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JP7171386B2 - Method for starting up ultrapure water production device and ultrapure water production device - Google Patents

Method for starting up ultrapure water production device and ultrapure water production device Download PDF

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JP7171386B2
JP7171386B2 JP2018219467A JP2018219467A JP7171386B2 JP 7171386 B2 JP7171386 B2 JP 7171386B2 JP 2018219467 A JP2018219467 A JP 2018219467A JP 2018219467 A JP2018219467 A JP 2018219467A JP 7171386 B2 JP7171386 B2 JP 7171386B2
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ultrapure water
water production
flow path
water
production apparatus
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JP2020081957A (en
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恭則 松井
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Nomura Micro Science Co Ltd
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Priority to KR1020217006613A priority patent/KR20210091115A/en
Priority to PCT/JP2019/044156 priority patent/WO2020105494A1/en
Priority to CN201980063396.5A priority patent/CN112770825B/en
Priority to TW108142091A priority patent/TWI851623B/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D61/00Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/14Ultrafiltration; Microfiltration
    • B01D61/145Ultrafiltration
    • B01D61/146Ultrafiltration comprising multiple ultrafiltration steps
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D61/00Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/14Ultrafiltration; Microfiltration
    • B01D61/147Microfiltration
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D61/00Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/14Ultrafiltration; Microfiltration
    • B01D61/22Controlling or regulating
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D61/00Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • B01D61/58Multistep processes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D65/00Accessories or auxiliary operations, in general, for separation processes or apparatus using semi-permeable membranes
    • B01D65/02Membrane cleaning or sterilisation ; Membrane regeneration
    • B01D65/022Membrane sterilisation
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/44Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/44Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis
    • C02F1/444Treatment of water, waste water, or sewage by dialysis, osmosis or reverse osmosis by ultrafiltration or microfiltration
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D19/00Degasification of liquids
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2311/00Details relating to membrane separation process operations and control
    • B01D2311/25Recirculation, recycling or bypass, e.g. recirculation of concentrate into the feed
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2313/00Details relating to membrane modules or apparatus
    • B01D2313/18Specific valves
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2313/00Details relating to membrane modules or apparatus
    • B01D2313/50Specific extra tanks
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2313/00Details relating to membrane modules or apparatus
    • B01D2313/56Specific mechanisms for loading the membrane in a module
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D2313/00Details relating to membrane modules or apparatus
    • B01D2313/57Tools used for removal of membranes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B01PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01DSEPARATION
    • B01D61/00Processes of separation using semi-permeable membranes, e.g. dialysis, osmosis or ultrafiltration; Apparatus, accessories or auxiliary operations specially adapted therefor
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/30Treatment of water, waste water, or sewage by irradiation
    • C02F1/32Treatment of water, waste water, or sewage by irradiation with ultraviolet light
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/42Treatment of water, waste water, or sewage by ion-exchange
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/02Non-contaminated water, e.g. for industrial water supply
    • C02F2103/04Non-contaminated water, e.g. for industrial water supply for obtaining ultra-pure water

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  • Engineering & Computer Science (AREA)
  • Water Supply & Treatment (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Environmental & Geological Engineering (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Toxicology (AREA)
  • Separation Using Semi-Permeable Membranes (AREA)
  • Degasification And Air Bubble Elimination (AREA)
  • Treatment Of Water By Ion Exchange (AREA)
  • Physical Water Treatments (AREA)

Description

本発明は、超純水製造装置を例えば新規に設置して立ち上げる際に用いられる超純水製造装置の立ち上げ方法、及びこの立ち上げ方法を適用可能な超純水製造装置に関する。 TECHNICAL FIELD The present invention relates to a method for starting up an ultrapure water production apparatus, which is used, for example, when a new ultrapure water production apparatus is installed and started up, and an ultrapure water production apparatus to which this startup method can be applied.

半導体の製造工程などで利用される超純水製造装置は、ユースポイント(使用場所)へ向う被処理水の流路を含む水処理系によって、流路上を流れる被処理水を水処理して超純水を得る。この種の超純水製造装置は、一次純水製造部及び二次純水製造部を主に備えている。一次純水製造部は、例えば原水中の懸濁物質を除去する前処理部と、前処理水中の全有機炭素(TOC)成分やイオン成分を除去する逆浸透膜装置やイオン交換装置と、を用いて一次純水を製造する。一方、二次純水製造部は、一次純水中に残留する微粒子、コロイダル物質、有機物、金属、陰イオンなどを除去することによって二次純水(超純水)を製造する。 Ultrapure water production equipment used in the semiconductor manufacturing process, etc., uses a water treatment system that includes a flow path for the water to be treated that is directed to the point of use (place of use). Get pure water. This type of ultrapure water production system mainly includes a primary pure water producing section and a secondary pure water producing section. The primary pure water production unit includes, for example, a pretreatment unit that removes suspended solids in the raw water, and a reverse osmosis membrane device or an ion exchange device that removes total organic carbon (TOC) components and ion components in the pretreated water. to produce primary pure water. On the other hand, the secondary pure water production section produces secondary pure water (ultra-pure water) by removing fine particles, colloidal substances, organic substances, metals, anions, etc. remaining in the primary pure water.

ここで、超純水製造装置を例えば新規に設置して立ち上げるために、その設置場所で超純水製造装置の例えば組み立て作業を行う場合に、上記した水処理系内に対する微粒子、生菌、全有機炭素成分の混入や、被処理水の流路を構成している配管からの金属成分の溶出などが生じるといった課題がある。そこで、この対策として、超純水製造装置の通常運転に先立ち、超純水製造装置内の水処理系を予め洗浄することが行われている(例えば特許文献1参照)。 Here, for example, in order to newly install and start up an ultrapure water production apparatus, for example, when assembling the ultrapure water production apparatus at the installation site, fine particles, viable bacteria, There are problems such as contamination of all organic carbon components and elution of metal components from pipes forming the flow path of the water to be treated. Therefore, as a countermeasure, prior to the normal operation of the ultrapure water production apparatus, the water treatment system in the ultrapure water production apparatus is washed in advance (see, for example, Patent Document 1).

特開2004-122020号公報Japanese Patent Application Laid-Open No. 2004-122020

しかしながら、上述した洗浄を長期間にわたって継続させた後でも、超純水製造装置で製造された超純水が、所期の製造スペック内に収まらないことがある。例えば、超純水製造装置内の配管類の接続箇所などが煩雑に接続された場合や、超純水製造装置を設置する環境の清浄性に課題がある場合には、例えば粒径の比較的大きい金属粒子や砂などが、ユースポイントの前段に配置された限外ろ過膜装置などに捕捉されたままの状態で水処理系内に存在していることがある。この際、金属粒子などの成分の溶出が水処理系内で長期間続き、この結果、製造される超純水の水質は、継続的に悪化した状態となる。 However, even after the above-described cleaning is continued for a long period of time, there are cases where the ultrapure water produced by the ultrapure water production apparatus does not fall within the expected production specifications. For example, if the connection points of pipes in the ultrapure water production equipment are complicatedly connected, or if there is a problem with the cleanliness of the environment where the ultrapure water production equipment is installed, Large metal particles, sand, etc. may exist in the water treatment system in a state of being captured by an ultrafiltration membrane device or the like placed upstream of the point of use. At this time, elution of components such as metal particles continues for a long period of time in the water treatment system, and as a result, the water quality of the produced ultrapure water continuously deteriorates.

本発明は、上記課題を解決するためになされたものであり、超純水製造装置の立ち上げ期間を短縮することができる超純水製造装置の立ち上げ方法及び超純水製造装置を提供することを目的とする。 The present invention has been made to solve the above problems, and provides a method for starting up an ultrapure water production apparatus and an ultrapure water production apparatus capable of shortening the startup period of the ultrapure water production apparatus. for the purpose.

