JPH0815596B2 - Ultrapure water production method - Google Patents
Ultrapure water production methodInfo
- Publication number
- JPH0815596B2 JPH0815596B2 JP61286015A JP28601586A JPH0815596B2 JP H0815596 B2 JPH0815596 B2 JP H0815596B2 JP 61286015 A JP61286015 A JP 61286015A JP 28601586 A JP28601586 A JP 28601586A JP H0815596 B2 JPH0815596 B2 JP H0815596B2
- Authority
- JP
- Japan
- Prior art keywords
- reverse osmosis
- osmosis membrane
- water
- pure water
- membrane device
- 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.)
- Expired - Fee Related
Links
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- Separation Using Semi-Permeable Membranes (AREA)
- Treatment Of Water By Ion Exchange (AREA)
- Physical Water Treatments (AREA)
Description
【発明の詳細な説明】 〈産業上の利用分野〉 本発明はLSIや超LSIを生産する電子工業において、そ
の中間製品である半導体ウエハーまたはチップ（以下半
導体ウエハーという。）の洗浄用の超純水を製造する方
法に関するものであり、特に原水を凝集沈殿、濾過、活
性炭処理、イオン交換処理、逆浸透膜装置、精密濾過、
紫外線照射処理等を組み合わせた一次側給水製造装置で
得られる一次純水を、末端において逆浸透膜装置を用い
てさらに処理して超純水を製造する方法に関するもので
ある。DETAILED DESCRIPTION OF THE INVENTION <Industrial field of application> The present invention is an ultrapure semiconductor for cleaning an intermediate product such as a semiconductor wafer or a chip (hereinafter referred to as a semiconductor wafer) in the electronic industry for producing LSI and VLSI. The present invention relates to a method for producing water, in particular, coagulating sedimentation of raw water, filtration, activated carbon treatment, ion exchange treatment, reverse osmosis membrane device, microfiltration,
The present invention relates to a method for producing ultrapure water by further treating primary pure water obtained by a primary side water supply production apparatus combined with ultraviolet irradiation treatment or the like at a terminal end with a reverse osmosis membrane device.
〈従来の技術〉 LSIや超LSIを生産する電子工業においては、その中間
製品である半導体ウエハーの洗浄にあたり、その歩留ま
りを向上するために、イオンの量および微粒子の量をpp
bオーダーまで減少させるだけでなく、生菌数を10-1個/
mlまで減少させた、いわゆる超純水を必要とする。<Prior art> In the electronic industry that produces LSIs and VLSIs, in order to improve the yield when cleaning semiconductor wafers that are intermediate products, the amount of ions and the amount of fine particles are
Not only reduces to b order, but also the viable cell count is 10 -1 /
So-called ultrapure water reduced to ml is required.
従って従来ではかかる超純水を製造するにあたり、原
水を凝集沈殿装置、砂濾過器、活性炭濾過器、２床３塔
式純水製造装置、逆浸透膜装置、紫外線照射装置、混床
式ポリシャー等を組み合わせた一次側給水製造装置で可
能なかぎり高純度の一次純水を製造し、そして半導体ウ
エハーを洗浄する直前で当該一次純水をさらに超濾過膜
（UF膜）装置で処理し、いわゆる超純水を得、洗浄水と
して供している。Therefore, conventionally, in producing such ultrapure water, raw water is coagulated and settled, a sand filter, an activated carbon filter, a two-bed three-column pure water production device, a reverse osmosis membrane device, an ultraviolet irradiation device, a mixed bed polisher, etc. The primary side pure water is manufactured as high as possible with the combined primary side water supply manufacturing equipment, and the primary pure water is further treated with the ultrafiltration membrane (UF membrane) equipment immediately before cleaning the semiconductor wafer. Pure water is obtained and used as washing water.
〈発明が解決しようとする問題点〉 ところが最近になって製品の歩留まりを決定する要因
のひとつにT.O.C（全有機炭素）量も指摘され、T.O.Cの
量も少なければ、少ない程、製品の歩留まりが向上する
と言われ、イオン量、微粒子量、生菌数に加えてT.O.C
もその管理の対象となっている。水中に含まれるT.O.C
は逆浸透膜装置で除去可能であるが、逆浸透膜装置の後
段に種々の装置が設置されると、当該後段装置からT.O.
Cが溶出し、かつ当該溶出したT.O.Cは比較的低分子の有
機物に起因するもので、前述した超濾過膜装置ではその
ほとんどが除去できない。<Problems to be solved by the invention> However, recently, one of the factors that determines the product yield is the amount of TOC (total organic carbon), and the smaller the amount of TOC, the smaller the product yield. It is said that the TOC is improved in addition to the amount of ions, the amount of fine particles, and the number of viable bacteria.
