JP2002151459A - Cleaning method - Google Patents
Cleaning methodInfo
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- JP2002151459A JP2002151459A JP2000343865A JP2000343865A JP2002151459A JP 2002151459 A JP2002151459 A JP 2002151459A JP 2000343865 A JP2000343865 A JP 2000343865A JP 2000343865 A JP2000343865 A JP 2000343865A JP 2002151459 A JP2002151459 A JP 2002151459A
- Authority
- JP
- Japan
- Prior art keywords
- ultrapure water
- cleaning
- water production
- gas
- fine particles
- Prior art date
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Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
- Cleaning Or Drying Semiconductors (AREA)
- Cleaning In General (AREA)
- Cleaning By Liquid Or Steam (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は超純水製造システム
の洗浄方法に関し、特に半導体製造プロセスの洗浄に好
適な洗浄方法に関する。また、本発明は、濾過膜、特に
限外濾過膜の洗浄に好適な洗浄方法に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a cleaning method for an ultrapure water production system, and more particularly to a cleaning method suitable for cleaning a semiconductor manufacturing process. The present invention also relates to a washing method suitable for washing a filtration membrane, particularly an ultrafiltration membrane.
【０００２】[0002]
【従来の技術及び先行技術】従来、半導体製造等の分野
における洗浄工程では、洗浄水として超純水が用いられ
ている。この超純水としては、洗浄トラブルの原因とな
る微粒子、有機物や無機物を含まないことが要求され、
例えば抵抗率：１８．２ＭΩ・ｃｍ以上、微粒子：１個
／ｍＬ以下、生菌：１個／Ｌ以下、ＴＯＣ (Total Orga
nic Carbon)：１μｇ／Ｌ以下、シリカ：１μｇ／Ｌ以
下、金属類：１ｎｇ／Ｌ以下、イオン類：１０ｎｇ／Ｌ
以下であることが要求水質となっている。2. Description of the Related Art Conventionally, ultrapure water has been used as cleaning water in a cleaning process in the field of semiconductor manufacturing and the like. As this ultrapure water, it is required that it does not contain fine particles, organic substances and inorganic substances that cause cleaning troubles,
For example, resistivity: 18.2 MΩ · cm or more, fine particles: 1 / mL or less, viable bacteria: 1 / L or less, TOC (Total Orga)
nic Carbon): 1 μg / L or less, silica: 1 μg / L or less, metals: 1 ng / L or less, ions: 10 ng / L
The required water quality is as follows.
【０００３】そして、上述した超純水の使用場所（ユー
スポイント）は、超純水製造装置と配管（流路）で接続
され、このユースポイントで使用されなかった残余の超
純水は別の流路を介して前記超純水製造装置に戻される
ことにより循環系が形成され、全体として超純水製造シ
ステムが構成されている。[0003] The above-mentioned use place (use point) of the ultrapure water is connected to the ultrapure water production apparatus by a pipe (flow path), and the remaining ultrapure water not used at this use point is separated into another. A circulation system is formed by returning to the ultrapure water production device via the flow path, and an ultrapure water production system is configured as a whole.
【０００４】ところで、上記超純水製造システムを新規
に建設したり長期間休止させた場合には、このシステム
内に、空気中のチリやシリカやアルミ等の微粒子や、バ
クテリアの死骸、鉄さびなどの水中に含まれる粒子、更
には製造工程で生じる膜や配管等の削り屑など（以下、
これらを「微粒子」と総称する）が混入して超純水の水
質が低下する。このため、適宜システム内の洗浄を行う
ことが必要となるが、この微粒子の洗浄除去は容易では
なく、洗浄に要する時間が長いことが、装置の稼動効率
低下の要因となっている。特に、工場の建設に伴って上
記システムを新設する場合、その施工時に微粒子がシス
テムの内部に付着することから、これを除去するための
洗浄作業が長期化し（例えば１カ月）、工場の稼動率が
低下している。When the above ultrapure water production system is newly constructed or suspended for a long period of time, fine particles such as dust and silica in the air, dead bacteria, iron rust and the like are contained in the system. Particles contained in water, as well as shavings such as films and pipes generated in the manufacturing process (hereinafter, referred to as
These are collectively referred to as “fine particles”) and the quality of ultrapure water is reduced. For this reason, it is necessary to appropriately clean the inside of the system. However, it is not easy to clean and remove the fine particles, and the long time required for the cleaning causes a reduction in the operation efficiency of the apparatus. In particular, when the above-mentioned system is newly established along with the construction of a factory, fine particles adhere to the inside of the system at the time of the construction, so that the cleaning work for removing the particles is lengthened (for example, one month), and the operation rate of the factory is increased. Is declining.
【０００５】このようなことから、超純水製造システム
を洗浄してから所定の要求水質を満たす超純水が得られ
るまでの時間を短縮すること（超純水製造システムの垂
直立上げ）が要望されており、洗浄効率を高めるため
に、例えば洗浄水として温水や過酸化水素水を用いるこ
とが行われている。また、特開平７−１９５０７３号公
報には、洗浄力の大きいアルコールを用いた洗浄方法が
提案されている。[0005] Therefore, it is necessary to shorten the time from cleaning the ultrapure water production system to obtaining ultrapure water satisfying the required water quality (vertical start-up of the ultrapure water production system). In order to increase the cleaning efficiency, for example, hot water or hydrogen peroxide water is used as cleaning water. Further, Japanese Patent Application Laid-Open No. 7-195073 proposes a cleaning method using alcohol having a high detergency.
【０００６】しかしながら、温水や過酸化水素では、洗
浄力が十分ではないため、超純水製造システムの配管等
に付着した微粒子を十分な洗浄効率で除去することはで
きない。However, warm water or hydrogen peroxide does not have sufficient cleaning power, so that fine particles adhering to a pipe or the like of an ultrapure water production system cannot be removed with sufficient cleaning efficiency.
【０００７】一方、洗浄にアルコールを用いた場合、微
粒子を十分に除去するためにはアルコールを比較的高濃
度（約１０〜８０％）とする必要があり、そのため、洗
浄後に超純水製造システム内にアルコールが残留して水
質の低下（ＴＯＣの増大）を招く可能性がある。従っ
て、残留アルコールを除去するための時間が必要とな
り、結果として洗浄時間の短縮は困難であった。On the other hand, when alcohol is used for cleaning, it is necessary to make the alcohol have a relatively high concentration (about 10 to 80%) in order to sufficiently remove the fine particles. There is a possibility that the alcohol remains in the water and lowers the water quality (increases TOC). Therefore, it takes time to remove the residual alcohol, and as a result, it has been difficult to shorten the cleaning time.