本発明の超純水製造装置の立ち上げ方法は、被処理水を流すための流路と、前記流路上に設けられ、前記被処理水をユースポイントの前段で水処理する限外ろ過膜装置と、を少なくとも含む水処理系を備えた超純水製造装置の立ち上げ方法であって、前記流路上における前記限外ろ過膜装置の前段に、仮置きのフィルタ装置を設置する工程と、前記仮置きのフィルタ装置の設置後に、前記流路に沿って送水を開始することにより前記水処理系を洗浄する工程と、前記送水による洗浄の開始から所定の期間経過後に、前記仮置きのフィルタ装置を前記超純水製造装置から分離する工程と、を有している。 A method for starting up an ultrapure water production apparatus of the present invention includes a flow path for flowing water to be treated, and an ultrafiltration membrane device provided on the flow path for treating the water to be treated before the point of use. and a method for starting up an ultrapure water production system comprising a water treatment system comprising at least a step of installing a temporarily placed filter device upstream of the ultrafiltration membrane device on the flow path; a step of cleaning the water treatment system by starting water supply along the flow path after installing the temporarily placed filter device; from the ultrapure water production apparatus.

前述した洗浄は、殺菌処理を含むものである。さらに、前記分離する工程の後、前記流路に沿った送水を開始し、所期の製造スペック内に収まる超純水が得られるまで水処理を行う工程を実施する。また、前記超純水製造装置は、前記流路上における前記仮置きのフィルタ装置の上流側にタンクをさらに備えている。また、前記流路は、前記限外ろ過膜装置を通過した後、前記タンクに戻る循環ラインを有している。さらに、前記所定の期間は、前記洗浄の開始に伴い、前記循環ライン内の水量と流量から計算される循環回数が、例えば0.5~2200回となる期間であることが望ましい。 The cleaning described above includes sterilization. Further, after the separating step, water treatment is carried out until ultrapure water within the desired manufacturing specifications is obtained by starting water supply along the flow path. Further, the ultrapure water production apparatus further includes a tank on the upstream side of the temporarily placed filter device on the flow path. Moreover, the flow path has a circulation line returning to the tank after passing through the ultrafiltration membrane device. Further, it is preferable that the predetermined period is a period in which the number of times of circulation calculated from the amount and flow rate of water in the circulation line is, for example, 0.5 to 2200 times when the cleaning is started.

一方、本発明の超純水製造装置は、被処理水を流すための流路と、前記流路上に設けられ、前記被処理水をユースポイントの前段で水処理する限外ろ過膜装置と、前記流路上における前記限外ろ過膜装置の前段に設けられ、前記流路に対して仮置きのフィルタ装置の着脱を可能にするフィルタ着脱機構と、を備えている。 On the other hand, the ultrapure water production apparatus of the present invention includes a flow path for flowing water to be treated, an ultrafiltration membrane device provided on the flow path, and performing water treatment on the water to be treated before the point of use, a filter attachment/detachment mechanism that is provided on the flow path before the ultrafiltration membrane device and that enables attachment and detachment of a temporarily placed filter device to the flow path.

上述した仮置きのフィルタ装置は、例えば精密ろ過膜装置である。また、前記流路は、第1の配管で構成されている。一方、前記フィルタ着脱機構は、前記流路から一旦分岐すると共に前記仮置きのフィルタ装置を経由しつつ前記流路の下流側で合流する分岐流路を構成した第2の配管を、前記第1の配管に対して、取り外し可能に接続する複数の継手と、前記第1の配管における前記分岐の位置と前記合流の位置との間に設けられた第1の開閉弁と、を備えている。さらに、前記第2の配管上には、例えば、前記仮置きのフィルタ装置の前後に一対の第2の開閉弁などがそれぞれ設けられている。 The temporary filter device described above is, for example, a microfiltration membrane device. Moreover, the said flow path is comprised by the 1st piping. On the other hand, the filter attachment/detachment mechanism connects a second pipe that forms a branched flow path that once branches from the flow path and merges on the downstream side of the flow path via the temporarily placed filter device to the first pipe. and a first on-off valve provided between the branch position and the confluence position in the first pipe. Further, on the second pipe, for example, a pair of second on-off valves and the like are provided before and after the temporarily placed filter device.

本発明によれば、超純水製造装置の立ち上げ期間を短縮することができる超純水製造装置の立ち上げ方法及び超純水製造装置を提供することが可能である。 According to the present invention, it is possible to provide a method for starting up an ultrapure water production apparatus and an ultrapure water production apparatus capable of shortening the startup period of the ultrapure water production apparatus.

本発明の実施形態に係る超純水製造装置の構成を概略的に示すブロック図。1 is a block diagram schematically showing the configuration of an ultrapure water production apparatus according to an embodiment of the present invention; FIG. 図1の超純水製造装置が備える二次純水製造部の構成を示すブロック図。FIG. 2 is a block diagram showing the configuration of a secondary pure water production unit provided in the ultrapure water production apparatus of FIG. 1; 図2の二次純水製造部から仮置きの精密ろ過膜装置を分離した状態を示す図。FIG. 3 is a diagram showing a state in which a temporarily placed microfiltration membrane device is separated from the secondary pure water production unit in FIG. 2 ; 本発明の実施形態に係る超純水製造装置の立ち上げ方法を示すフローチャート。4 is a flow chart showing a method for starting up the ultrapure water production apparatus according to the embodiment of the present invention. 図2の二次純水製造部とは、被処理水の循環ラインが一部異なる構成例を示した図。The figure which showed the structural example which the circulation line of to-be-processed water partially differs from the secondary pure water production part of FIG. 図3の精密ろ過膜装置の分離状態とは異なる他の分離状態を例示した図。FIG. 4 is a view exemplifying another separation state different from the separation state of the microfiltration membrane device of FIG. 3 ;

以下、本発明の実施の形態を図面に基づき説明する。
図1に示すように、本実施形態に係る超純水製造装置10は、被処理水を水処理して超純水を得る装置であって、前処理部12、一次純水製造部14、被処理水の流路31、タンク16、二次純水製造部18、を含む水処理系15を備えている。前処理部12は、原水として、市水、井水、工業用水などを導入する。この前処理部12は、原水の水質などに応じて適宜の構成を有し、原水の懸濁物質を除去して前処理水を生成する。前処理部12は、例えば砂ろ過装置や精密ろ過装置などを備え、さらに、必要に応じて被処理水の温度を調節するための熱交換器などを有している。
BEST MODE FOR CARRYING OUT THE INVENTION Hereinafter, embodiments of the present invention will be described based on the drawings.
As shown in FIG. 1, an ultrapure water production apparatus 10 according to the present embodiment is an apparatus for obtaining ultrapure water by treating water to be treated, and includes a pretreatment unit 12, a primary pure water production unit 14, A water treatment system 15 including a flow path 31 for water to be treated, a tank 16 and a secondary pure water production unit 18 is provided. The pretreatment unit 12 introduces city water, well water, industrial water, or the like as raw water. The pretreatment unit 12 has an appropriate configuration according to the quality of the raw water, etc., and removes suspended solids from the raw water to generate pretreated water. The pretreatment unit 12 includes, for example, a sand filter device, a microfiltration device, and the like, and further has a heat exchanger and the like for adjusting the temperature of the water to be treated as necessary.

