではオ
ゾンを含み従ってバクテリアの繁殖を抑制して、バクテ
リアを実質的に含まない超純水により各ユースポイント
21での被処理体の処理を行うことを可能にしている。With such an operation, each use point 21
The object is treated with ultrapure water at the supply line
Since ozone-containing gas is injected into the ultrapure water by the ozonizer 23 in the return line 22 and the return line 22, the pure water or ultrapure water circulating in the system contains ozone up to the hydrogen diffuser 15 and therefore the propagation of bacteria. Each point of use is suppressed by ultrapure water that is substantially free of bacteria.
It makes it possible to process the object at 21.
【００１８】[0018]
【実施例】次に本発明による超純水オゾン殺菌の実施例
を記載するが、該実施例は本発明を限定するものではな
い。EXAMPLES Next, examples of ultrapure water ozone sterilization according to the present invention will be described, but the examples do not limit the present invention.
【００１９】[0019]
【実施例１】図１に示したフローチャートに従って超純
水オゾン殺菌を行った。比抵抗が104 Ωｃｍである原水
を純水製造装置内でアニオン及びカチオン交換樹脂と接
触させて不純物を除去し一次純水タンク内に貯留した。
この純水をポリシャーとミクロンフィルター（孔径0.1
μｍ）を含む超純水製造装置に供給して超純水を製造
し、更にこの超純水を半導体基板洗浄工程に供給して洗
浄前の比抵抗、ＴＯＣ、バクテリア数、オゾン濃度及び
溶存酸素量を測定した。その結果を表１に示した。該純
水による洗浄を行い、洗浄後のリターンライン中で前記
電気分解オゾン−酸素混合ガスを１ｍｇ／分で注入した
後、前記一次純水タンクに循環させた。この時点で比抵
抗、ＴＯＣ、バクテリア数、オゾン濃度及び溶存酸素量
を測定し、その結果を表１に示した。この純水を、担体
ポリプロピレン樹脂に触媒金属Ｐｄを10ｍｇ／ｃｍ2 の
割合で担持した触媒を充填した水素散気装置中に20ミリ
リットル／分の割合で噴霧した。該水素散気装置から取
り出された純水中のオゾン濃度は０であった。Example 1 Ultrapure water ozone sterilization was performed according to the flow chart shown in FIG. Raw water having a specific resistance of 10 4 Ωcm was brought into contact with anion and cation exchange resins in a pure water production apparatus to remove impurities and stored in a primary pure water tank.
Use this pure water with polisher and micron filter (pore size 0.1
micrometer) to produce ultrapure water, which is then supplied to the semiconductor substrate cleaning step to obtain specific resistance before cleaning, TOC, number of bacteria, ozone concentration and dissolved oxygen. The quantity was measured. The results are shown in Table 1. After cleaning with pure water, the electrolyzed ozone-oxygen mixed gas was injected at 1 mg / min in the return line after cleaning, and then circulated in the primary pure water tank. At this time, the specific resistance, TOC, number of bacteria, ozone concentration and dissolved oxygen amount were measured, and the results are shown in Table 1. This pure water was sprayed at a rate of 20 ml / min into a hydrogen diffuser filled with a catalyst in which a carrier polypropylene resin was loaded with a catalytic metal Pd at a rate of 10 mg / cm 2 . The ozone concentration in pure water taken out from the hydrogen diffuser was 0.
【００２０】[0020]
【比較例１】オゾン注入を行わずかつ水素散気装置を設
置しなかったこと以外は実施例１と同じ装置を使用して
超純水オゾン殺菌を行い、一次純水タンク内及びユース
ポイントでの超純水又は純水の比抵抗、ＴＯＣ、バクテ
リア数、オゾン濃度及び溶存酸素量を測定した。その結
果を表１に示した。表１から、ユースポイントでのＴＯ
Ｃ、溶存酸素及びバクテリア数が実施例１では大きく減
少していること判る。[Comparative Example 1] Ultrapure water ozone sterilization was performed using the same apparatus as in Example 1 except that ozone was not injected and a hydrogen diffuser was not installed, and the ultrapure water ozone was sterilized in the primary pure water tank and at the point of use. The specific resistance, TOC, number of bacteria, ozone concentration, and dissolved oxygen amount of ultrapure water or pure water were measured. The results are shown in Table 1. From Table 1, TO at the point of use
It can be seen that C, dissolved oxygen and the number of bacteria are greatly reduced in Example 1.