【０００８】ところで、超純水製造装置を構成する濾過
膜装置に用いられる限外濾過膜などの濾過膜は、製造時
や濾過膜装置の超純水製造装置への取り付け時に超純水
により洗浄される。この洗浄に当っては、比抵抗率、Ｔ
ＯＣにより洗浄の終点が判断されている。現状において
は、これらの指標に影響を与える物質についてはほぼ満
足できる洗浄効果が得られているが、これらの指標には
影響を及ぼさない微粒子については必ずしも十分な洗浄
が行われているとは言えず、膜表面に付着した微粒子が
徐々に流出して超純水の水質が低下するという問題があ
った。Meanwhile, a filtration membrane such as an ultrafiltration membrane used in a filtration membrane apparatus constituting an ultrapure water production apparatus is washed with ultrapure water at the time of production or when the filtration membrane apparatus is attached to the ultrapure water production apparatus. Is done. In this cleaning, the specific resistance, T
The end point of the cleaning is determined by the OC. At present, almost satisfactory cleaning effects are obtained for substances that affect these indices, but fine particles that do not affect these indices are not necessarily sufficiently cleaned. However, there is a problem that the fine particles adhering to the film surface gradually flow out and the quality of the ultrapure water deteriorates.
【０００９】上記従来の問題点を解決し、洗浄力（微粒
子の除去能力）に優れると共に、洗浄後のシステム内に
洗浄液中の成分が残留することが少ないことから、洗浄
に要する時間を短縮することができ、従って、超純水製
造装置の垂直立上げが可能な超純水製造システムの洗浄
方法、及び、洗浄力に優れ、短時間で効率的に濾過膜を
洗浄する方法として、本出願人は先に、超純水製造シス
テムの超純水との接触面に付着した微粒子の表面電位を
変化させることにより、この微粒子を除去する超純水製
造システムの洗浄方法と、濾過膜に付着した微粒子の表
面電位を変化させることにより、この微粒子を除去する
濾過膜の洗浄方法を提案した（特願２０００−２４２６
０２（以下「先願」という。））。[0009] The above-mentioned conventional problems are solved, and the cleaning time (the ability to remove fine particles) is excellent, and the time required for cleaning is reduced because the components in the cleaning solution hardly remain in the system after cleaning. The present invention relates to a method for cleaning an ultrapure water production system capable of vertically starting an ultrapure water production apparatus and a method for efficiently cleaning a filtration membrane in a short time with excellent detergency. The person first changes the surface potential of the fine particles attached to the contact surface of the ultrapure water production system with the ultrapure water, thereby removing the particles and cleaning the ultrapure water production system. A method for cleaning a filtration membrane that removes the fine particles by changing the surface potential of the fine particles has been proposed (Japanese Patent Application No. 2000-2426).
02 (hereinafter referred to as “first application”)).
【００１０】上記先願の方法において、微粒子の表面電
位を変化させる手段としては、具体的には塩基性溶液を
用いて洗浄する方法が採用されている。In the method of the prior application, as a means for changing the surface potential of the fine particles, specifically, a method of washing with a basic solution is employed.
【００１１】この先願の方法における微粒子除去の原理
は以下の通りである。The principle of removing fine particles in the method of the prior application is as follows.
【００１２】即ち、超純水製造システムの配管等に付着
した微粒子は、その表面電位により配管などと電気的つ
まり静電的に付着している。一般に、洗浄液などの溶液
中における微粒子の表面電位は、その液性により変化す
るが、特に溶液のｐＨを変化させることによって顕著に
変化させることができ、液のｐＨをアルカリ性側に変化
させることによって微粒子はマイナスに帯電し、かつ、
その電荷も増大する。一方、超純水製造システムの配管
系等を構成しているＰＶＣ（ポリ塩化ビニル）やＰＰＳ
（ポリフェニレンサルファイド）など、或いは限外濾過
膜を構成しているポリスルホンなどの有機高分子材料
は、表面電位の変化を起こさず、接触する液体のｐＨ変
化に関係なくマイナス荷電を有する。従って、接触する
液体のｐＨをアルカリ性に変化させることにより、マイ
ナスに帯電した微粒子がシステム構成材料と電気的に反
発して剥離、除去しやすくなる。That is, the fine particles adhering to the pipes and the like of the ultrapure water production system are electrically or electrostatically attached to the pipes and the like due to the surface potential. In general, the surface potential of fine particles in a solution such as a washing solution changes depending on its liquidity, but it can be significantly changed particularly by changing the pH of the solution, and by changing the pH of the solution to the alkaline side. The particles are negatively charged, and
Its charge also increases. On the other hand, PVC (polyvinyl chloride) and PPS which constitute the piping system etc. of the ultrapure water production system
(Polyphenylene sulfide) or an organic polymer material such as polysulfone constituting an ultrafiltration membrane does not cause a change in surface potential and has a negative charge irrespective of a change in pH of a contacting liquid. Therefore, by changing the pH of the liquid to be contacted to alkaline, the negatively charged fine particles are easily repelled from the system constituent materials, and thus are easily separated and removed.
【００１３】そして、この剥離、除去作用は、洗浄液と
して用いる塩基性溶液の濃度が低くても（例えば数１０
ｍｇ／Ｌ）十分に発揮される。従って、洗浄液を低濃度
とすることができる。そのため、洗浄液の成分がシステ
ム内に残留する割合が少なくなり、この成分に由来して
ＴＯＣが増大することも抑制される。その結果、洗浄作
業を短時間で終了させることができ、超純水製造システ
ムの垂直立上げが可能となる。[0013] This peeling and removing action can be performed even when the concentration of the basic solution used as the cleaning solution is low (for example, several tens of
(mg / L). Therefore, the concentration of the cleaning liquid can be reduced. Therefore, the ratio of the components of the cleaning liquid remaining in the system is reduced, and the increase in TOC due to the components is also suppressed. As a result, the cleaning operation can be completed in a short time, and the vertical startup of the ultrapure water production system can be performed.
【００１４】[0014]
【発明が解決しようとする課題】上記先願の方法は、微
粒子の除去能力に優れているので、超純水製造システム
や濾過膜に付着した微粒子を速やかに剥離、除去するこ
とができる。しかも、洗浄液は低濃度であるため、洗浄
後に洗浄液中の成分が残留してＴＯＣを増大させること
も少ない。このため、洗浄作業を短時間で行うことが可
能であるが、より一層の洗浄効率の向上、洗浄時間の短
縮が望まれているのが現状である。Since the method of the prior application is excellent in the ability to remove fine particles, the fine particles adhering to the ultrapure water production system or the filtration membrane can be quickly separated and removed. In addition, since the cleaning solution has a low concentration, it is unlikely that the components in the cleaning solution remain after cleaning and increase the TOC. For this reason, the cleaning operation can be performed in a short time, but at present, it is desired to further improve the cleaning efficiency and shorten the cleaning time.