一次純水製造部14は、前処理水中の有機成分、イオン成分、溶存ガスなどを除去して一次純水を製造し、この一次純水をタンク(TK)16に供給する。一次純水製造部14は、例えば、逆浸透膜装置、イオン交換装置(陽イオン交換装置、陰イオン交換装置、混床式イオン交換装置など)、紫外線酸化装置、及び脱気装置(真空脱気装置、脱気膜装置など)のうちの1つ以上を適宜組み合わせて構成される。一次純水は、例えば全有機炭素(TOC:Total Organic Carbon)濃度が5μgC/L以下、抵抗率が17MΩ・cm以上である。タンク16は、一次純水を貯留し、その必要量を二次純水製造部18に供給する。 The primary pure water production unit 14 removes organic components, ion components, dissolved gases, etc. from the pretreated water to produce primary pure water, and supplies this primary pure water to the tank (TK) 16 . The primary pure water production unit 14 includes, for example, a reverse osmosis membrane device, an ion exchange device (cation exchange device, anion exchange device, mixed bed ion exchange device, etc.), an ultraviolet oxidation device, and a degassing device (vacuum degassing device, degassing membrane device, etc.). The primary pure water has, for example, a total organic carbon (TOC) concentration of 5 μgC/L or less and a resistivity of 17 MΩ·cm or more. The tank 16 stores primary pure water and supplies the required amount to the secondary pure water producing section 18 .

一方、二次純水製造部18は、一次純水製造部14により製造された一次純水中の不純物を除去して超純水となる二次純水を製造し、超純水の使用場所であるユースポイント(POU:Point Of Use)20に供給する。流路31は、被処理水を流すための流路であって、水処理系15を構成する前処理部12、一次純水製造部14及び二次純水製造部18によって水処理された被処理水をユースポイント20へ向けて送る。また、図1、図2に示すように、上記したタンク16は、流路31上における後記の精密ろ過膜装置(仮置きのフィルタ装置)27の上流側に備えられている。さらに、流路31は、後記の限外ろ過膜装置28を通過した後、タンク16に戻る循環ライン31bを有している。ここで、図1、図2の例では、循環ライン31bは、最下流に位置するユースポイント20の位置から、タンク16及び二次純水製造部18を経由して、ユースポイント20の位置へ戻る経路を構成している。つまり、ユースポイント20を通過した余剰分の超純水は、流路31の循環ライン31bを通ってタンク16にて回収される。 On the other hand, the secondary pure water production unit 18 removes impurities from the primary pure water produced by the primary pure water production unit 14 to produce secondary pure water that becomes ultrapure water, is supplied to a point of use (POU) 20 . The flow path 31 is a flow path for flowing the water to be treated, and the water to be treated by the pretreatment unit 12, the primary pure water production unit 14, and the secondary pure water production unit 18, which constitute the water treatment system 15. Direct the treated water to the point of use 20. Further, as shown in FIGS. 1 and 2, the tank 16 described above is provided upstream of a microfiltration membrane device (temporary filter device) 27 described later on the flow path 31 . Further, the flow path 31 has a circulation line 31b that returns to the tank 16 after passing through the ultrafiltration membrane device 28 described later. Here, in the examples of FIGS. 1 and 2, the circulation line 31b extends from the position of the point of use 20 located most downstream to the position of the point of use 20 via the tank 16 and the secondary pure water production unit 18. Constructing a return route. That is, the surplus ultrapure water that has passed through the point of use 20 passes through the circulation line 31 b of the flow path 31 and is collected in the tank 16 .

具体的には、図2、図3に示すように、二次純水製造部18は、サークルポンプ(被処理水供給ポンプ)22、熱交換器(HEX:Heat Exchanger)23、紫外線酸化装置(TOC-UV)24、膜脱気装置(MDG:membrane degasifier)25、ポリッシャ26、フィルタ着脱機構30、限外ろ過膜(UF:Ultrafiltration Membrane)装置28、及び微粒子計29を備えている。 Specifically, as shown in FIGS. 2 and 3, the secondary pure water production unit 18 includes a circle pump (water supply pump to be treated) 22, a heat exchanger (HEX) 23, an ultraviolet oxidation device ( TOC-UV) 24 , membrane degasifier (MDG) 25 , polisher 26 , filter attachment/detachment mechanism 30 , ultrafiltration membrane (UF) device 28 , and particle counter 29 .

サークルポンプ22は、タンク16内に収容された被処理水(一次純水)を熱交換器23に供給する被処理水供給ポンプである。熱交換器23は、サークルポンプ22から供給された被処理水の温度を調節する。この際、被処理水は、熱交換器23によって例えば25±3℃に温度調節されることが好ましい。 The circle pump 22 is a to-be-treated water supply pump that supplies the to-be-treated water (primary pure water) contained in the tank 16 to the heat exchanger 23 . The heat exchanger 23 adjusts the temperature of the water to be treated supplied from the circle pump 22 . At this time, the temperature of the water to be treated is preferably adjusted to, for example, 25±3° C. by the heat exchanger 23 .

紫外線酸化装置24は、熱交換器23で温度調節された被処理水(一次純水)に紫外線を照射して、被処理水中の微量有機物を分解除去する。紫外線酸化装置24は、例えば紫外線ランプを有し、波長185nm付近の紫外線を発生させる。紫外線酸化装置24は、波長254nm付近の紫外線を発生させるものであってもよい。このような紫外線酸化装置24内で被処理水に紫外線が照射されると、紫外線が被処理水を分解してOHラジカルを生成し、このOHラジカルが、被処理水中の有機物を酸化分解する。 The ultraviolet oxidation device 24 irradiates the water to be treated (primary pure water) temperature-controlled by the heat exchanger 23 with ultraviolet rays to decompose and remove trace organic substances in the water to be treated. The ultraviolet oxidation device 24 has, for example, an ultraviolet lamp and generates ultraviolet rays with a wavelength of about 185 nm. The ultraviolet oxidation device 24 may generate ultraviolet rays having a wavelength of about 254 nm. When the water to be treated is irradiated with ultraviolet rays in such an ultraviolet oxidation device 24, the ultraviolet rays decompose the water to generate OH radicals, and the OH radicals oxidize and decompose organic matter in the water to be treated.

膜脱気装置25は、気体透過性の膜の二次側を減圧して、一次側を通流する被処理水中の溶存ガスのみを二次側に透過させて除去する装置である。ポリッシャ26は、陽イオン交換樹脂と陰イオン交換樹脂とが混合された混床式のイオン交換樹脂を有し、被処理水の中の微量の陽イオン成分及び陰イオン成分を吸着除去する非再生型の混床式イオン交換装置である。 The membrane degassing device 25 is a device that decompresses the secondary side of a gas-permeable membrane and allows only the dissolved gas in the water to be treated flowing through the primary side to permeate the secondary side and remove it. The polisher 26 has a mixed-bed type ion exchange resin in which a cation exchange resin and an anion exchange resin are mixed, and is a non-regenerating non-regenerating resin that adsorbs and removes trace amounts of cation and anion components in the water to be treated. It is a mixed-bed ion exchange apparatus of the type.

後に詳述するフィルタ着脱機構(フィルタ取付・取外機構)30は、被処理水の流路31上における限外ろ過膜装置28の前段(直前)に設けられており、前記流路31に対して、精密ろ過膜装置27の着脱を可能にする。限外ろ過膜装置28は、流路31上における最下流のユースポイント20の前段(直前)に設けられている。 A filter attachment/detachment mechanism (filter attachment/removal mechanism) 30, which will be described in detail later, is provided in the front stage (immediately) of the ultrafiltration membrane device 28 on the flow path 31 of the water to be treated. to enable attachment and detachment of the microfiltration membrane device 27 . The ultrafiltration membrane device 28 is provided in the front stage (immediately before) the most downstream point of use 20 on the channel 31 .

限外ろ過膜装置28は、複数の中空糸型モジュールを有しており、この中空糸型モジュールの1つあたりの通水流量は、5m3/h以上である。一般的には10m3/h以上である。流路31上に設けられたこの限外ろ過膜装置28は、ポリッシャ26(又は装着時の精密ろ過膜装置27)による被処理水を、ユースポイント20の前段でさらに水処理することにより、例えば粒子径50nm以上の微粒子を除去して超純水(二次純水)を得る。 The ultrafiltration membrane device 28 has a plurality of hollow fiber modules, and the water flow rate per hollow fiber module is 5 m 3 /h or more. Generally, it is 10 m 3 /h or more. The ultrafiltration membrane device 28 provided on the flow path 31 further treats the water to be treated by the polisher 26 (or the microfiltration membrane device 27 when attached) at the front stage of the point of use 20, for example Ultrapure water (secondary pure water) is obtained by removing fine particles having a particle size of 50 nm or more.