Is also subject to that management. TOC contained in water
Can be removed by a reverse osmosis membrane device, but if various devices are installed in the latter stage of the reverse osmosis membrane device, the
C is eluted, and the eluted TOC is due to relatively low-molecular organic matter, and most of it cannot be removed by the above-mentioned ultrafiltration membrane device.
従って半導体ウエハーを洗浄する直前で再度逆浸透膜
装置で処理することが考えられるが、このように末端に
逆浸透膜装置を用いると以下のような問題点が生ずる。Therefore, it is conceivable that the semiconductor wafer is treated again by the reverse osmosis membrane device immediately before cleaning, but the use of the reverse osmosis membrane device at the end causes the following problems.
すなわち逆浸透膜装置はその構造上、細菌が発生し易
く、従って定期的に殺菌処理を実施する必要がある。That is, due to the structure of the reverse osmosis membrane device, bacteria are likely to be generated, and therefore it is necessary to regularly perform sterilization treatment.
当該殺菌処理は通常１週間に１回、熱水あるいは0.5
〜１％の過酸化水素溶液で逆浸透膜装置を洗浄するもの
であるが、このような殺菌処理を実施しないと、逆浸透
膜装置から多量の生菌が漏洩する。従って半導体ウエハ
ーを洗浄する直前で逆浸透膜装置を用いるかぎり、当該
殺菌処理を省略することができない。The sterilization is usually performed once a week with hot water or 0.5
Although the reverse osmosis membrane device is washed with a hydrogen peroxide solution of ˜1%, a large amount of viable bacteria leaks from the reverse osmosis membrane device unless such sterilization treatment is performed. Therefore, unless the reverse osmosis membrane device is used immediately before cleaning the semiconductor wafer, the sterilization treatment cannot be omitted.
ところがこのような殺菌処理をすると、処理後におい
て透過水中に不純物が漏出するので、多量の純水で洗浄
せねばならない。However, when such a sterilization treatment is carried out, impurities are leaked into the permeated water after the treatment, so that it has to be washed with a large amount of pure water.
しかしながら当該純水は前述したごとく種々の装置に
よって高コストをかけて製造したものであり、これを逆
浸透膜装置の洗浄のために多量に消費することは甚だ不
経済である。However, the pure water is produced at high cost by various devices as described above, and it is very uneconomical to consume a large amount of this pure water for cleaning the reverse osmosis membrane device.
また逆浸透膜装置は、運転を休止し、水が滞留すると
比較的早期に細菌が発生するので、運転を休止すること
は好ましくない。In addition, the reverse osmosis membrane device stops its operation, and when water accumulates, bacteria are generated relatively early, so it is not preferable to stop the operation.
本発明は前記一次側給水製造装置で処理された一次純
水中に含まれるT.O.Cを逆浸透膜装置で除去するととも
に、細菌の発生を極力防止し、また細菌処理を実施しも
その処理水に不純物を全く漏洩させず、かつ洗浄用の純
水を可及的少量とすることを目的とするものである。The present invention removes TOC contained in the primary pure water treated by the primary side water supply manufacturing device by a reverse osmosis membrane device, prevents the generation of bacteria as much as possible, and also performs bacterial treatment on the treated water. The purpose is to prevent impurities from leaking at all and to make the amount of pure water for cleaning as small as possible.
〈問題点を解決するための手段〉 本発明は一次純水を紫外線照射装置、混床式ポリシャ
ー、逆浸透膜装置の順に処理して超純水を得ることを基
本フローとし、逆浸透膜装置をすくなくとも２系列以上
設置し、１系列の逆浸透膜装置を殺菌処理している間
に、他の系列の逆浸透膜装置で超純水を製造し、当該殺
菌処理後の逆浸透膜装置を用いて超純水を製造するとと
もに、超純水を製造していた他の系列の逆浸透膜装置を
続いて殺菌処理するように、殺菌処理と超純水の製造を
順に切り換えて行い、また前記殺菌処理は、熱水あるい
は過酸化水素溶液からなる殺菌液を逆浸透膜装置に通す
第１工程、一次純水で逆浸透膜装置を洗浄する第２工
程、一次純水を紫外線照射装置、混床式ポリシャーに通
した後、逆浸透膜装置に通し、その透過水を紫外線照射
装置の前段に循環する第３工程を順に行い、他の系列の
逆浸透膜装置を殺菌処理に切り換える直前まで前記第３
工程を継続するものであることを特徴とする。<Means for Solving Problems> The basic flow of the present invention is to obtain ultrapure water by treating primary pure water in the order of an ultraviolet irradiation device, a mixed bed polisher, and a reverse osmosis membrane device. Install at least 2 or more series, and while sterilizing one series of reverse osmosis membrane devices, produce ultrapure water with the other series of reverse osmosis membrane apparatuses, and install the reverse osmosis membrane apparatus after the sterilization treatment. Along with the production of ultrapure water by using it, the sterilization treatment and the production of ultrapure water are sequentially switched so that the other series of reverse osmosis membrane devices that were producing ultrapure water are subsequently sterilized. In the sterilization treatment, a first step of passing a sterilizing solution composed of hot water or a hydrogen peroxide solution through the reverse osmosis membrane device, a second step of cleaning the reverse osmosis membrane device with primary pure water, an ultraviolet irradiation device for primary pure water, After passing through a mixed bed polisher, pass it through a reverse osmosis membrane device, The third step of circulating the external radiation irradiation device is sequentially performed, and the third step is performed until just before switching the reverse osmosis membrane device of another series to sterilization treatment.