【００１５】従って、本発明は、上先願の洗浄効果をよ
り一層高める洗浄方法を提供することを目的とする。Accordingly, an object of the present invention is to provide a cleaning method which further enhances the cleaning effect of the earlier application.
【００１６】[0016]
【課題を解決するための手段】請求項１の超純水製造シ
ステムの洗浄方法は、超純水製造装置、超純水のユース
ポイント、並びに前記超純水製造装置と前記ユースポイ
ントとを接続する超純水の流路からなる超純水製造シス
テムの超純水接触面に付着した微粒子を除去する洗浄方
法において、微細気泡を共存させた塩基性溶液で前記超
純水製造システムの少なくとも一部を洗浄することを特
徴とする。According to a first aspect of the present invention, there is provided a method of cleaning an ultrapure water production system, comprising the steps of connecting an ultrapure water production apparatus, an ultrapure water use point, and the ultrapure water production apparatus to the use point. In the cleaning method for removing fine particles adhered to the ultrapure water contact surface of the ultrapure water production system comprising the ultrapure water flow path, at least one of the ultrapure water production systems is treated with a basic solution in which microbubbles coexist. It is characterized in that the part is washed.
【００１７】請求項２の濾過膜の洗浄方法は、濾過膜の
洗浄方法において、微細気泡を共存させた塩基性溶液で
前記濾過膜を洗浄することを特徴とする。The method for cleaning a filtration membrane according to a second aspect is characterized in that in the method for cleaning a filtration membrane, the filtration membrane is washed with a basic solution in which fine bubbles coexist.
【００１８】前述の如く、超純水製造システムの配管等
に付着した微粒子の表面電位は、水中において液性によ
り変化し、特にｐＨを変化させることにより顕著に変化
させることが可能である。一方で、超純水製造システム
を構成している有機高分子材料（ＰＶＣ、ＰＰＳ等）
は、表面電位の変化を起こさず、マイナス荷電を有す
る。従って、液性をアルカリ性に変化させて微粒子をマ
イナスに帯電させることにより、付着した微粒子は、マ
イナス荷電の構成材料と反発して剥離されやすくなる。As described above, the surface potential of the fine particles adhering to the piping or the like of the ultrapure water production system changes due to the liquidity in water, and can be significantly changed by changing the pH in particular. On the other hand, the organic polymer materials (PVC, PPS, etc.) that make up the ultrapure water production system
Has no change in surface potential and has a negative charge. Therefore, by changing the liquid property to alkaline and charging the fine particles negatively, the adhered fine particles are easily repelled from the negatively charged constituent material and easily peeled off.
【００１９】この状況において、液中に溶存ガスを混在
させると、微粒子表面は疎水性であるため、表面にガス
の吸着が起こる。この吸着量が増加すると微細気泡が発
生し、これが微粒子表面を覆い、配管等の表面と微粒子
との間に隙間ができる。このため、配管等に付着した微
粒子をより一層効果的に剥離、除去することができるよ
うになる。In this situation, if a dissolved gas is mixed in the liquid, the gas is adsorbed on the surface of the fine particles because the surface of the fine particles is hydrophobic. When the amount of adsorption increases, fine bubbles are generated, which cover the surface of the fine particles, and a gap is formed between the surface of a pipe or the like and the fine particles. For this reason, the fine particles adhering to the pipe or the like can be more effectively peeled and removed.
【００２０】このように本発明では、塩基性溶液を用い
ることによる電気的な剥離作用と、微細気泡による物理
的な剥離作用とで、先願の方法よりも更に極めて効果的
な洗浄を行える。As described above, according to the present invention, an extremely effective cleaning can be performed by the electric peeling action by using the basic solution and the physical peeling action by the fine bubbles as compared with the method of the prior application.
【００２１】本発明において、塩基性溶液に微細気泡を
共存させる方法としては、塩基性溶液に過酸化水素、炭
酸ガス、酸素ガス、水素ガス、及び窒素ガスよりなる群
から選ばれる１種又は２種以上を注入する方法が好適で
ある。また、塩基性溶液としては、超純水に、アンモニ
ア、アンモニウム化合物、アルカリ金属の水酸化物及び
アルカリ金属の酸化物よりなる群から選ばれる１種又は
２種以上を溶解させたものが好適である。In the present invention, as a method for causing fine bubbles to coexist in the basic solution, one or two selected from the group consisting of hydrogen peroxide, carbon dioxide gas, oxygen gas, hydrogen gas, and nitrogen gas can be used in the basic solution. A method of injecting more than a seed is preferred. Further, as the basic solution, one obtained by dissolving one or more selected from the group consisting of ammonia, an ammonium compound, an alkali metal hydroxide and an alkali metal oxide in ultrapure water is preferable. is there.
【００２２】[0022]
【発明の実施の形態】以下に本発明の実施の形態を詳細
に説明する。Embodiments of the present invention will be described below in detail.
【００２３】本発明において、洗浄液として用いる塩基
性溶液としては、超純水に、アンモニア、アンモニウム
化合物、アルカリ金属の水酸化物及びアルカリ金属の酸
化物よりなる群から選ばれる１種又は２種以上を溶解さ
せたもの、特に、アンモニア、アンモニウム塩、テトラ
アルキルアンモニウム化合物、水酸化ナトリウム、水酸
化カリウムなどを超純水に溶解させたものを好適に用い
ることができる。In the present invention, the basic solution used as the cleaning solution may be one or more selected from the group consisting of ultrapure water, ammonia, ammonium compounds, alkali metal hydroxides and alkali metal oxides. In particular, those in which ammonia, ammonium salts, tetraalkylammonium compounds, sodium hydroxide, potassium hydroxide, and the like are dissolved in ultrapure water can be preferably used.
【００２４】塩基性溶液として、このようなアンモニア
水又は水酸化ナトリウム等の水溶液を使用する場合は、
そのｐＨを７〜１４、特に９〜１１に設定することが好
ましい。When such an aqueous solution of ammonia water or sodium hydroxide is used as the basic solution,
It is preferable to set the pH at 7-14, especially at 9-11.
【００２５】また、これらの濃度は、低過ぎると微粒子
の剥離効果を十分に得ることができず、高過ぎると洗浄
液成分の残留の問題が生じ、これを除去するための洗浄
時間が長くなる。超純水製造システムを洗浄する際に
は、例えば、アンモニア水の場合は５〜５００ｍｇ／
Ｌ、特に５０〜１００ｍｇ／Ｌとすることが好ましく、
水酸化ナトリウム水溶液の場合は０．０１〜４０００ｍ
ｇ／Ｌ、特に０．４〜４０ｍｇ／Ｌの範囲に設定するこ
とが好ましい。On the other hand, if the concentration is too low, the effect of removing fine particles cannot be sufficiently obtained, and if the concentration is too high, there is a problem that cleaning liquid components remain, and the cleaning time for removing these components becomes long. When cleaning the ultrapure water production system, for example, in the case of ammonia water, 5 to 500 mg /
L, particularly preferably 50 to 100 mg / L,
In the case of sodium hydroxide aqueous solution, 0.01-4000m
g / L, particularly preferably in the range of 0.4 to 40 mg / L.