ここで、本実施形態の超純水製造装置10における製造スペック内の超純水(所期の水質条件を満足する超純水)は、粒子径50nm以上の粒子の数が200個/L以下であり、また、全有機炭素濃度が1μgC/L以下であり、さらには抵抗率が18MΩ・cm以上である。微粒子計29は、限外ろ過膜装置28によって水処理された二次純水(超純水)中の粒子の粒径を計測する。 Here, ultrapure water (ultrapure water that satisfies the desired water quality conditions) within the manufacturing specifications of the ultrapure water production apparatus 10 of the present embodiment has a particle size of 50 nm or more and the number of particles is 200/L or less. and a total organic carbon concentration of 1 μgC/L or less, and a resistivity of 18 MΩ·cm or more. The particle counter 29 measures the particle size of particles in the secondary pure water (ultra-pure water) treated by the ultrafiltration membrane device 28 .

次に、フィルタ着脱機構30及び仮置きの精密ろ過膜装置27について詳述する。フィルタ着脱機構30は、図2、図3に示すように、複数の継手36、37、41、42及び開閉弁(第1の開閉弁)33を備えている。一方、精密ろ過膜(MF:Microfiltration Membrane)装置27は、後段の限外ろ過膜装置28の膜の孔径よりも大きい孔径の膜を備えている。この精密ろ過膜の孔径は、特に限定されないものの、0.2μm以上の粒子を分離するろ過精度を有しているものがより好ましい。これは、本発明において早期立ち上がりを阻害する原因物質が、比較的大きな微粒子であることから、比較的大きい孔径の精密ろ過膜で十分だからである。さらに、このような精密ろ過膜は、実質的に膜本数が低減されて圧力損失が小さくなるため、良好な通水性能が得られる。 Next, the filter attaching/detaching mechanism 30 and the temporarily placed microfiltration membrane device 27 will be described in detail. The filter attachment/detachment mechanism 30 includes a plurality of joints 36, 37, 41, and 42 and an on-off valve (first on-off valve) 33, as shown in FIGS. On the other hand, the microfiltration membrane (MF) device 27 has a membrane with a pore size larger than that of the ultrafiltration membrane device 28 in the subsequent stage. Although the pore size of the microfiltration membrane is not particularly limited, it is more preferable that the microfiltration membrane has a filtration accuracy to separate particles of 0.2 μm or more. This is because, in the present invention, the causative substances that inhibit the early start-up are relatively large fine particles, so a microfiltration membrane with a relatively large pore size is sufficient. Furthermore, such a microfiltration membrane has a substantially reduced number of membranes and a small pressure loss, so that good water permeability can be obtained.

精密ろ過膜としては、表層ろ過式のものでも、デプスろ過式のものでもよい。後者のデプスろ過式の精密ろ過膜は、多くの通水流量を確保でき、これにより、使用する膜本数が少なく安価なため、より好ましい。 The microfiltration membrane may be of a surface layer filtration type or a depth filtration type. The latter depth filtration type microfiltration membrane is more preferable because it can secure a large flow rate of water flow, thereby reducing the number of membranes to be used and being inexpensive.

なお、デプスろ過式の精密ろ過膜は、一般的に、超純水製造装置の前段側、例えば、一次純水製造部に設置される逆浸透膜のガードフィルター等、もしくは前処理部に用いられるが、本実施形態のように二次純水製造部に適用しようとする場合、デプスろ過式の精密ろ過膜では孔径が大きすぎるため、微細微粒子の除去は期待できないと考えていたので、立ち上げにて効果を示すことは意外性を持つものであった。 In addition, the depth filtration type microfiltration membrane is generally used in the upstream side of the ultrapure water production apparatus, for example, the guard filter of the reverse osmosis membrane installed in the primary pure water production unit, or in the pretreatment unit. However, when trying to apply it to the secondary pure water production part like this embodiment, the pore size of the depth filtration type microfiltration membrane is too large, so we thought that removal of fine particles could not be expected. It was unexpected to show the effect in .

表層ろ過式の精密ろ過膜としては、HDCIIシリーズ、ポリファインIIシリーズ(以上Pall社製)など、デプスろ過式の精密ろ過膜としては、Betafineシリーズ(スリーエムジャパン社製)、プロファイルII、ネクシスシリーズ、プロファイルUPシリーズ(以上Pall社製)等を好適に用いることが可能である。 Surface filtration type microfiltration membranes include the HDCII series and Polyfine II series (manufactured by Pall). Profile UP series (manufactured by Pall) and the like can be preferably used.

つまり、精密ろ過膜装置27は、超純水製造装置10内の例えば配管類から脱離した金属粒子(異物)や、超純水製造装置10の設置環境中から水処理系15内に混入した砂など、を捕捉することが可能となる。 In other words, the microfiltration membrane device 27 contains metal particles (foreign matter) detached from, for example, piping in the ultrapure water production device 10, and mixed into the water treatment system 15 from the installation environment of the ultrapure water production device 10. It is possible to capture sand and the like.

精密ろ過膜装置27は、仮置きの(一時的な)保護フィルタ(Temporary Guard Filter)装置である。この精密ろ過膜装置27は、超純水製造装置10を例えば新規に設置して立ち上げる際には、超純水製造装置10に取り付けられているものの、超純水製造装置の立ち上げ完了後には、超純水製造装置10から、フィルタ着脱機構30を介して、取り外し(撤去)される。 The microfiltration membrane device 27 is a temporary (temporary) protective filter (Temporary Guard Filter) device. This microfiltration membrane device 27 is attached to the ultrapure water production device 10 when the ultrapure water production device 10 is newly installed and started up, for example, but after the startup of the ultrapure water production device is completed is removed (removed) from the ultrapure water production apparatus 10 via the filter attachment/detachment mechanism 30 .

ここで、被処理水の流路31は、配管31aによって構成されている。また、精密ろ過膜装置27を仮置きするために、流路31から一旦分岐すると共に精密ろ過膜装置27を経由しつつ当該流路31の下流側で合流する分岐流路32を構成するための配管(第2の配管)32aが用意されている。つまり、精密ろ過膜装置27は、配管32aの途中に介在される。 Here, the flow path 31 for the water to be treated is configured by a pipe 31a. Also, in order to temporarily place the microfiltration membrane device 27, a branch flow path 32 that once branches from the flow path 31 and merges on the downstream side of the flow path 31 via the microfiltration membrane device 27 is provided. A pipe (second pipe) 32a is prepared. That is, the microfiltration membrane device 27 is interposed in the middle of the pipe 32a.

図2、図3に示すように、継手41、42は、配管32aを、配管31aに対して、取り外し可能に接続する。また、継手36、37も、配管32aを、配管31aに対して、取り外し可能に接続している。具体的には、継手36、37は、開閉弁34、35と共に配管32aを、配管31aから取り外し可能としている。本実施形態では、図3に示すように、主に、継手41、42を介して、配管31aから、配管32a及び仮置きの精密ろ過膜装置27を取り外す態様を例示する。 As shown in FIGS. 2 and 3, joints 41 and 42 detachably connect pipe 32a to pipe 31a. Joints 36 and 37 also detachably connect the pipe 32a to the pipe 31a. Specifically, the joints 36 and 37 allow the pipe 32a to be detached from the pipe 31a together with the on-off valves 34 and 35. As shown in FIG. In the present embodiment, as shown in FIG. 3, a mode of removing the pipe 32a and the temporarily placed microfiltration membrane device 27 from the pipe 31a mainly through the joints 41 and 42 will be exemplified.