The feature is that the process is continued.
〈作用〉 以下に本発明を図面を用いて詳細に説明する。<Operation> The present invention will be described in detail below with reference to the drawings.
図面は本発明の実施態様の一例を示すフローの説明図
であり、１は一次純水貯槽、２は送水ポンプ、３は紫外
線照射装置、４は混床式ポリシャー、５は高圧ポンプ、
6a〜6dは逆浸透膜装置、７は過酸化水素溶液槽、８は洗
浄ポンプ、９は注入ポンプ、10はミキサーをそれぞれ示
し、11ないし38は弁である。The drawing is an explanatory view of a flow showing an example of an embodiment of the present invention, 1 is a primary pure water storage tank, 2 is a water feed pump, 3 is an ultraviolet irradiation device, 4 is a mixed bed polisher, 5 is a high pressure pump,
6a to 6d are reverse osmosis membrane devices, 7 is a hydrogen peroxide solution tank, 8 is a washing pump, 9 is an injection pump, 10 is a mixer, and 11 to 38 are valves.
図面に示した例は、逆浸透膜装置６を４系列用いるも
のであり、本発明においては、当該複数系列の逆浸透膜
装置の内、１系列はかならず後述する工程よりなる殺菌
処理を行っており、他の系列で超純水を製造するもので
ある。In the example shown in the drawings, the reverse osmosis membrane device 6 is used in four series. In the present invention, one series of the plurality of series of reverse osmosis membrane apparatuses must be sterilized by the steps described below. And the other series produce ultrapure water.
たとえば逆浸透膜装置6aが殺菌処理に切り換わった直
後から本発明を説明すると、逆浸透膜装置6bないし6dに
おいては、次のような超純水の製造を行う。For example, the present invention will be described immediately after the reverse osmosis membrane device 6a is switched to the sterilization process. In the reverse osmosis membrane devices 6b to 6d, the following ultrapure water is produced.
すなわち弁11、20を閉じるとともに、弁13、15、17、
23、26、29、34、36、38を開口して、一次純水供給管39
からの一次純水を、一次純水貯槽１、送水ポンプ２、紫
外線照射装置３、混床式ポリシャー４、高圧ポンプ５を
介して、逆浸透膜装置6bないし6dで処理する。このよう
な処理により一次純水中に含まれる生菌を紫外線照射装
置３によって殺菌し、また一次純水中に含まれる微量の
アルコール等の非電解質不純物を酸等の電解質に分解す
る。さらに混床式ポリシャー４によって一次純水中に含
まれる前述の酸あるいは他の電解質不純物を除去し、そ
して末端に設置した逆浸透膜装置6bないし6dによって、
残留する微量の微粒子、T.O.C等を除去し、半導体ウエ
ハーの洗浄水として最も適した超純水を製造し、超純水
配管40を介してユースポイントに供給する。なお非透過
水管41から得られる非透過水をたとえば一次側給水製造
装置側に回収すう。一方細菌処理のために一次純水の製
造を中断した逆浸透膜装置6aは直ちに以下の殺菌処理を
行う。That is, the valves 11, 20 are closed and the valves 13, 15, 17,
Open the 23, 26, 29, 34, 36, and 38 to supply the primary pure water supply pipe 39
The primary pure water from the above is processed by the reverse osmosis membrane devices 6b to 6d through the primary pure water storage tank 1, the water feed pump 2, the ultraviolet irradiation device 3, the mixed bed polisher 4, and the high pressure pump 5. By such a treatment, live bacteria contained in the primary pure water are sterilized by the ultraviolet irradiation device 3, and a trace amount of non-electrolyte impurities such as alcohol contained in the primary pure water is decomposed into an electrolyte such as an acid. Further, the above-mentioned acid or other electrolyte impurities contained in the primary pure water are removed by the mixed bed polisher 4, and by the reverse osmosis membrane devices 6b to 6d installed at the ends,
The remaining trace amount of fine particles, TOC, etc. are removed to produce ultrapure water most suitable as cleaning water for semiconductor wafers, and the ultrapure water is supplied to the point of use through the ultrapure water pipe 40. In addition, the non-permeated water obtained from the non-permeated water pipe 41 is collected, for example, on the primary side water supply manufacturing device side. On the other hand, the reverse osmosis membrane device 6a, which has suspended the production of primary pure water for bacterial treatment, immediately carries out the following sterilization treatment.