【００２６】また、限外濾過膜などの濾過膜を洗浄する
際は、アンモニア水の場合は２０〜２０００ｍｇ／Ｌ、
特に１００〜１０００ｍｇ／Ｌとすることが好ましく、
水酸化ナトリウムの場合は０．４〜１００００ｍｇ／
Ｌ、特に１００〜１０００ｍｇ／Ｌの範囲に設定するこ
とが好ましい。Further, when washing a filtration membrane such as an ultrafiltration membrane, in the case of aqueous ammonia, 20 to 2000 mg / L,
Particularly, it is preferable to be 100 to 1000 mg / L,
In the case of sodium hydroxide, 0.4 to 10,000 mg /
L, particularly preferably in the range of 100 to 1000 mg / L.
【００２７】このような塩基性溶液に微細気泡を共存さ
せる方法としては、塩基性溶液に過酸化水素、炭酸ガ
ス、酸素ガス、水素ガス、及び窒素ガスよりなる群から
選ばれる１種又は２種以上を注入する方法が好適であ
る。As a method for causing fine bubbles to coexist in such a basic solution, one or two types selected from the group consisting of hydrogen peroxide, carbon dioxide gas, oxygen gas, hydrogen gas, and nitrogen gas are used in the basic solution. The method of injecting the above is preferable.
【００２８】塩基性溶液にガスを注入する場合、ガスの
注入量は、システムの運転圧力、使用するガスの種類に
よっても異なるが、水素ガスであれば０．１〜１００ｐ
ｐｍ程度溶存させることが好ましい。また、過酸化水素
はその自己分解で酸素ガスを発生させるものであるが、
過酸化水素を用いる場合には、１００〜１０００ｍｇ／
Ｌ程度添加することが好ましい。なお、過酸化水素を用
いた場合には、微粒子の剥離作用の向上効果のみなら
ず、殺菌効果も得ることができ、好ましい。When injecting a gas into the basic solution, the amount of gas to be injected varies depending on the operating pressure of the system and the type of gas used.
It is preferable to dissolve about pm. Hydrogen peroxide generates oxygen gas by its self-decomposition,
When using hydrogen peroxide, 100 to 1000 mg /
It is preferable to add about L. In addition, when hydrogen peroxide is used, not only the effect of improving the action of separating fine particles but also the effect of sterilization can be obtained, which is preferable.
【００２９】微細気泡を共存させるための上記ガスや過
酸化水素の添加量が少ないと十分量の微細気泡が発生せ
ず、微細気泡による微粒子の剥離性の向上効果が十分に
得られない。逆に、多過ぎても不経済である上に、ガス
のかたまりが発生して洗浄不良となる問題を生じる。If the amount of the gas or hydrogen peroxide for coexisting the fine bubbles is small, a sufficient amount of the fine bubbles is not generated, and the effect of improving the removability of the fine particles by the fine bubbles cannot be sufficiently obtained. On the other hand, if it is too much, it is uneconomical, and there is a problem that a gas lump is generated and cleaning becomes defective.
【００３０】なお、本発明においては、洗浄中の塩基性
溶液内に微細気泡を共存させるものであるため、洗浄中
の塩基性溶液中に微細気泡が存在するように、配管等の
洗浄対象系内の圧力条件下で飽和溶解度以上となるよう
にガス（又は過酸化水素）を注入することが必要とな
る。In the present invention, since fine bubbles coexist in the basic solution being cleaned, the system to be cleaned such as a pipe or the like is so arranged that the fine bubbles are present in the basic solution being cleaned. It is necessary to inject a gas (or hydrogen peroxide) so as to have a saturation solubility or higher under the internal pressure conditions.
【００３１】従って、例えば、塩基性溶液に高圧下でガ
スを注入し（この状態では、ガスは塩基性溶液中に溶解
して微細気泡は存在しない）、洗浄ポイントで脱圧して
微細気泡を発生させたり、或いは、洗浄ポイントで温度
を上げることにより、溶解している過酸化水素の自己分
解を促して微細気泡を発生させるなどの方法を採用する
ことにより、洗浄対象系内において微細気泡を共存させ
るようにする。Therefore, for example, a gas is injected into a basic solution under high pressure (in this state, the gas is dissolved in the basic solution and no fine bubbles are present), and depressurized at a washing point to generate fine bubbles. Or by raising the temperature at the cleaning point to promote the self-decomposition of the dissolved hydrogen peroxide to generate microbubbles, so that microbubbles coexist in the system to be cleaned. Let it do.
【００３２】なお、この微細気泡の粒径は１〜１００μ
ｍ程度であることが好ましく、また、ガス洗浄液中の発
生量は洗浄ポイントにおいて０．１〜１０体積％、特に
１〜１０体積％であることが望ましい。The fine bubbles have a particle size of 1 to 100 μm.
m, and the amount generated in the gas cleaning solution is preferably 0.1 to 10% by volume, particularly 1 to 10% by volume at the cleaning point.
【００３３】本発明では、洗浄対象系内で微細気泡が共
存する塩基性溶液を用いて、超純水製造システムにおい
て配管などに付着した微粒子の洗浄除去或いは、医薬品
製造装置などに用いられる濾過膜装置の限外濾過膜など
の濾過膜に付着した微粒子の洗浄除去を行う。According to the present invention, a basic solution in which microbubbles coexist in a system to be cleaned is used to wash and remove fine particles adhering to a pipe or the like in an ultrapure water production system, or a filtration membrane used in a pharmaceutical manufacturing apparatus or the like. The fine particles attached to the filtration membrane such as the ultrafiltration membrane of the apparatus are washed and removed.
【００３４】以下に図面を参照して、本発明の超純水製
造システムの洗浄方法の実施の形態を説明する。Hereinafter, an embodiment of a cleaning method for an ultrapure water production system according to the present invention will be described with reference to the drawings.
【００３５】図１は、本発明による超純水製造システム
の洗浄方法の実施の形態を示す系統図である。この超純
水製造システム１は、超純水製造装置２、超純水のユー
スポイント４、及びこれらを接続する超純水の流路６
ａ，６ｂから成っている。そして、超純水製造装置２で
製造された超純水は流路６ａを介してユースポイント４
へ送られて該ユースポイント４でその一部が使用され、
未使用の超純水は流路６ｂを経て超純水製造装置２に戻
る循環系をなしている。FIG. 1 is a system diagram showing an embodiment of a cleaning method for an ultrapure water production system according to the present invention. The ultrapure water production system 1 includes an ultrapure water production apparatus 2, an ultrapure water use point 4, and an ultrapure water flow path 6 connecting these.
a, 6b. Then, the ultrapure water produced by the ultrapure water production apparatus 2 is used at the point of use 4 through the flow path 6a.