開閉弁33は、配管31aにおける前記分岐の位置と前記合流の位置との間に設けられており、配管31a内に対する通水と遮断(非通水)とを切り換える。また、配管32a上には、仮置きの精密ろ過膜装置27の前後に一対の開閉弁(第2の開閉弁)34、35がそれぞれ設けられている。開閉弁34、35は、配管32a内に対する通水と遮断(非通水)とを切り換える。 The on-off valve 33 is provided between the branch position and the confluence position in the pipe 31a, and switches between water flow and cutoff (non-flow) to the pipe 31a. A pair of on-off valves (second on-off valves) 34 and 35 are provided on the pipe 32a before and after the temporarily placed microfiltration membrane device 27, respectively. The on-off valves 34 and 35 switch between passing water and blocking (not passing water) to the inside of the pipe 32a.

したがって、図2に示すように、例えば、精密ろ過膜装置27が設置されている状態で、流路31から一旦分岐し分岐流路32及び精密ろ過膜装置27を経て流路31の下流側で合流する経路で送水する場合には、開閉弁33が閉じられる一方で、開閉弁34、35が開かれる。また、図3に示すように、超純水製造装置10から精密ろ過膜装置27が分離(撤去)されている状態や、図2に示すように、精密ろ過膜装置27が設置されている状態を含めて、分岐流路32及び精密ろ過膜装置27を経由させない経路で流路31に対して送水する場合には、開閉弁33が開かれる一方で、開閉弁34、35が閉じられる。 Therefore, as shown in FIG. 2, for example, in a state where the microfiltration membrane device 27 is installed, once branched from the flow channel 31 and passed through the branch flow channel 32 and the microfiltration membrane device 27, on the downstream side of the flow channel 31 When water is fed through a confluence route, the on-off valve 33 is closed, while the on-off valves 34 and 35 are opened. In addition, as shown in FIG. 3, the microfiltration membrane device 27 is separated (removed) from the ultrapure water production apparatus 10, and as shown in FIG. 2, the microfiltration membrane device 27 is installed. When water is sent to the channel 31 through a route that does not pass through the branch channel 32 and the microfiltration membrane device 27, the on-off valve 33 is opened, while the on-off valves 34 and 35 are closed.

次に、本実施形態に係る超純水製造装置10の立ち上げ方法(超純水製造装置10による超純水の製造方法)を、図1~図3に加え、図4に示すフローチャートに基づき説明する。超純水製造装置10の立ち上げに際して、まず、ポリッシャ26、限外ろ過膜装置28、流路31(配管31a)などの組み付けに加え、フィルタ着脱機構30を介して、図2、図4に示すように、超純水製造装置10本体に仮置きの精密ろ過膜装置27を設置(組み付け)する(S1)。 Next, a method for starting up the ultrapure water production apparatus 10 according to the present embodiment (method for producing ultrapure water by the ultrapure water production apparatus 10) will be described based on the flowchart shown in FIG. 4 in addition to FIGS. explain. When starting up the ultrapure water production device 10, first, in addition to assembling the polisher 26, the ultrafiltration membrane device 28, the flow path 31 (piping 31a), etc. As shown, the temporary microfiltration membrane device 27 is installed (assembled) in the main body of the ultrapure water production device 10 (S1).

精密ろ過膜装置27の設置後には、配管31a上の開閉弁33を閉じる一方で、配管32a(分岐流路32)上の開閉弁34、35を開く。精密ろ過膜装置27のこのような設置後に、例えば前処理部12の前段から、分岐流路32及び循環ライン31bを含む流路31に沿って送水を開始することにより、図1、図2、図4に示すように、前処理部12、一次純水製造部14内の各装置、上記した流路31、ポリッシャ26、限外ろ過膜装置28などを含む水処理系15を洗浄する(S2)。この際、超純水製造装置10内の例えば配管類から脱離した金属粒子や、水処理系15に混入した砂などが、精密ろ過膜装置27によって捕捉される。 After the microfiltration membrane device 27 is installed, the on-off valve 33 on the pipe 31a is closed, while the on-off valves 34 and 35 on the pipe 32a (branch flow path 32) are opened. After such installation of the microfiltration membrane device 27, for example, by starting water supply from the front stage of the pretreatment unit 12 along the flow path 31 including the branch flow path 32 and the circulation line 31b, FIGS. As shown in FIG. 4, the water treatment system 15 including the pretreatment unit 12, each device in the primary pure water production unit 14, the flow path 31 described above, the polisher 26, the ultrafiltration membrane device 28, etc. is washed (S2 ). At this time, the microfiltration membrane device 27 captures metal particles detached from, for example, piping in the ultrapure water production apparatus 10 and sand mixed in the water treatment system 15 .

前述した洗浄において、水処理系15を洗浄するための送水用の水(洗浄水)は、一次純水がよい。また、このような洗浄は、当該洗浄の開始に伴い、ユースポイント20の位置を通過した洗浄のための水(洗浄水)が、少なくとも、循環ライン31bを一巡して前記ユースポイント20の位置へ戻る所定の期間以上実施される。 In the cleaning described above, the water (cleaning water) for cleaning the water treatment system 15 is preferably primary pure water. In addition, in such washing, when the washing is started, the water for washing (washing water) that has passed through the position of the point of use 20 at least circulates through the circulation line 31b to the position of the point of use 20. It is implemented for a predetermined period of time or longer.

前記洗浄の開始に伴い、循環ライン31b内の水量と流量から計算される循環回数は、0.5~2200回が好ましく、1~1000回がより好ましく、40~500回がさらに好ましい。また、通水時間は、0.25時間~1000時間が好ましく、0.5時間~720時間がより好ましく、24時間~170時間がさらに好ましい。なお、異物は循環系の前段側に多く含まれているため、循環回数が0.5回でも効果は得られるが、1回を超えると効果は大きくなる。 With the start of washing, the number of circulations calculated from the amount and flow rate of water in the circulation line 31b is preferably 0.5 to 2200 times, more preferably 1 to 1000 times, and even more preferably 40 to 500 times. Also, the water flow time is preferably 0.25 hours to 1000 hours, more preferably 0.5 hours to 720 hours, and even more preferably 24 hours to 170 hours. In addition, since many foreign matters are contained in the front stage of the circulation system, the effect can be obtained even if the number of times of circulation is 0.5, but the effect becomes large when the number of times exceeds 1.

循環回数や通水時間が少ない場合、精密ろ過膜で異物を十分補足できないため、立ち上げ時間の短縮効果が得られなくなる。一方、循環回数や通水時間が多い場合、精密ろ過膜に捕捉された異物が例えば粉砕されて後段に流出するため、立ち上げ時間の短縮効果が得られなくなる。なお、敷設された配管の長さや口径、分岐の数などによって最も適した条件は異なってくるのが、上記範囲のなかで適宜条件を選定して洗浄を実施する。 If the number of times of circulation or the water flow time is small, the microfiltration membrane cannot sufficiently trap foreign matter, so the effect of shortening the start-up time cannot be obtained. On the other hand, if the number of times of circulation or the water flow time is large, the foreign matter captured by the microfiltration membrane is pulverized and flows out to the subsequent stage, so that the effect of shortening the start-up time cannot be obtained. Although the most suitable conditions differ depending on the length and diameter of the installed pipe, the number of branches, etc., washing is carried out by appropriately selecting the conditions within the above range.

ここで、所定の期間は、例えば一週間などであってもよい。また、洗浄中については、前処理部12、一次純水製造部14及び二次純水製造部18内の各装置は、稼働状態とされる。前述したような洗浄により、超純水製造装置10内の例えば配管類から脱離した金属粒子などが精密ろ過膜装置27によって捕捉される。 Here, the predetermined period may be, for example, one week. During cleaning, each device in the pretreatment unit 12, the primary pure water production unit 14, and the secondary pure water production unit 18 is in operation. Due to the washing as described above, the microfiltration membrane device 27 captures metal particles and the like detached from, for example, pipes in the ultrapure water production device 10 .