まず弁12、31を開口するとともに、洗浄ポンプ８、注
入ポンプ９を駆動し、過酸化水素溶液槽７内の過酸化水
素溶液を一次純水で希釈混合してミキサー10を介して逆
浸透膜装置6aに供給する第１工程を行う。逆浸透膜装置
に供給する過酸化水素溶液の濃度としては0.5〜１％程
度とし、まず逆浸透膜の表面を過酸化水素溶液で洗浄
し、その排液をブロー管42aから排出する。次いで弁21
も開口し、過酸化水素溶液を逆浸透膜に通過させ、その
透過排液をブロー管42bから排出する。First, the valves 12 and 31 are opened, the cleaning pump 8 and the injection pump 9 are driven, the hydrogen peroxide solution in the hydrogen peroxide solution tank 7 is diluted and mixed with primary pure water, and the reverse osmosis membrane is passed through the mixer 10. The first step of supplying the device 6a is performed. The concentration of the hydrogen peroxide solution supplied to the reverse osmosis membrane device is set to about 0.5 to 1%, the surface of the reverse osmosis membrane is first washed with the hydrogen peroxide solution, and the drainage is discharged from the blow pipe 42a. Then valve 21
The hydrogen peroxide solution is passed through the reverse osmosis membrane, and the permeated drainage liquid is discharged from the blow pipe 42b.
当該第１工程の前半部を約10分、後半部を約50分行う
が、このような過酸化水素溶液で処理することにより、
逆浸透膜あるいはモジュール内に付着した生菌およびス
ライム等を殺菌および剥離することができる。The first half of the first step is performed for about 10 minutes and the latter half for about 50 minutes. By treating with such a hydrogen peroxide solution,
It is possible to sterilize and remove live bacteria, slime, etc. attached to the reverse osmosis membrane or the module.
このような第１工程が終了した後、次の第２工程を行
う。After the first step is completed, the next second step is performed.
すなわち注入ポンプ９の駆動を停止し、弁12、31、21
を開口したまま、洗浄ポンプ８からの一次純水を逆浸透
膜装置6aに供給し、過酸化水素溶液を置換および洗浄す
る操作を行う。当該第２工程は10〜20分程度で充分であ
る。That is, the drive of the injection pump 9 is stopped and the valves 12, 31, 21
With the opening of, the primary pure water from the cleaning pump 8 is supplied to the reverse osmosis membrane device 6a, and the operation of replacing and cleaning the hydrogen peroxide solution is performed. About 10 to 20 minutes is sufficient for the second step.
次いで以下の第３工程を行う。 Then, the following third step is performed.
まず弁31、21を開口したまま、弁11を開口するととも
に弁12を閉じ、洗浄ポンプ８の駆動を停止し、逆浸透膜
装置6bないし6dの供給水と同様なもの、すなわち紫外線
照射装置３、混床式ポリシャー４を通過した一次純水を
逆浸透膜装置6aに供給し、非透過水および透過水とも
に、ブロー管42aおよび42bから排出する。First, while leaving the valves 31 and 21 open, the valve 11 is opened and the valve 12 is closed, the driving of the washing pump 8 is stopped, and the same thing as the supply water of the reverse osmosis membrane devices 6b to 6d, that is, the ultraviolet irradiation device 3 The primary pure water that has passed through the mixed bed polisher 4 is supplied to the reverse osmosis membrane device 6a, and both the non-permeated water and the permeated water are discharged from the blow pipes 42a and 42b.
当該排出を30〜60分程度行い、非透過水、および透過
水中に含まれる過酸化水素等の不純物の量が極微量にな
った時点で、弁31、21を閉じるとともに弁32、19を開口
し、非透過水を逆浸透膜装置6bないし6dと同様に非透過
水管41から取り出し、これを一次側給水製造装置側に回
収し、一次透過水を循環配管43を用いて紫外線照射装置
３の前段、すなわち図面のフローでは一次純水貯槽１に
循環する。The discharge is performed for about 30 to 60 minutes, and when the amount of impurities such as hydrogen peroxide contained in the non-permeated water and the permeated water becomes extremely small, the valves 31 and 21 are closed and the valves 32 and 19 are opened. Then, the non-permeated water is taken out from the non-permeated water pipe 41 in the same manner as the reverse osmosis membrane devices 6b to 6d, is collected in the primary side water supply manufacturing device side, and the primary permeated water is circulated in the ultraviolet irradiation device 3 using the circulation pipe 43. In the first stage, that is, in the flow of the drawing, it circulates in the primary pure water storage tank 1.