Is sent to the use point 4 and a part of it is used,
Unused ultrapure water forms a circulation system returning to the ultrapure water production device 2 via the flow path 6b.
【００３６】超純水製造装置（２次純水装置）２は、紫
外線酸化装置２４及び限外濾過膜分離装置２６を有し、
１次純水１０を紫外線酸化装置２４で処理して有機物を
除去した後、限外濾過膜分離装置２６で微粒子を除去す
ることにより、例えば前述の要求水質を満たす超純水を
製造するものである。１次純水１０は、原水を例えば逆
浸透膜で処理した後、アニオン性及びカチオン性のイオ
ン交換樹脂による処理を順に行い、さらに逆浸透膜処理
することにより得られる。The ultrapure water production device (secondary pure water device) 2 has an ultraviolet oxidation device 24 and an ultrafiltration membrane separation device 26,
The primary pure water 10 is treated with an ultraviolet oxidizer 24 to remove organic substances, and then the ultrafiltration membrane separator 26 is used to remove fine particles to produce, for example, ultrapure water satisfying the above-mentioned required water quality. is there. The primary pure water 10 is obtained by treating raw water with, for example, a reverse osmosis membrane, sequentially performing treatment with an anionic and cationic ion exchange resin, and further treating with a reverse osmosis membrane.
【００３７】図１に示す実施の形態においては、超純水
製造装置２の入口側に１次純水１０及びユースポイント
４から戻された未使用の超純水を収容するタンク２１が
配設される。そして、タンク２１に収容された超純水は
ポンプ２２を介して熱交換器２３で温度調整された後、
紫外線酸化装置２４で処理され、さらにイオン交換樹脂
塔２５で脱塩処理されて限外濾過膜分離装置２６で最終
的に処理される。これらに加え、図示しない逆浸透膜、
その他の膜処理装置が超純水製造装置２に組み込まれる
場合もある。In the embodiment shown in FIG. 1, a tank 21 for accommodating the primary pure water 10 and unused ultrapure water returned from the use point 4 is provided at the inlet side of the ultrapure water production apparatus 2. Is done. Then, after the ultrapure water contained in the tank 21 is temperature-controlled by the heat exchanger 23 via the pump 22,
It is treated in an ultraviolet oxidation device 24, further desalted in an ion exchange resin tower 25, and finally treated in an ultrafiltration membrane separation device 26. In addition to these, a reverse osmosis membrane not shown,
Other membrane processing devices may be incorporated in the ultrapure water production device 2 in some cases.
【００３８】ユースポイント４は超純水の使用場所を示
し、対象物（例えば半導体）を洗浄するための洗浄装置
（洗浄槽）４ａの他、適宜配管やノズル類等を含んでも
よい。なお、ユースポイント４で使用された超純水は、
適宜排水として回収される。The use point 4 indicates a place where the ultrapure water is used, and may include a pipe, a nozzle, etc. as appropriate in addition to a cleaning device (cleaning tank) 4a for cleaning an object (for example, a semiconductor). The ultrapure water used at use point 4 is
Collected as wastewater as appropriate.
【００３９】超純水製造装置２とユースポイント４とを
接続する超純水の流路６ａ，６ｂは基本的には配管やチ
ューブで構成されるが、本発明では流路の途中に適宜タ
ンク、ポンプ、継手、及び弁、その他の設備を配置した
ものも含めて流路と称する。流路６ａ，６ｂに用いる材
料としては、超純水中にその成分が溶出するものでなけ
ればよく、例えば、ＰＶＣ（ポリ塩化ビニル）、ＰＰＳ
（ポリフェニレンサルファイド）、ＰＶＤＦ（ポリビニ
ルジフロライド）、ＦＲＰ（繊維強化プラスチック）、
ＰＦＡ（テトラフルオロエチレン・パーフルオロアルキ
ルビニルエーテル共重合体）、ステンレス等を用いるこ
とができる。The ultrapure water flow paths 6a and 6b connecting the ultrapure water production apparatus 2 and the point of use 4 are basically constituted by pipes and tubes. , Pumps, fittings, valves and other equipment are also referred to as flow paths. The material used for the flow paths 6a and 6b may be any material that does not elute its components in ultrapure water. For example, PVC (polyvinyl chloride), PPS
(Polyphenylene sulfide), PVDF (polyvinyl difluoride), FRP (fiber reinforced plastic),
PFA (tetrafluoroethylene / perfluoroalkyl vinyl ether copolymer), stainless steel, or the like can be used.
【００４０】このような超純水製造システム１の洗浄を
行うには、超純水製造装置２の入り側タンク２１に循環
路２７を設けると共に、イオン交換樹脂塔２５をバイパ
スするバイパス流路２８とガス注入配管２９とを設け、
循環路２７にアンモニア水や水酸化ナトリウム等の塩基
性化合物を添加して、タンク及びシステム内の超純水と
混合して所定のｐＨ及び濃度に調整し、同時にガス注入
配管２９から微細気泡発生源としてガス又は過酸化水素
を注入し、イオン交換樹脂塔２５をバイパスすること以
外は通常の超純水の循環フローに従って、系内に循環さ
せると共に、注入したガス又は過酸化水素で微細気泡を
共存させて、システム全体を洗浄すれば良い。なお、以
下において、微細気泡を共存させた塩基性溶液を「ガス
洗浄液」と称す場合がある。In order to clean the ultrapure water production system 1, a circulation path 27 is provided in the inlet tank 21 of the ultrapure water production apparatus 2, and a bypass flow path 28 which bypasses the ion exchange resin tower 25. And a gas injection pipe 29,
A basic compound such as ammonia water or sodium hydroxide is added to the circulation path 27 and mixed with ultrapure water in the tank and the system to adjust to a predetermined pH and concentration, and at the same time, fine bubbles are generated from the gas injection pipe 29. Except for injecting gas or hydrogen peroxide as a source and circulating through the system according to a normal ultrapure water circulation flow except for bypassing the ion exchange resin tower 25, fine bubbles are injected with the injected gas or hydrogen peroxide. Coexist and the whole system may be cleaned. In the following, a basic solution in which fine bubbles coexist may be referred to as a “gas cleaning liquid”.
【００４１】このときのガス洗浄液の流速は、０．５ｍ
／ｓｅｃ以上、特に０．７５〜２．０ｍ／ｓｅｃの範囲
とすることが好ましい。このような流速とすることによ
り、このガス洗浄液の流れによる物理的な力がシステム
の配管内に付着した微粒子に加えられることにより、塩
基性溶液及び微細気泡による剥離効果と相俟って、これ
らの微粒子の配管からの剥離、除去が一層促進される。At this time, the flow rate of the gas cleaning liquid is 0.5 m
/ Sec or more, particularly preferably in the range of 0.75 to 2.0 m / sec. With such a flow rate, the physical force due to the flow of the gas cleaning liquid is applied to the fine particles adhered to the piping of the system, and in combination with the peeling effect of the basic solution and the fine bubbles, these Separation and removal of fine particles from the pipe are further promoted.