洗浄の開始から所定の期間経過後に(S3のYES)、金属粒子などを捕捉した精密ろ過膜装置27を超純水製造装置10から撤去(分離)する(S4)。具体的には、送水を停止した後、配管32a(分岐流路32)上の開閉弁34、35を閉じる。さらに、図3に示すように、継手41、42を介して、配管32aと共に仮置きの精密ろ過膜装置27の取り外しを行う。 After a predetermined period of time has elapsed from the start of cleaning (YES in S3), the microfiltration membrane device 27 that has captured metal particles and the like is removed (separated) from the ultrapure water production device 10 (S4). Specifically, after stopping the water supply, the on-off valves 34 and 35 on the pipe 32a (the branch flow path 32) are closed. Further, as shown in FIG. 3, the temporarily placed microfiltration membrane device 27 is removed together with the pipe 32a via the joints 41 and 42 .

精密ろ過膜装置27を撤去した後、開閉弁33を開くとともに、前処理部12、一次純水製造部14及び二次純水製造部18内の各装置を稼働状態にし、さらに循環ライン31bを含む流路31に沿った送水(前処理部12への原水の供給)を開始して、水処理系15による水処理を実施する(S5)。なお、撤去するステップ(S4)と水処理を実施するステップ(S5)との操作の間、送水を停止せずに洗浄を行うことも可能である。その場合、開閉弁33を開き、同時に、もしくは、しかる後、開閉弁34、35を閉じる。そして、精密ろ過膜装置27の取り外しを行えばよい。この水処理は、先に例示した所期の製造スペック内に収まる超純水が得られる(超純水の水質がスペックインする)まで、継続される(S6)。この際、二次純水(超純水)中の粒子の粒径が製造スペック内であるか否かについては、微粒子計29によって計測される。この後、製造スペック内に収まる超純水が得られた場合(S6のYES)、超純水製造装置10の立ち上げが完了となる(S7)。 After removing the microfiltration membrane device 27, the on-off valve 33 is opened, each device in the pretreatment unit 12, the primary pure water production unit 14, and the secondary pure water production unit 18 is put into operation, and the circulation line 31b is closed. The water supply (supply of raw water to the pretreatment unit 12) along the flow path 31 is started, and water treatment is performed by the water treatment system 15 (S5). It is also possible to perform washing without stopping water supply between the step of removing (S4) and the step of water treatment (S5). In that case, the on-off valve 33 is opened, and the on-off valves 34 and 35 are closed at the same time or after that. Then, the microfiltration membrane device 27 may be removed. This water treatment is continued until ultrapure water within the desired manufacturing specifications exemplified above is obtained (the quality of the ultrapure water meets the specifications) (S6). At this time, the particle size counter 29 measures whether the particle size of the particles in the secondary pure water (ultra-pure water) is within the manufacturing specifications. After that, when ultrapure water within the manufacturing specifications is obtained (YES in S6), startup of the ultrapure water production apparatus 10 is completed (S7).

ここで、本実施形態の超純水製造装置10の立ち上げ方法では、限外ろ過膜装置28の前段(直前)に精密ろ過膜装置27を設置した状態で水処理系15内の洗浄を開始し、所定の期間経過後に、例えば金属粒子や砂などを捕捉した精密ろ過膜装置27を、超純水製造装置10から撤去(分離)したうえで、水処理を実施するので、水処理系15内から上記した金属粒子や砂などを取り去ることができる。したがって、本実施形態の超純水製造装置10の立ち上げ方法によれば、水処理系15内に存在し得る例えば砂や金属粒子の成分の溶出などが続き、超純水の水質が低下したままの状態になることなどを回避できる。すなわち、精密ろ過膜装置27の撤去後の水処理では、所期の製造スペック内に収まる超純水が迅速に得られ、これにより、超純水製造装置10の立ち上げ期間を短縮することができる。 Here, in the method for starting up the ultrapure water production apparatus 10 of the present embodiment, cleaning inside the water treatment system 15 is started with the microfiltration membrane device 27 installed in the preceding stage (immediately) of the ultrafiltration membrane device 28. Then, after a predetermined period of time has passed, the microfiltration membrane device 27 that captures metal particles, sand, etc., for example, is removed (separated) from the ultrapure water production device 10, and water treatment is performed. It is possible to remove the above-mentioned metal particles, sand, etc. from the inside. Therefore, according to the method for starting up the ultrapure water production apparatus 10 of the present embodiment, the elution of components such as sand and metal particles that may exist in the water treatment system 15 continues, and the quality of the ultrapure water deteriorates. You can avoid being stuck. That is, in the water treatment after removing the microfiltration membrane device 27, ultrapure water within the expected manufacturing specifications can be obtained quickly, thereby shortening the start-up period of the ultrapure water production device 10. can.

なお、本操作のいずれかの段階で、過酸化水素等による二次純水製造部18内の殺菌操作を行うことが可能である。この場合、ポリッシャ26、及び/もしくは、限外ろ過膜装置28をバイパスするライン(図示していない)を用いて、ポリッシャ26、及び/もしくは、限外ろ過膜装置28を系(水処理系15)から外し、二次純水製造部18のいずれか、例えば、タンク16、もしくはポンプ22の吸入側に設けられた分岐バルブを用いて、系内に過酸化水素を添加する。しかる後、所定時間循環を行なう。十分な殺菌処理が行われた後、過酸化水素水をいずれかの場所から排水する。系内の過酸化水素がなくなった後、ポリッシャ26及び/もしくは、限外ろ過膜装置28のバイパスを行うことを停止する。 At any stage of this operation, it is possible to sterilize the inside of the secondary pure water production section 18 with hydrogen peroxide or the like. In this case, a line (not shown) that bypasses the polisher 26 and/or the ultrafiltration membrane device 28 is used to connect the polisher 26 and/or the ultrafiltration membrane device 28 to the system (water treatment system 15 ), and hydrogen peroxide is added into the system using a branch valve provided on the suction side of either the secondary pure water production unit 18 , for example, the tank 16 or the pump 22 . After that, circulation is performed for a predetermined time. After sufficient sterilization, the hydrogen peroxide solution is drained from some place. Bypassing the polisher 26 and/or the ultrafiltration membrane device 28 is stopped after the hydrogen peroxide in the system has disappeared.

また、本発明の超純水製造装置の立ち上げ方法において、イオン交換樹脂をポリッシャ26本体内に充填していない状態でポリッシャ26を含めた水処理系15の洗浄を行い、いずれかの段階で洗浄操作を止めてポリッシャ26本体内にイオン交換樹脂を充填するようにしてもよい。 Further, in the method for starting up the ultrapure water production apparatus of the present invention, the water treatment system 15 including the polisher 26 is cleaned while the ion exchange resin is not filled in the main body of the polisher 26. The cleaning operation may be stopped and the body of the polisher 26 may be filled with ion exchange resin.

さらに、以上の操作は、ユースポイント20を含む循環ライン31bを適用して説明したが、図5に示すように、ユースポイント20をバイパスした循環ライン31cを用いることも可能である。その場合には、いずれかの段階で、循環ライン内にユースポイント20を含ませる操作をすることになる。なお、より立ち上がりの時間を短縮するためには、ユースポイント20を含んだ循環ライン31bでの立ち上げ方法を選択することが好ましい。 Furthermore, the above operation has been described by applying the circulation line 31b including the point of use 20, but it is also possible to use the circulation line 31c bypassing the point of use 20 as shown in FIG. In that case, at some stage, an operation is performed to include the point of use 20 in the circulation line. In addition, in order to shorten the start-up time, it is preferable to select the start-up method in the circulation line 31b including the point of use 20. FIG.