【００２１】[0021]
【表１】 [Table 1]
【００２２】[0022]
【発明の効果】本発明は、一次純水タンク中の一次純水
を少なくともポリシャーを含む超純水製造装置に供給し
て超純水とし、該超純水を供給ラインを経由してユース
ポイントに送水し該ユースポイントで前記超純水を使用
して被処理体を処理し、使用済純水をリターンラインを
経由して前記一次純水タンクに循環する超純水オゾン殺
菌方法において、前記ユースポイントと前記一次純水タ
ンク間で前記使用済純水中にオゾン含有ガスを注入し、
かつ前記一次純水タンクと前記超純水製造装置間で水素
含有ガスを供給して残留オゾン除去及び脱酸素を行うこ
とを特徴とする超純水オゾン殺菌方法及び該方法に使用
できる装置である。According to the present invention, the primary pure water in the primary pure water tank is supplied to an ultrapure water producing apparatus containing at least a polisher to obtain ultrapure water, and the ultrapure water is passed through a supply line to a use point. In the ultrapure water ozone sterilization method in which the ultrapure water is used to treat the object to be treated at the point of use and the used pure water is circulated to the primary pure water tank through a return line, Injecting ozone-containing gas into the used pure water between the point of use and the primary pure water tank,
Further, there is provided an ultrapure water ozone sterilization method characterized in that a hydrogen-containing gas is supplied between the primary pure water tank and the ultrapure water production apparatus to perform residual ozone removal and deoxidation, and an apparatus usable for the method. .
【００２３】従って本発明では、オゾン注入部より下流
側の水素散気装置までに位置する超純水又は純水中にオ
ゾンが存在しバクテリア等の発生及び繁殖を防止して、
運転を停止することなく超純水中のバクテリア濃度を実
質的に零にする。従って該超純水により処理される被処
理体の品質が向上して超純水の処理能力が最大限に発揮
される。しかもオゾンに対する耐性に乏しい前記超純水
製造装置の上流側に水素含有ガスを供給して残留オゾン
を水に変換して除去するようにしてあるため、超純水製
造装置の超純水製造能力が損なわれることがない。Therefore, in the present invention, ozone is present in ultrapure water or pure water located up to the hydrogen diffuser on the downstream side of the ozone injecting section to prevent the generation and propagation of bacteria and the like,
The bacteria concentration in ultrapure water is made substantially zero without stopping the operation. Therefore, the quality of the object to be treated by the ultrapure water is improved and the treatment capacity of the ultrapure water is maximized. Moreover, since a hydrogen-containing gas is supplied to the upstream side of the ultrapure water production system, which has poor resistance to ozone, to convert residual ozone into water and remove it, the ultrapure water production capability of the ultrapure water production system. Is not damaged.
【図１】本発明による超純水オゾン殺菌の要領を例示す
るフローシート。FIG. 1 is a flow sheet illustrating the procedure of ultrapure water ozone sterilization according to the present invention.
【図２】従来技術による超純水オゾン殺菌の要領を例示
するフローシート。FIG. 2 is a flow sheet illustrating the procedure of ultrapure water ozone sterilization according to a conventional technique.
11・・・純水製造装置 12・・・一次純水タンク 13・
・・循環ポンプ 15・・・水素散気装置 16・・・超純
水製造装置 17・・・ポリシャー 18・・・精密濾過装
置 19・・・供給ライン 21・・・ユースポイント 22
・・・リターンライン 23・・・オゾナイザー11 ・ ・ ・ Pure water production system 12 ・ ・ ・ Primary pure water tank 13 ・
・ ・ Circulation pump 15 ・ ・ ・ Hydrogen aeration device 16 ・ ・ ・ Ultrapure water production device 17 ・ ・ ・ Pollisher 18 ・ ・ ・ Microfiltration device 19 ・ ・ ・ Supply line 21 ・ ・ ・ Use point 22
... Return line 23 ... Ozonizer
フロントページの続き (51)Int.Cl.6 識別記号 庁内整理番号 ＦＩ 技術表示箇所 Ｃ０２Ｆ 1/50 ５５０ Ｈ 9045−4Ｄ Continuation of front page (51) Int.Cl. 6 Identification number Office reference number FI technical display location C02F 1/50 550 H 9045-4D
Claims (3)
もポリシャーを含む超純水製造装置に供給して超純水と
し、該超純水を供給ラインを経由してユースポイントに
送水し該ユースポイントで前記超純水を使用して被処理
体を処理し、使用済純水をリターンラインを経由して前
記一次純水タンクに循環する超純水オゾン殺菌方法にお
いて、前記ユースポイントと前記一次純水タンク間で前
記使用済純水中にオゾン含有ガスを注入し、かつ前記一
次純水タンクと前記超純水製造装置間に水素含有ガスを
供給して残留オゾン除去及び脱酸素を行うことを特徴と
する超純水オゾン殺菌方法。1. The primary pure water in the primary pure water tank is supplied to an ultrapure water producing apparatus containing at least a polisher to obtain ultrapure water, and the ultrapure water is sent to a point of use via a supply line. In the ultrapure water ozone sterilization method of treating an object to be treated with the ultrapure water at a use point and circulating the used pure water to the primary pure water tank through a return line, the use point and the An ozone-containing gas is injected into the used pure water between primary pure water tanks, and a hydrogen-containing gas is supplied between the primary pure water tank and the ultrapure water producing apparatus to remove residual ozone and deoxidize. An ultrapure water ozone sterilization method characterized by the above.