【００４２】この洗浄は、好ましくは０．５〜３時間程
度ガス洗浄液が流れるよう適宜ガス洗浄液を循環させて
行うのが好ましく、洗浄後は、ガス洗浄液をブロー配管
等から排出させ、次いでシステム内に通常の超純水を導
入して残留したガス洗浄液の除去を行う。ガス洗浄液を
含んだ排水は、例えば弱酸性の陽イオン交換樹脂で吸着
処理すればよい。This cleaning is preferably performed by circulating the gas cleaning liquid appropriately so that the gas cleaning liquid flows preferably for about 0.5 to 3 hours. After the cleaning, the gas cleaning liquid is discharged from a blow pipe or the like, and then the system is cleaned. Then, ordinary ultrapure water is introduced to remove the remaining gas cleaning liquid. The wastewater containing the gas cleaning solution may be subjected to, for example, an adsorption treatment with a weakly acidic cation exchange resin.
【００４３】図１に示す方法において、塩基性化合物の
注入箇所やガス（或いは過酸化水素）の注入箇所は任意
であり、何ら図示の箇所に制限されるものではない。In the method shown in FIG. 1, the injection location of the basic compound and the injection location of the gas (or hydrogen peroxide) are arbitrary, and are not limited to the illustrated locations.
【００４４】ガス洗浄液の温度については特に制限はな
いが、超純水製造システムを構成する部材や配管の耐熱
温度を超えない範囲でなるべく高い温度とするのが洗浄
力の点で好ましく、具体的には２０〜１００℃とするの
がよい。例えば、耐熱温度が約４５℃であるＰＶＣを構
成材料とする場合はガス洗浄液の温度を４０℃程度と
し、耐熱温度が約８０℃であるＰＶＤＦの場合はガス洗
浄液の温度を７５〜８０℃とすればよい。また、ステン
レスを構成材料とする場合は１００℃程度の温度で洗浄
することができる。また、このように温度を上げること
は微細気泡の発生の面でも好適である。The temperature of the gas cleaning liquid is not particularly limited, but it is preferable to set the temperature as high as possible within the range not exceeding the heat resistant temperature of the members and piping constituting the ultrapure water production system, from the viewpoint of the cleaning power. The temperature is preferably 20 to 100 ° C. For example, when using PVC having a heat-resistant temperature of about 45 ° C. as a constituent material, the temperature of the gas cleaning liquid is about 40 ° C., and in the case of PVDF having a heat-resistant temperature of about 80 ° C., the temperature of the gas cleaning liquid is 75 to 80 ° C. do it. When stainless steel is used as a constituent material, cleaning can be performed at a temperature of about 100 ° C. It is also preferable to raise the temperature in this way in terms of generation of fine bubbles.
【００４５】また、その他の方法としては、超純水製造
システムの洗浄箇所に上記ガス洗浄液を満たした状態
で、例えば超音波などによりガス洗浄液に微小振動を与
えて微粒子に物理的な力を加えて剥離、除去効果を高め
る方法を採用してもよい。Another method is to apply a physical force to the fine particles by applying a minute vibration to the gas cleaning liquid by, for example, ultrasonic waves while the cleaning point of the ultrapure water production system is filled with the gas cleaning liquid. A method of increasing the peeling / removing effect may be adopted.
【００４６】このようにして、超純水製造システム全体
を洗浄する他、限外濾過膜分離装置や紫外線酸化装置と
いった個別の装置や配管の一部、配管継手部分などの上
記システムの一部分を個別に洗浄してもよい。この場
合、被洗浄部の直前にガス洗浄液を注入すると共に被洗
浄部の直後にガス洗浄液の排出口を設け、一定時間ガス
洗浄液を通液したり、ガス洗浄液を満たした状態で振動
を与えるようにすればよい。In this way, in addition to cleaning the entire ultrapure water production system, individual devices such as an ultrafiltration membrane separation device and an ultraviolet oxidation device, a part of the pipe, and a part of the system such as a pipe joint are individually separated. May be washed. In this case, the gas cleaning liquid is injected immediately before the part to be cleaned, and an outlet for the gas cleaning liquid is provided immediately after the part to be cleaned, so that the gas cleaning liquid is supplied for a certain period of time, or vibration is given when the gas cleaning liquid is filled. What should I do?
【００４７】なお、限外濾過膜などの濾過膜を洗浄する
際は、ガス洗浄液の流速は０．５〜２．５ｍ／ｓｅｃさ
らには０．７５〜２．０ｍ／ｓｅｃとすることが好まし
い。When cleaning a filtration membrane such as an ultrafiltration membrane, the flow rate of the gas cleaning solution is preferably 0.5 to 2.5 m / sec, more preferably 0.75 to 2.0 m / sec.
【００４８】なお、本発明において、限外濾過膜などの
濾過膜の洗浄は、これが超純水製造装置や医薬品製造装
置などに取り付けられている場合、当該濾過膜装置を上
記製造装置に取り付けた状態でガス洗浄液を通液し、あ
るいはガス洗浄液を満たした状態で振動を与えて洗浄し
てもよく、これらの装置から取り外された状態で洗浄し
てもよい。In the present invention, when a filtration membrane such as an ultrafiltration membrane is washed in an ultrapure water production device or a pharmaceutical production device, the filtration membrane device is attached to the production device. The cleaning may be performed by passing the gas cleaning liquid in this state, or by applying vibration while being filled with the gas cleaning liquid, or may be performed in a state where the apparatus is detached from these devices.
【００４９】濾過膜を上記製造装置から取り外した状態
で洗浄する場合、濾過膜はハウジングに収納した状態で
ガス洗浄液を通液し、あるいはガス洗浄液を満たした状
態で振動を与えて洗浄してもよく、もしくはハウジング
から取り出した状態で、超音波や振動などの物理的力を
与えながら洗浄することもできる。When the filter membrane is washed with the filter membrane removed from the manufacturing apparatus, the filter membrane may be washed by passing a gas cleaning liquid in a state housed in a housing, or by applying vibration while the filter membrane is filled with the gas cleaning liquid. Cleaning may be performed while applying physical force such as ultrasonic waves or vibrations in a state of being removed from the housing.