このような循環を行うことにより、その循環水はかな
らず紫外線照射装置３および混床式ポリシャー４を通過
するので、逆浸透膜装置6aの透過水中にたとえ微量の過
酸化水素あるいは他の不純物が含まれていても、これら
の不純物は紫外線照射により分解され、また当該分解に
より生ずる電解質は混床式ポリシャー４で効果的に除去
でき、かつその後段に位置する逆浸透膜装置で残留する
微粒子、T.O.C等の不純物を可及的に除去できるので、
半導体ウエハーの洗浄水として最も適した超純水を供給
することができる。By performing such circulation, the circulating water always passes through the ultraviolet irradiation device 3 and the mixed-bed polisher 4, so that even a trace amount of hydrogen peroxide or other impurities is contained in the permeated water of the reverse osmosis membrane device 6a. However, these impurities are decomposed by UV irradiation, and the electrolyte generated by the decomposition can be effectively removed by the mixed bed polisher 4, and the fine particles and TOC remaining in the reverse osmosis membrane device located at the subsequent stage can be removed. Since impurities such as can be removed as much as possible,
It is possible to supply ultrapure water that is most suitable as cleaning water for semiconductor wafers.
本発明における第３工程は、次の逆浸透膜装置たとえ
ば逆浸透膜装置6bを殺菌処理するまで継続して行う。The third step in the present invention is continuously performed until the next reverse osmosis membrane device, for example, the reverse osmosis membrane device 6b is sterilized.
すなわち逆浸透膜装置はその構造上、殺菌が発生し易
く、まして処理を中断して水を滞留すると殺菌がより繁
殖し易くなる。That is, due to the structure of the reverse osmosis membrane device, sterilization is likely to occur, and if the treatment is interrupted and water is retained, the sterilization is more likely to propagate.
したがって本発明は末端に設置する逆浸透膜装置の運
転停止を極力を行わず、前述したごとくの第３工程を継
続して行う。Therefore, according to the present invention, the reverse osmosis membrane device installed at the end is not stopped as much as possible, and the third step as described above is continuously performed.
次に逆浸透膜装置6bを殺菌処理するが、この場合は前
述したと同様に相当する各弁の開閉を行い、逆浸透膜装
置6bを前述したと同様の殺菌処理をするとともに、逆浸
透膜装置6a、6c、6dによって超純水を製造して、超純水
配管40によりユースポイントに供給する。Next, the reverse osmosis membrane device 6b is sterilized. In this case, the corresponding valves are opened and closed in the same manner as described above, and the reverse osmosis membrane device 6b is sterilized in the same manner as described above. Ultrapure water is produced by the devices 6a, 6c, and 6d, and is supplied to the use point through the ultrapure water pipe 40.
本発明は以上説明したごとく、複数系列の逆浸透膜装
置を順に殺菌工程に切り換え、殺菌処理後の逆浸透膜装
置で超純水を製造するものである。As described above, the present invention sequentially switches a plurality of series of reverse osmosis membrane devices to a sterilization process, and produces ultrapure water by the reverse osmosis membrane device after the sterilization treatment.
次に本発明に用いる逆浸透膜を説明する。 Next, the reverse osmosis membrane used in the present invention will be described.
従来から逆浸透膜としては、酢酸セルローズ系膜、ポ
リアミド系膜、ポリアミド系とポリスルホン系の複合膜
等があるが、末端逆浸透膜装置においては、T.O.Cの除
去性能に優れ、かつそれ程高圧を要しなくとも透過水量
の大なるものが適している。Conventionally, reverse osmosis membranes include cellulose acetate-based membranes, polyamide-based membranes, composite membranes of polyamide-based and polysulfone-based membranes, but the terminal reverse osmosis membrane device has excellent TOC removal performance and requires high pressure. Even if it does not, a large amount of permeated water is suitable.
この点において、脱塩の目的のために従来から用いら
れている酢酸セルローズ系膜は膜基材そのものが菌類の
栄養源となり、菌類が極めて繁殖し易いという点で、末
端処理には適してなく、また従来から海水淡水化装置に
用いられているポリアミド系膜はT.O.Cの除去性能につ
いては申し分ないが、透過水量が少ない点で適していな
い。In this respect, the cellulose acetate-based membrane that has been conventionally used for the purpose of desalting is not suitable for terminal treatment because the membrane substrate itself serves as a nutrient source for the fungus, and the fungus is extremely easy to reproduce. Also, the polyamide-based membranes that have been used in seawater desalination systems have been satisfactory in terms of TOC removal performance, but they are not suitable because they have a small amount of permeated water.
一方ポリアミド系とポリスルホン系の複合膜は、T.O.