ガスであり、水素含有ガスが水電解で生成する陰極ガス
である請求項１に記載の方法。2. The method according to claim 1, wherein the ozone-containing gas is an anode gas produced by water electrolysis and the hydrogen-containing gas is a cathode gas produced by water electrolysis.
一次純水タンクの下流側に位置し前記一次純水を超純水
にするポリシャーを含む超純水製造装置、該超純水製造
装置から供給ラインを通して供給される前記超純水で被
処理体を処理する１又は２以上のユースポイント、該ユ
ースポイントでの使用済純水を前記一次純水タンクへ循
環するリターンラインを含んで成る超純水オゾン殺菌装
置において、前記ユースポイントと前記一次純水タンク
間に前記使用済純水中にオゾン含有ガスを注入するオゾ
ン注入部及び前記一次純水タンクと前記超純水製造装置
間に水素含有ガスを供給して前記一次純水中に含有され
るオゾンを除去し脱酸素を行う水素散気装置を有するこ
とを特徴とする超純水オゾン殺菌装置。3. An ultrapure water production apparatus including a primary pure water tank for storing primary pure water, a polisher located downstream of the primary pure water tank for converting the primary pure water into ultrapure water, and the ultrapure water. It includes one or more use points for treating the object with the ultrapure water supplied from the manufacturing apparatus through the supply line, and a return line for circulating the used pure water at the use points to the primary pure water tank. In the ultrapure water ozone sterilizer, the ozone injection unit for injecting an ozone-containing gas into the used pure water between the point of use and the primary pure water tank, the primary pure water tank, and the ultrapure water producing apparatus. An ultrapure water ozone sterilizer having a hydrogen diffusing device for supplying oxygen between the primary pure water to remove ozone contained in the primary pure water and deoxidize the ozone.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18925193A JPH0716581A (en) | 1993-06-30 | 1993-06-30 | Method for sterilizing ultrapure water with ozone and device therefor |
| US08/266,588 US5447640A (en) | 1993-06-28 | 1994-06-28 | Method and apparatus for sterilization of and treatment with ozonized water |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP18925193A JPH0716581A (en) | 1993-06-30 | 1993-06-30 | Method for sterilizing ultrapure water with ozone and device therefor |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH0716581A true JPH0716581A (en) | 1995-01-20 |
Family
ID=16238167
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP18925193A Pending JPH0716581A (en) | 1993-06-28 | 1993-06-30 | Method for sterilizing ultrapure water with ozone and device therefor |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0716581A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6183646B1 (en) | 1995-07-19 | 2001-02-06 | Baker Hughes Incorporated | Biofouling reduction |
| JP2001038364A (en) * | 1999-08-02 | 2001-02-13 | Kurita Water Ind Ltd | Sterilization method and device for ultrapure water production and feed device |
| JP2012096187A (en) * | 2010-11-04 | 2012-05-24 | Sumitomo Metal Mining Co Ltd | Ultrapure water production system, method for washing the same, and method for producing ultrapure water using the same |
-
1993
- 1993-06-30 JP JP18925193A patent/JPH0716581A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6183646B1 (en) | 1995-07-19 | 2001-02-06 | Baker Hughes Incorporated | Biofouling reduction |
| JP2001038364A (en) * | 1999-08-02 | 2001-02-13 | Kurita Water Ind Ltd | Sterilization method and device for ultrapure water production and feed device |
| JP2012096187A (en) * | 2010-11-04 | 2012-05-24 | Sumitomo Metal Mining Co Ltd | Ultrapure water production system, method for washing the same, and method for producing ultrapure water using the same |
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