【００５０】本発明において、ガス洗浄液には、界面活
性剤を添加しても良い。この場合界面活性剤としては、
アルキルベンゼンスルホン塩などの陰イオン界面活性剤
を用いることができ、その濃度は１〜１０００ｍｇ／
Ｌ、通常は数１０ｍｇ／Ｌ程度で十分である。In the present invention, a surfactant may be added to the gas cleaning liquid. In this case, as the surfactant,
An anionic surfactant such as an alkylbenzene sulfonate can be used, and its concentration is 1 to 1000 mg /
L, usually several tens mg / L is sufficient.
【００５１】[0051]
【実施例】以下に実施例及び比較例を挙げて本発明をよ
り具体的に説明する。The present invention will be described more specifically below with reference to examples and comparative examples.
【００５２】実施例１ 次のようにして図１に示す超純水製造システムの洗浄を
行った。Example 1 The ultrapure water production system shown in FIG. 1 was cleaned as follows.
【００５３】まず、超純水製造装置２の循環路２７か
ら、タンク２１にアンモニア水を濃度５０ｍｇ／Ｌ、ｐ
Ｈ１０．５となるように添加すると共に、ガス注入配管
２９よりＨ２ガスを２ｐｐｍ注入し、ポンプ２２により
流速０．７５ｍ／ｓｅｃで熱交換器２３に送って４０℃
の温度に調整した後、超純水製造装置２、流路６ａ、ユ
ースポイント４、流路６ｂの順にガス洗浄液を２時間循
環させてこのシステムを洗浄した。但し、イオン交換樹
脂塔２４は洗浄せず、バイパス流路２８を介してガス洗
浄液を迂回させた。First, ammonia water is supplied to the tank 21 from the circulation path 27 of the ultrapure water producing apparatus 2 at a concentration of 50 mg / L, p
At the same time, H 2 gas was added at 2 ppm from the gas injection pipe 29 and sent to the heat exchanger 23 at a flow rate of 0.75 m / sec by the pump 22 to obtain a temperature of 40 ° C.
, The gas cleaning liquid was circulated in the order of the ultrapure water producing apparatus 2, the flow path 6a, the use point 4, and the flow path 6b for 2 hours to clean the system. However, the ion exchange resin tower 24 was not washed, and the gas washing liquid was bypassed via the bypass flow path 28.
【００５４】なお、このＨ２ガス濃度は、大気圧中での
最大溶解量約１．５ｐｐｍを超えるものであり、この条
件ではＨ２ガスは過飽和となり、ガス洗浄液中には粒径
１００μｍ程度のバブル（微細気泡）が約１体積％共存
している。The H 2 gas concentration exceeds the maximum dissolved amount of about 1.5 ppm under atmospheric pressure. Under this condition, the H 2 gas becomes supersaturated and the gas cleaning solution has a particle size of about 100 μm. About 1% by volume of bubbles (fine bubbles) coexist.
【００５５】次いで、ガス洗浄液を図示しないブロー配
管から排出させ、タンク２１に１次純水１０を供給し、
得られた超純水をシステム内に適宜循環させてシステム
の内部に残った洗浄液を排出した。なお、排出された洗
浄液は中和処理した。Next, the gas cleaning liquid is discharged from a blow pipe (not shown), and the primary pure water 10 is supplied to the tank 21.
The obtained ultrapure water was appropriately circulated in the system to discharge the cleaning liquid remaining in the system. The discharged cleaning liquid was subjected to a neutralization treatment.
【００５６】上記した洗浄が終了した後、通常の運転を
行い、ユースポイント４における超純水の水質の経時変
化を、微粒子数とＴＯＣを測定することにより調査し
た。超純水中の微粒子量は、一定量の超純水をフィルタ
で濾過し、このフィルタ上にトラップされた微粒子（粒
径０．０５μｍ以上）を走査型電子顕微鏡で計数した。
また、超純水中のＴＯＣは、紫外線酸化−抵抗率検出法
によって測定した。After the completion of the above-mentioned washing, normal operation was performed, and the change over time in the quality of the ultrapure water at use point 4 was investigated by measuring the number of fine particles and the TOC. The amount of the fine particles in the ultrapure water was determined by filtering a predetermined amount of the ultrapure water with a filter, and counting the fine particles (particle diameter: 0.05 μm or more) trapped on the filter with a scanning electron microscope.
The TOC in ultrapure water was measured by an ultraviolet oxidation-resistivity detection method.
【００５７】以上の結果を図２、図３に示す。各図中の
破線は通常の超純水に要求される水質を示す。The above results are shown in FIGS. The broken line in each figure indicates the water quality required for ordinary ultrapure water.
【００５８】また、運転再開時の生菌数を調べ、結果を
表１に示した。Further, the number of viable bacteria at the time of restarting the operation was examined, and the results are shown in Table 1.
【００５９】比較例１ 実施例１において、Ｈ２ガスを注入しなかったこと以外
は同様にして洗浄を行い、ユースポイント４における超
純水の水質の経時変化を調べ、結果を図２，３に示し
た。また、運転再開時の生菌数を調べ、結果を表１に示
した。Comparative Example 1 In Example 1, cleaning was carried out in the same manner except that H 2 gas was not injected, and the temporal change in the quality of ultrapure water at use point 4 was examined. It was shown to. In addition, the number of viable bacteria at the time of restart of operation was examined, and the results are shown in Table 1.
【００６０】実施例２ 実施例１において、水素ガスの代りに過酸化水素を１０
０ｍｇ／Ｌ注入すると共に洗浄系内を５０℃として、粒
径１００μｍ程度の微細気泡を約３体積％発生させたこ
と以外は同様にして洗浄を行い、ユースポイント４にお
ける超純水の水質の経時変化を調べ、結果を図２，３に
示した。また、運転再開時の生菌数を調べ、結果を表１
に示した。Example 2 In Example 1, hydrogen peroxide was used instead of hydrogen gas.
Cleaning was performed in the same manner except that 0 mg / L was injected, the inside of the cleaning system was set to 50 ° C., and about 3% by volume of microbubbles having a particle size of about 100 μm were generated. The changes were examined and the results are shown in FIGS. In addition, the number of viable bacteria at the time of restart of operation was checked, and the results were shown in Table 1.
It was shown to.
【００６１】[0061]
【表１】 [Table 1]
【００６２】図２より明らかなように、微細気泡を共存
させた実施例１，２では、超純水製造システムの洗浄後
に微粒子数が要求水質（１個／ｍＬ以下）に達するまで
の時間が極めて短く（７〜８時間程度）、微粒子の除去
能力に優れている。一方、比較例１では、要求水質にな
るまでに２０時間以上かかっており、微粒子の除去能力
が劣る。As is clear from FIG. 2, in Examples 1 and 2 in which microbubbles coexist, the time required for the number of fine particles to reach the required water quality (1 / mL or less) after cleaning of the ultrapure water production system is obtained. It is extremely short (about 7 to 8 hours) and has an excellent ability to remove fine particles. On the other hand, in Comparative Example 1, it took 20 hours or more to reach the required water quality, and the ability to remove fine particles was poor.