C除去性能に優れ、また透過水量も大きい。しかしなが
ら過酸化水素溶液で殺菌処理した後の洗浄において、透
過水の比抵抗の上昇が悪いという欠点を有している。On the other hand, polyamide-based and polysulfone-based composite membranes are
Excellent C removal performance and large amount of permeated water. However, it has a drawback that the specific resistance of permeated water does not increase in the washing after sterilization treatment with a hydrogen peroxide solution.
これらの逆浸透膜に対して、ポリビニルアルコール系
とポリスルホン系の複合膜は、膜の支持体としてポーラ
スなポリスルホン系膜を配し、その上部にポリビニルア
ルコール系の膜を配したもので、発明者等の実験によれ
ば、T.O.C除去性能に優れ、また透過水量が大であり、
さらに過酸化水素溶液で殺菌処理した後の洗浄において
も、透過水の比抵抗の上昇が早く、末端逆浸透膜装置に
使用する逆浸透膜として最も優れている。In contrast to these reverse osmosis membranes, a polyvinyl alcohol-based and polysulfone-based composite membrane has a porous polysulfone-based membrane as a support for the membrane and a polyvinyl alcohol-based membrane on top of it. According to experiments such as, the TOC removal performance is excellent and the amount of permeated water is large,
Further, even in the washing after the sterilization treatment with the hydrogen peroxide solution, the specific resistance of the permeated water rapidly increases, and it is the most excellent reverse osmosis membrane used in the terminal reverse osmosis membrane device.
よって本発明においては上述した理由によりポリビニ
ルアルコール系とポリスルホン系の複合膜を用いること
が好ましい。Therefore, in the present invention, it is preferable to use a polyvinyl alcohol-based and polysulfone-based composite film for the reasons described above.
なお上述した実施態様においては、殺菌液として過酸
化水素溶液を用いたが、耐熱性の逆浸透膜を用いること
により、殺菌液として熱水を使用することができ、また
熱水を殺菌液として用いる殺菌工程も殺菌液が変わるだ
けで殺菌工程そのものは前述の工程と全く同様にして行
う。In the embodiment described above, the hydrogen peroxide solution was used as the sterilizing solution, but by using the heat-resistant reverse osmosis membrane, hot water can be used as the sterilizing solution, and the hot water can be used as the sterilizing solution. The sterilization process used is exactly the same as the above-described process, except that the sterilizing solution is changed.
〈効果〉 以上説明したごとく、本発明は一次純水を紫外線照射
装置、混床式ポリシャーで処理し、次いで末端に設置し
た逆浸透膜装置で処理するので、生菌、電解質、微粒
子、T.O.C等のあらゆる不純物を可及的に除去した超純
水を得ることができる。<Effects> As described above, since the present invention treats primary pure water with an ultraviolet irradiation device and a mixed bed polisher, and then with a reverse osmosis membrane device installed at the end, viable bacteria, electrolytes, fine particles, TOC, etc. It is possible to obtain ultrapure water in which all the impurities are removed as much as possible.
また逆浸透膜装置を複数系列設置し、その内１系列を
常に殺菌処理、他系列を超純水の製造に用い、かつ複数
系列の逆浸透膜装置を順に殺菌処理に切り換えるので、
逆浸透膜装置を効率的に運用することができ、したがっ
て、装置の設置コストを低減し得ることができる。また
逆浸透膜装置は殺菌処理および超純水の製造と連続して
運転されるので、水が滞留することがなく、細菌の発生
を極力防止することができる。In addition, since multiple reverse osmosis membrane devices are installed, one of them is always used for sterilization, the other is used for the production of ultrapure water, and multiple series of reverse osmosis membrane devices are sequentially switched to sterilization.
The reverse osmosis membrane device can be operated efficiently, and thus the installation cost of the device can be reduced. Further, since the reverse osmosis membrane device is continuously operated in the sterilization process and the production of ultrapure water, water does not stay and the generation of bacteria can be prevented as much as possible.
さらに殺菌処理の最終工程である第３工程から得られ
る透過水および非透過水の大半を循環使用するので、洗
浄用の純水を可及的に少量とすることができる。Furthermore, since most of the permeated water and the non-permeated water obtained from the third step which is the final step of the sterilization treatment are circulated and used, the amount of pure water for cleaning can be made as small as possible.
また当該第３工程により循環する透過水中に過酸化水
素等の不純物がたとえ含まれていたとしても、紫外線照
射装置、混床式ポリシャーを必ず通過するので、得られ
る超純水中にこれらの不純物が混入することを完全に防
止することができる。Further, even if impurities such as hydrogen peroxide are contained in the permeated water circulated in the third step, they will pass through the ultraviolet irradiation device and the mixed bed polisher without fail, so that these impurities will be contained in the obtained ultrapure water. Can be completely prevented.
以下に本発明の実施例を説明する。 Examples of the present invention will be described below.