また、サークルポンプ22による給水を補足するために、図5に示すように、ポリッシャ26と継手36との間にブースタポンプ43を設けてもよい。このようなブースタポンプ43は、図2、図3に例示した二次純水製造部や、後述する図6に示す二次純水製造部に、追加することも可能である。 In order to supplement the water supply by the circle pump 22, a booster pump 43 may be provided between the polisher 26 and the joint 36 as shown in FIG. Such a booster pump 43 can also be added to the secondary pure water producing section illustrated in FIGS. 2 and 3 or the secondary pure water producing section shown in FIG. 6, which will be described later.

一方、超純水製造装置10の装置構成に対して、上述したような仮置きのフィルタ装置(精密ろ過膜装置27)を備えていない超純水製造装置を用い、洗浄水による洗浄を行ったうえで、水処理を実施した場合、このような洗浄及び水処理を例えば4カ月の期間、継続したとしても、製造スペック内に収まる超純水が得られないことが検証されている。この場合、限外ろ過膜装置28内の中空糸型モジュールに金属粉や砂などが捕捉されたままの状態となっており、捕捉された異物が時間とともに粉砕され後段に流出することが原因で製造スペック内に収まらなかったのである。そこで、限外ろ過膜装置28内の全ての中空糸型モジュールを新品と交換して再度の水処理を実施したことで、ようやく製造スペック内に収まる超純水が得られた。 On the other hand, with respect to the device configuration of the ultrapure water production device 10, an ultrapure water production device that does not have a temporary filter device (microfiltration membrane device 27) as described above was used, and cleaning was performed with cleaning water. In addition, it has been verified that when water treatment is performed, even if such washing and water treatment are continued for a period of, for example, four months, ultrapure water within manufacturing specifications cannot be obtained. In this case, the hollow fiber module in the ultrafiltration membrane device 28 is in a state where metal powder, sand, etc. are trapped, and the trapped foreign matter is pulverized over time and flows out to the subsequent stage. It didn't fit within the manufacturing specs. Therefore, by replacing all the hollow fiber modules in the ultrafiltration membrane device 28 with new ones and performing the water treatment again, ultrapure water within the manufacturing specifications was finally obtained.

また、超純水製造装置10と同じ装置構成の超純水製造装置を用い、精密ろ過膜装置27を取り付けた状態のまま、洗浄水による洗浄、及び水処理も実施した場合、このような洗浄及び水処理を例えば3カ月の期間、継続したとしても、製造スペック内に収まる超純水が得られないことが検証されている。この場合、精密ろ過膜装置27内に例えば目視可能なサイズの金属粉や砂などが捕捉されており、精密ろ過膜装置27を撤去した後、再度の水処理を実施したことで、ようやく製造スペック内に収まる超純水が得られた。 In addition, when using an ultrapure water production apparatus having the same device configuration as the ultrapure water production apparatus 10 and with the microfiltration membrane device 27 attached, cleaning with cleaning water and water treatment are also performed. And even if the water treatment is continued for a period of, for example, three months, it has been verified that ultrapure water that falls within the manufacturing specifications cannot be obtained. In this case, the microfiltration membrane device 27 contains, for example, metal powder and sand of a size that can be seen with the naked eye. Ultrapure water was obtained that fits within the

これに対して、本実施形態の超純水製造装置10の立ち上げ方法によれば、精密ろ過膜装置27を設置した状態で、過酸化水素を含む洗浄液を用いた洗浄を1週間行った後、超純水製造装置10から、例えば金属粒子や砂などを捕捉した精密ろ過膜装置27を、撤去したうえで、水処理を実施することで、直ちに、製造スペック内に収まる超純水が得られたことが検証されている。 On the other hand, according to the method for starting up the ultrapure water production apparatus 10 of the present embodiment, after one week of cleaning using the cleaning liquid containing hydrogen peroxide with the microfiltration membrane apparatus 27 installed, After removing the microfiltration membrane device 27 that captures, for example, metal particles and sand from the ultrapure water production device 10, water treatment is performed to immediately obtain ultrapure water that falls within the manufacturing specifications. It has been verified that

既述したように、本実施形態の超純水製造装置10の立ち上げ方法(及びこの立ち上げ方法を適用可能な超純水製造装置10)によれば、仮置きのフィルタ装置(精密ろ過膜装置27)及びフィルタ着脱機構30を有効に活用した洗浄及び水処理を実施することで、超純水製造装置10の立ち上げ期間の短縮化を図ることができる。なお、図3に示したフィルタ着脱機構30に代えて、図6に示すように、フィルタ着脱機構40を超純水製造装置及びその立ち上げ方法に適用することも可能である。このフィルタ着脱機構40の場合、開閉弁34、35を閉じた後、継手36、37を介して、開閉弁34、35と共に、配管32(分岐流路32a)及び精密ろ過膜装置27が撤去(分離)される。開閉弁34、35及び配管32aと共に仮置きの精密ろ過膜装置27を、超純水製造装置10から撤去した後には、継手36、37における配管32aを取り付けていた部位に、例えば閉塞プラグ(止め栓)38、39などが取り付けられることになる。 As described above, according to the startup method of the ultrapure water production apparatus 10 of the present embodiment (and the ultrapure water production apparatus 10 to which this startup method can be applied), a temporary filter device (microfiltration membrane By effectively utilizing the device 27) and the filter attachment/detachment mechanism 30 to perform cleaning and water treatment, it is possible to shorten the start-up period of the ultrapure water production device 10. FIG. As shown in FIG. 6, instead of the filter attaching/detaching mechanism 30 shown in FIG. 3, it is also possible to apply a filter attaching/detaching mechanism 40 to the ultrapure water production apparatus and its start-up method. In the case of this filter attachment/detachment mechanism 40, after the on-off valves 34 and 35 are closed, the piping 32 (branch flow path 32a) and the microfiltration membrane device 27 are removed ( separated). After removing the temporarily placed microfiltration membrane device 27 together with the on-off valves 34 and 35 and the pipe 32a from the ultrapure water production system 10, a blocking plug (stopper Plugs) 38, 39, etc. will be attached.

以上、本発明を実施の形態により具体的に説明したが、本発明は、この実施形態そのままに限定されるものではなく、実施段階ではその要旨を逸脱しない範囲で種々変更可能である。例えば、実施形態に示される全構成要素からいくつかの構成要素を削除してもよいし、上記実施形態に開示した複数の構成要素を適宜組み合わせることも可能である。 Although the present invention has been specifically described with reference to the embodiments, the present invention is not limited to the embodiments as they are, and various changes can be made in the implementation stage without departing from the scope of the invention. For example, some constituent elements may be deleted from all the constituent elements shown in the embodiments, and it is also possible to appropriately combine a plurality of constituent elements disclosed in the above embodiments.

10…超純水製造装置、12…前処理部、14…一次純水製造部、15…水処理系、16…タンク(TK)、18…二次純水製造部、20…ユースポイント(POU)、22…サークルポンプ、23…熱交換器(HEX)、24…紫外線酸化装置(TOC-UV)、25…膜脱気装置(MDG)、26…ポリッシャ、27…精密ろ過膜装置(MF)、28…限外ろ過膜装置(UF)、29…微粒子計、30,40…フィルタ着脱機構、31…流路、31a…配管(第1の配管)、31b,31c…循環ライン、32…分岐流路、32a…配管(第2の配管)、33…開閉弁(第1の開閉弁)、34,35……開閉弁(第2の開閉弁)、36,37,41,42…継手、38,39…閉塞プラグ。 10... Ultrapure water production device, 12... Pretreatment unit, 14... Primary pure water production unit, 15... Water treatment system, 16... Tank (TK), 18... Secondary pure water production unit, 20... Point of use (POU ), 22... Circle pump, 23... Heat exchanger (HEX), 24... Ultraviolet oxidation device (TOC-UV), 25... Membrane degassing device (MDG), 26... Polisher, 27... Microfiltration membrane device (MF) , 28... Ultrafiltration membrane device (UF), 29... Particle counter, 30, 40... Filter attachment/detachment mechanism, 31... Flow path, 31a... Pipe (first pipe), 31b, 31c... Circulation line, 32... Branch Flow path 32a Piping (second piping) 33 On-off valve (first on-off valve) 34, 35 On-off valve (second on-off valve) 36, 37, 41, 42 Joint, 38, 39... Closing plugs.