【００６３】また、図３から明らかなように、実施例
１，２では、残留ＴＯＣも少なく、洗浄後にＴＯＣが要
求水質（１μｇ／Ｌ以下）になるまでは５時間で済み、
有機物の除去能力に優れている。これに対して、比較例
１では残留ＴＯＣも若干多く要求水質になるまでに１２
〜１３時間を要し、有機物の除去能力も実施例１，２に
比べて低い。As is clear from FIG. 3, in Examples 1 and 2, the residual TOC is small, and it takes only 5 hours until the TOC reaches the required water quality (1 μg / L or less) after washing.
Excellent in removing organic matter. On the other hand, in Comparative Example 1, the residual TOC was slightly larger than
It takes 13 to 13 hours, and the ability to remove organic substances is lower than in Examples 1 and 2.
【００６４】また、表１より、微細気泡発生源として過
酸化水素を用いることにより過酸化水素の殺菌効果で系
内が殺菌され、生菌数が著しく低減することがわかる。From Table 1, it can be seen that the use of hydrogen peroxide as a source of microbubbles sterilizes the inside of the system due to the bactericidal effect of hydrogen peroxide and significantly reduces the number of viable bacteria.
【００６５】[0065]
【発明の効果】以上詳述した通り、本発明の超純水製造
システムの洗浄方法によれば、先願の洗浄方法よりも更
に微粒子や残留ＴＯＣ除去能力に優れているため、シス
テム内に付着した微粒子を速やかに剥離、除去すると共
にＴＯＣの残留を防止して短時間で効率的に超純水製造
システムを洗浄することができ、超純水製造システムの
垂直立上げが可能となる。As described above in detail, according to the cleaning method of the ultrapure water production system of the present invention, the cleaning method of the prior application is more excellent in the ability to remove fine particles and residual TOC, so that it adheres to the system. The ultrafine water production system can be efficiently cleaned in a short period of time by removing and removing the fine particles promptly and at the same time preventing the TOC from remaining, thereby enabling the vertical startup of the ultrapure water production system.
【００６６】また、本発明の濾過膜の洗浄方法によれ
ば、濾過膜、特に限外濾過膜を優れた洗浄力で短時間で
効率的に洗浄することができる。Further, according to the method for cleaning a filtration membrane of the present invention, a filtration membrane, particularly an ultrafiltration membrane, can be efficiently cleaned in a short time with excellent cleaning power.
【図１】本発明の超純水製造システムの洗浄方法の実施
の形態を示す系統図である。FIG. 1 is a system diagram showing an embodiment of a cleaning method for an ultrapure water production system of the present invention.
【図２】実施例１，２及び比較例１における洗浄後の超
純水中の微粒子数の経時変化を示すグラフである。FIG. 2 is a graph showing the change over time in the number of fine particles in ultrapure water after washing in Examples 1 and 2 and Comparative Example 1.
【図３】実施例１，２及び比較例１における洗浄後の超
純水中のＴＯＣの経時変化を示すグラフである。FIG. 3 is a graph showing the change over time of TOC in ultrapure water after cleaning in Examples 1 and 2 and Comparative Example 1.
１ 超純水製造システム ２ 超純水製造装置 ４ ユースポイント ２１ タンク ２２ ポンプ ２３ 熱交換器 ２４ 紫外線酸化装置 ２５ イオン交換樹脂塔 ２６ 限外濾過膜分離装置 DESCRIPTION OF SYMBOLS 1 Ultrapure water production system 2 Ultrapure water production apparatus 4 Use point 21 Tank 22 Pump 23 Heat exchanger 24 Ultraviolet oxidation apparatus 25 Ion exchange resin tower 26 Ultrafiltration membrane separation apparatus
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.7 識別記号 ＦＩ テーマコート゛(参考） Ｂ０８Ｂ 9/027 Ｂ０８Ｂ 9/06 Ｆターム(参考） 3B116 AA13 AB51 BB62 BB82 CC01 CC05 3B201 AA13 AB51 BB62 BB82 BB93 BB98 CC01 CC21 4D006 GA06 KA01 KB04 KB11 KC14 KC16 KC20 KD04 KD17 KD22 KD30 PB07 PC02 PC42 ──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 7 Identification symbol FI Theme coat ゛ (Reference) B08B 9/027 B08B 9/06 F term (Reference) 3B116 AA13 AB51 BB62 BB82 CC01 CC05 3B201 AA13 AB51 BB62 BB82 BB93 BB98 CC01 CC21 4D006 GA06 KA01 KB04 KB11 KC14 KC16 KC20 KD04 KD17 KD22 KD30 PB07 PC02 PC42
Claims (4)
ト、並びに前記超純水製造装置と前記ユースポイントと
を接続する超純水の流路からなる超純水製造システムの
超純水接触面に付着した微粒子を除去する洗浄方法にお
いて、 微細気泡を共存させた塩基性溶液で前記超純水製造シス
テムの少なくとも一部を洗浄することを特徴とする超純
水製造システムの洗浄方法。1. An ultrapure water production system comprising an ultrapure water production apparatus, an ultrapure water use point, and an ultrapure water production system comprising an ultrapure water flow path connecting the ultrapure water production apparatus and the use point. A cleaning method for removing fine particles attached to a contact surface, wherein at least a part of the ultrapure water production system is cleaned with a basic solution in which microbubbles coexist.
共存させた塩基性溶液で前記濾過膜を洗浄することを特
徴とする濾過膜の洗浄方法。2. A method for cleaning a filtration membrane, comprising washing the filtration membrane with a basic solution in which fine bubbles coexist.
素ガス、水素ガス、及び窒素ガスよりなる群から選ばれ
る１種又は２種以上を注入することにより、該塩基性溶
液に微細気泡を共存させることを特徴とする請求項１又
は２に記載の洗浄方法。3. Injecting one or more selected from the group consisting of hydrogen peroxide, carbon dioxide gas, oxygen gas, hydrogen gas, and nitrogen gas into the basic solution, thereby forming fine bubbles in the basic solution. The cleaning method according to claim 1, wherein the cleaning method is performed.
ンモニウム化合物、アルカリ金属の水酸化物及びアルカ
リ金属の酸化物よりなる群から選ばれる１種又は２種以
上を溶解させたものである請求項１ないし３のいずれか
１項に記載の洗浄方法。4. A basic solution in which one or more selected from the group consisting of ammonia, ammonium compounds, alkali metal hydroxides and alkali metal oxides are dissolved in ultrapure water. The cleaning method according to claim 1.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP2000343865A JP2002151459A (en) | 2000-11-10 | 2000-11-10 | Cleaning method |
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|---|---|
| JP2002151459A true JP2002151459A (en) | 2002-05-24 |
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ID=18818162
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