実施例 原水を凝集沈殿濾過処理し、次いで活性炭濾過器、２
床３塔式純水製造装置、混床式ポリシャー、精密濾過器
で処理することにより得た一次純水を一次純水貯槽に貯
留し、この一次純水を、図面に示したフローに順じて紫
外線照射装置、混床式ポリシャーで処理した後、スパイ
ラル型のポリビニルアルコール系とポリスルホン系の複
合膜を装置した逆浸透膜装置で処理して超純水を得た。Example Raw water is subjected to coagulation sedimentation filtration, followed by an activated carbon filter, 2
Primary pure water obtained by treatment with a three-bed floor pure water production system, a mixed bed polisher, and a microfilter is stored in a primary pure water storage tank, and this primary pure water is subjected to the flow shown in the drawing. Then, it was treated with an ultraviolet irradiation device and a mixed bed polisher, and then treated with a reverse osmosis membrane device equipped with a spiral type polyvinyl alcohol-based and polysulfone-based composite membrane to obtain ultrapure water.
なお、当該逆浸透膜装置は２系列用い、一方の逆浸透
膜装置で超純水の製造を3,000時間行った後、他方の殺
菌処理の第３工程を行っている逆浸透膜装置を超純水の
製造に切り換え、一方の逆浸透膜装置を殺菌処理すると
いうように、超純水の製造と殺菌処理を交互に行った。Two reverse osmosis membrane devices were used, and one reverse osmosis membrane device was used to perform ultrapure water production for 3,000 hours, and then the other reverse osmosis membrane device was subjected to the third step of sterilization treatment. The production of ultrapure water and the sterilization treatment were alternately performed, such as switching to the production of water and sterilizing one reverse osmosis membrane device.
なお殺菌処理は以下の工程に従った。 The sterilization treatment was performed according to the following steps.
すなわち殺菌液として0.5％過酸化水素溶液を用い、
まず透過水側の弁を閉じ、非透過水側の弁を開口して当
該殺菌液で逆浸透膜の膜面を10分間洗浄し、次いで透過
水側の弁も開口して、殺菌液を逆浸透膜に50分間透過さ
せた（第１工程）。That is, using a 0.5% hydrogen peroxide solution as a sterilizing solution,
First, close the permeate side valve and open the non-permeate side valve to wash the reverse osmosis membrane surface with the sterilizing solution for 10 minutes, and then open the permeate side valve to reverse the sterilizing solution. Permeation through the osmotic membrane for 50 minutes (first step).
次いで一次純水を逆浸透膜に10分間供給して、非透過
水および透過水ともにブローすることにより逆浸透膜装
置を洗浄し（第２工程）、次いで紫外線照射装置、混床
式ポリシャーに通過させた一次純水を逆浸透膜装置に供
給し、約60分間のみ透過水および非透過水ともにブロー
した。続いて、透過水を一次純水貯槽に循環する操作
（第３工程）を行い、当該逆浸透膜装置を超純水の製造
に切り換えるまで当該循操作を続行した。Next, primary pure water is supplied to the reverse osmosis membrane for 10 minutes, and the reverse osmosis membrane device is washed by blowing both non-permeated water and permeated water (second step), and then passed through an ultraviolet irradiation device and a mixed bed polisher. The thus-prepared primary pure water was supplied to the reverse osmosis membrane device, and both permeated water and non-permeated water were blown only for about 60 minutes. Subsequently, an operation (third step) of circulating the permeated water in the primary pure water storage tank was performed, and the circulation operation was continued until the reverse osmosis membrane device was switched to the production of ultrapure water.
このような殺菌処理と、超純水の製造を交互に続行し
たところ、逆浸透膜装置から得られる透過水の水質は第
１表の通りであった。When the sterilization treatment and the production of ultrapure water were alternately continued, the quality of the permeated water obtained from the reverse osmosis membrane device was as shown in Table 1.