Claims (12)

被処理水を流すための流路と、前記流路上に設けられ、前記被処理水をユースポイントの前段で水処理する限外ろ過膜装置と、を少なくとも含む水処理系を備えた超純水製造装置の立ち上げ方法であって、
前記流路上における前記限外ろ過膜装置の前段に、仮置きのフィルタ装置と、前記流路から一旦分岐すると共に前記仮置きのフィルタ装置を経由しつつ前記流路の下流側で合流する分岐流路と、を設置する工程と、
前記仮置きのフィルタ装置の設置後に、前記流路に沿って純水の送水を開始することにより前記水処理系を洗浄する工程と、
前記純水の送水による洗浄の開始から所定の期間経過後に、前記仮置きのフィルタ装置と前記分岐流路とを前記超純水製造装置から分離する工程と、
を有する超純水製造装置の立ち上げ方法。
Ultrapure water provided with a water treatment system including at least a flow path for flowing water to be treated, and an ultrafiltration membrane device provided on the flow path for treating the water to be treated before a point of use. A method for starting up a manufacturing apparatus,
A temporarily placed filter device is provided on the flow channel before the ultrafiltration membrane device, and a branch flow that once branches from the flow channel and merges on the downstream side of the flow channel while passing through the temporarily placed filter device. installing a path ;
a step of cleaning the water treatment system by starting to supply pure water along the channel after installing the temporary filter device;
a step of separating the temporarily placed filter device and the branch flow path from the ultrapure water production device after a predetermined period of time has elapsed since the start of cleaning by feeding the pure water;
A method for starting up an ultrapure water production apparatus having
前記洗浄は、殺菌処理を含む、
請求項1に記載の超純水製造装置の立ち上げ方法。
The washing includes a sterilization treatment,
The method for starting up the ultrapure water production apparatus according to claim 1.
前記分離する工程の後、前記流路に沿って前記被処理水の送水を開始し所期の製造スペック内に収まる超純水が得られるまで水処理を行う工程、
をさらに有する請求項1又は2に記載の超純水製造装置の立ち上げ方法。
After the separating step, a step of starting to feed the water to be treated along the flow path and performing water treatment until ultrapure water within the desired manufacturing specifications is obtained;
The method for starting up an ultrapure water production apparatus according to claim 1 or 2, further comprising:
前記超純水製造装置は、前記分岐流路上における前記仮置きのフィルタ装置の上流側にタンクをさらに備え、
前記流路は、前記限外ろ過膜装置を通過した後、前記タンクに戻る循環ラインを有し、
前記洗浄において、前記送水された前記純水を前記循環ラインに循環させる、
請求項1から3までのいずれか1項に記載の超純水製造装置の立ち上げ方法。
The ultrapure water production apparatus further comprises a tank on the upstream side of the temporarily placed filter device on the branch flow path,
The flow path has a circulation line that returns to the tank after passing through the ultrafiltration membrane device ,
In the cleaning, the sent pure water is circulated through the circulation line;
A method for starting up an ultrapure water production apparatus according to any one of claims 1 to 3.
前記所定の期間は、前記洗浄の開始に伴い、前記循環ライン内の水量と流量から計算される循環回数が、0.5~2200回となる期間である、
請求項4に記載の超純水製造装置の立ち上げ方法。
The predetermined period is a period in which the number of circulations calculated from the water volume and flow rate in the circulation line is 0.5 to 2200 when the cleaning is started.
The method for starting up the ultrapure water production apparatus according to claim 4.
前記仮置きのフィルタ装置は、0.2μm以上の粒子を分離するろ過精度を有する、
請求項1から5までのいずれか1項に記載の超純水製造装置の立ち上げ方法。
The temporarily placed filter device has a filtration accuracy that separates particles of 0.2 μm or more,
A method for starting up an ultrapure water production apparatus according to any one of claims 1 to 5.
前記限外ろ過膜装置は、複数の中空糸型モジュールを有し、
前記中空糸型モジュールの1つあたりの通水流量は、10m3/h以上である、
請求項1から6までのいずれか1項に記載の超純水製造装置の立ち上げ方法。
The ultrafiltration membrane device has a plurality of hollow fiber modules,
A water flow rate per one of the hollow fiber modules is 10 m 3 /h or more.
A method for starting up an ultrapure water production apparatus according to any one of claims 1 to 6.
所期の製造スペック内に収まる超純水は、粒子径50nm以上の粒子の数が200個/L以下である、
請求項1から7までのいずれか1項に記載の超純水製造装置の立ち上げ方法。
Ultrapure water that fits within the expected manufacturing specifications has a particle size of 50 nm or more and the number of particles is 200/L or less.
A method for starting up an ultrapure water production apparatus according to any one of claims 1 to 7.
被処理水を流すための流路と、
前記流路上に設けられ、前記被処理水をユースポイントの前段で水処理する限外ろ過膜装置と、
前記流路上における前記限外ろ過膜装置の前段に設けられ、前記流路に対して仮置きのフィルタ装置の着脱を可能にするフィルタ着脱機構と、を備え、
前記流路は、第1の配管で構成され、
前記フィルタ着脱機構は、
前記流路から一旦分岐すると共に前記仮置きのフィルタ装置を経由しつつ前記流路の下流側で合流する分岐流路を構成する第2の配管を、前記第1の配管に対して、取り外し可能に接続する複数の継手と、
前記第1の配管における前記分岐の位置と前記合流の位置との間に設けられた第1の開閉弁と、
を備える超純水製造装置。
a channel for flowing the water to be treated;
an ultrafiltration membrane device that is provided on the flow path and that treats the water to be treated before the point of use;
a filter attachment/detachment mechanism that is provided in front of the ultrafiltration membrane device on the flow path and enables attachment and detachment of a temporarily placed filter device to the flow path ,
The flow path is composed of a first pipe,
The filter attachment/detachment mechanism includes:
A second pipe, which once branches from the flow channel and forms a branched flow channel that merges on the downstream side of the flow channel via the temporarily placed filter device, can be removed from the first pipe. a plurality of fittings that connect to
a first on-off valve provided between the branch position and the confluence position in the first pipe;
An ultrapure water production device comprising:
前記仮置きのフィルタ装置は、精密ろ過膜装置である、
請求項9に記載の超純水製造装置。
The temporarily placed filter device is a microfiltration membrane device,
The ultrapure water production apparatus according to claim 9.
前記第2の配管上には、前記仮置きのフィルタ装置の前後に一対の第2の開閉弁がそれぞれ設けられている、
請求項に記載の超純水製造装置。
A pair of second on-off valves are provided on the second pipe before and after the temporarily placed filter device, respectively.
The ultrapure water production apparatus according to claim 9 .
前記流路上における前記仮置きのフィルタ装置の上流側にタンクをさらに備え、 A tank is further provided on the upstream side of the temporarily placed filter device on the flow path,
前記流路は、前記限外ろ過膜装置を通過した後、前記タンクに戻る循環ラインを有する、請求項9から11までのいずれか1項に記載の超純水製造装置。 The ultrapure water production apparatus according to any one of claims 9 to 11, wherein the flow path has a circulation line returning to the tank after passing through the ultrafiltration membrane device.
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