図面は本発明の実施態様の一例を示すフローの説明図で
ある。 １…一次純水貯槽、２…送水ポンプ ３…紫外線照射装置、４…混床式ポリシャー ５…高圧ポンプ、６…逆浸透膜装置 ７…過酸化水素溶液槽、８…洗浄ポンプ ９…注入ポンプ、10…ミキサー 11〜38…弁、39…一次純水供給管 40…超純水配管、41…非透過水管 42…ブロー管、43…循環配管The drawing is an explanatory diagram of a flow showing an example of an embodiment of the present invention. DESCRIPTION OF SYMBOLS 1 ... Primary pure water storage tank, 2 ... Water supply pump 3 ... Ultraviolet irradiation device, 4 ... Mixed bed type polisher 5 ... High pressure pump, 6 ... Reverse osmosis membrane device 7 ... Hydrogen peroxide solution tank, 8 ... Washing pump 9 ... Injection pump , 10 ... Mixer 11 to 38 ... Valve, 39 ... Primary pure water supply pipe 40 ... Ultra pure water pipe, 41 ... Non-permeate water pipe 42 ... Blow pipe, 43 ... Circulation pipe
───────────────────────────────────────────────────── 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 1/50 ５３１ Ｑ ５４０ Ｂ ５５０ Ｈ ５６０ Ｅ ─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. 6 Identification code Internal reference number FI Technical indication C02F 1/50 531 Q 540 B 550 H 560 E
Claims (1)
紫外線照射装置、混床式ポリシャー、逆浸透膜装置の順
に処理して超純水を製造するにあたり、逆浸透膜装置を
すくなくとも２系列以上設置し、１系列の逆浸透膜装置
を殺菌処理している間に、他の系列の逆浸透膜装置で超
純水を製造し、当該殺菌処理後の逆浸透膜装置を用いて
超純水を製造するとともに、超純水を製造していた他の
系列の逆浸透膜装置を続いて殺菌処理するように殺菌処
理と超純水の製造を順に切り換えて行い、前記殺菌処理
は、熱水あるいは過酸化水素溶液からなる殺菌液を逆浸
透膜装置に通す第１工程、一次純水で逆浸透膜装置を洗
浄する第２工程、一次純水を紫外線照射装置、混床式ポ
リシャーに通した後、逆浸透膜装置に通してその透過水
を紫外線照射装置の前段に循環する第３工程を順に行
い、他の系列の逆浸透膜装置を殺菌処理に切り換える直
前まで前記第３工程を継続するものであることを特徴と
する超純水の製造方法。1. A method of treating ultrapure water by treating primary pure water obtained by a primary side water supply production device in order of an ultraviolet irradiation device, a mixed bed polisher, and a reverse osmosis membrane device, and at least 2 reverse osmosis membrane devices are required. Install one or more series of reverse osmosis membrane devices while sterilizing one series of reverse osmosis membrane devices to produce ultrapure water with another series of reverse osmosis membrane devices. Along with the production of pure water, the sterilization treatment and the production of ultrapure water are sequentially switched so as to sterilize the other series of reverse osmosis membrane devices that were producing ultrapure water, and the sterilization treatment is performed. The first step of passing a sterilizing solution consisting of hot water or hydrogen peroxide solution through the reverse osmosis membrane device, the second step of cleaning the reverse osmosis membrane device with primary pure water, the primary pure water to the ultraviolet irradiation device, the mixed bed polisher. After passing it through the reverse osmosis membrane device, the permeated water is irradiated with ultraviolet light. The third step of sequentially performed, the production method of ultra-pure water characterized in that to continue the third step until just before switching the reverse osmosis membrane apparatus of another sequence to sterilize circulating in front.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61286015A JPH0815596B2 (en) | 1986-12-02 | 1986-12-02 | Ultrapure water production method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP61286015A JPH0815596B2 (en) | 1986-12-02 | 1986-12-02 | Ultrapure water production method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPS63141694A JPS63141694A (en) | 1988-06-14 |
| JPH0815596B2 true JPH0815596B2 (en) | 1996-02-21 |
Family
ID=17698879
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP61286015A Expired - Fee Related JPH0815596B2 (en) | 1986-12-02 | 1986-12-02 | Ultrapure water production method |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH0815596B2 (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0529119Y2 (en) * | 1989-05-15 | 1993-07-26 | ||
| JPH0790219B2 (en) * | 1990-08-01 | 1995-10-04 | 日本錬水株式会社 | Pure water production apparatus and production method |
| JP3187629B2 (en) * | 1993-12-16 | 2001-07-11 | オルガノ株式会社 | Reverse osmosis membrane treatment method |
| JP4661009B2 (en) * | 2001-09-04 | 2011-03-30 | 栗田工業株式会社 | Ultrapure water production system |
| WO2006061583A1 (en) * | 2004-12-06 | 2006-06-15 | Axsia Serck Baker Limited | Improvements in and relating to biocide treatment of seawater treatment membranes |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS56141811A (en) * | 1980-04-03 | 1981-11-05 | Asahi Chem Ind Co Ltd | Ultrafiltration method |
| JPS6078689A (en) * | 1983-10-06 | 1985-05-04 | Kobe Steel Ltd | Operation of reverse osmosis apparatus |
-
1986
- 1986-12-02 JP JP61286015A patent/JPH0815596B2/en not_active Expired - Fee Related
Non-Patent Citations (1)
| Title |
|---|
| 大矢晴彦「純水・超純水製造法−要素技術と応用システム−」（昭６０−３−２０）幸書房Ｐ．１８０図２．６．１ |
Also Published As
| Publication number | Publication date |
|---|---|
| JPS63141694A (en) | 1988-06-14 |
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